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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: C581 − 20

Standard Practice for


Determining Chemical Resistance of Thermosetting Resins
Used in Glass-Fiber-Reinforced Structures Intended for
Liquid Service1
This standard is issued under the fixed designation C581; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* 2. Referenced Documents


1.1 This practice is designed to evaluate, in an unstressed 2.1 ASTM Standards:2
state, the chemical resistance of thermosetting resins used in D790 Test Methods for Flexural Properties of Unreinforced
the fabrication of reinforced thermosetting plastic (RTP) lami- and Reinforced Plastics and Electrical Insulating Materi-
nates. This practice provides for the determination of changes als
in the properties, described as follows, of the test specimens D883 Terminology Relating to Plastics
and test reagent after exposure of the specimens to the reagent: D2563 Practice for Classifying Visual Defects in Glass-
hardness of specimens, weight change thickness, appearance of Reinforced Plastic Laminate Parts
specimens, appearance of immersion media, and flexural D2583 Test Method for Indentation Hardness of Rigid Plas-
strength and modulus. tics by Means of a Barcol Impressor
1.1.1 This practice is also useful to evaluate other factors, D2584 Test Method for Ignition Loss of Cured Reinforced
such as surfacing veils and the effect of resin additives, on the Resins
chemical resistance of the resin.
1.2 The values stated in inch-pound units are to be regarded 3. Terminology
as standard. The values given in parentheses are mathematical 3.1 Definitions of Terms:
conversions to SI units that are provided for information only 3.1.1 For definitions of terms associated with plastic
and are not considered standard. materials, see Terminology D883.
NOTE 1—There is no known ISO equivalent to this standard.
4. Significance and Use
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4.1 The results obtained by this practice shall serve as a
responsibility of the user of this standard to establish appro- guide in, but not as the sole basis for, selection of a thermo-
priate safety, health, and environmental practices and deter- setting resin used in an RTP structure. No attempt has been
mine the applicability of regulatory limitations prior to use. made to incorporate into the practice all the various factors that
1.4 This international standard was developed in accor- will potentially affect the serviceability of an RTP structure
dance with internationally recognized principles on standard- when subjected to chemical environments. These factors will
ization established in the Decision on Principles for the potentially include stress, different resin-to-glass ratios, and
Development of International Standards, Guides and Recom- multiple veils.
mendations issued by the World Trade Organization Technical
5. Apparatus
Barriers to Trade (TBT) Committee.
5.1 Hardness Testing Instrument—This shall be as described
in Test Method D2583.
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and
is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic Piping
2
Systems and Chemical Equipment. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 15, 2020. Published March 2020. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1965. Last previous edition approved in 2015 as C581 – 15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C0581-20. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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C581 − 20
5.2 Flexural Properties Testing Apparatus, in accordance 7.2.1 Laminate Size—A suitable laminate size has been
with Test Methods D790. found to be 26 by 33 in. (660 by 838 mm) after trimming. This
laminate size is not restrictive and other dimensions are
5.3 Thickness Measurement—A micrometer suitable for
acceptable.
measurement to 0.001 in. (0.025 mm).
7.2.2 Thickness—The thickness of the cured standard lami-
5.4 Containers, of sufficient size, capacity, and inertness to nate shall be between 0.120 and 0.140 in. (3.05 and 3.56 mm).
allow total immersion of reinforced thermosetting plastic 7.2.3 Reinforcement Content—The glass fiber and binder
specimens in the specific corrosives chosen for testing. These shall be 4.73 6 0.47 oz/ft2 (three layers of 1.5 oz/ft2 chopped
containers shall, when necessary, be capable of maintaining strand mat 4.5 oz/ft2 having a nominal binder content of 3.5 %
liquid levels of volatile solutions, that is, solvents. This can be and two layers of 10 mil surfacing mat 0.23 oz/ft2 having a
accomplished by the use of reflux condensers. nominal binder content of 7 %)—determined by pre-weighing
5.5 Heating Apparatus—A constant temperature oven, heat- the materials prior to construction of the laminate. This is
ing mantle, or liquid bath capable of maintaining temperature equivalent to 23.6 weight % (12.5 volume %) glass fiber when
within range of 64.0°F (62.2°C). Take proper precautions if using a resin having a cured specific gravity of 1.15. Such a
the corrosives selected are flammable liquids. laminate will have a thickness of 0.125 in. (3.18 mm). The use
of resins having different specific gravities will result in
5.6 Analytical Balance, suitable for accurate weighing to different weight percentages of glass fiber, but the volume
0.001 g. percentage of glass fiber will remain the same. When using
synthetic organic fiber surfacing veil, the glass content shall be
6. Reagents 4.50 6 0.45 oz/ft2 (three layers of 1.5 oz/ft2 chopped strand
6.1 The test media shall consist of the reagents or solutions mat having a nominal binder content of 3.5 %).
to which the RTP laminates are to be exposed. 7.2.4 Hardness—The hardness shall be at least 90 % of that
of a fully-cured clear casting of the resin, or of a similarly
7. Test Specimens constructed laminate as defined by the resin manufacturer.
Hardness shall be determined in accordance with s5.1. Note
7.1 Standard Laminates—Prepare standard fiber-reinforced that the use of synthetic veil will result in significantly lower
laminates using identical reinforcement in all of the laminates. hardness values. The hardness value will vary with the type of
The laminates shall be constructed of the following materials: resin and number of plies of synthetic veil. The resin manu-
7.1.1 Surfacing Mat (Veil)—A thin mat of fine fibers used facturer needs to be contacted for the allowable Barcol
primarily to produce a smooth, resin-rich surface on a rein- hardness value of a laminate containing synthetic veils with the
forced plastic. The surfacing veil helps determine the thickness specific resin.
of the resin-rich layer, reduces microcracking and provides a 7.2.5 Laminate Condition—The laminate shall meet Accep-
non-wicking chemically–resistant layer. The surfacing veil tance Level I of Table I of Practice D2563.
shall be compatible with the resin and manufactured with
uniform fiber distribution and non-bundled fibers. The dry veil 7.3 Fabrication of Standard Laminate—The sequence of
layer(s) shall be a minimum 10 mils in thickness and produce lay-up shall be as follows:
a 10 to 15 mil resin-saturated veil layer per 10 mils of dry veil. 7.3.1 Apply catalyzed resin and a 10-mil (0.25-mm) surfac-
To eliminate the surfacing veil as a variable in corrosion tests, ing mat on a flat surface covered with plastic release film or
prepare each laminate within a test group with the same treated with a suitable release agent and roll to distribute resin.
surfacing veil. NOTE 3—Use the following formula as a guide to determine the total
7.1.2 Chopped Strand Mat—Type E glass fiber with sizing weight of resin to be used. This is equivalent to 12.5 volume % glass fiber
and binder compatible with the resin. It is acceptable to use in the laminate. Grams resin equals grams glass fiber material per 7.2.3
times 2.82 G. Where G equals specific gravity of cured resin. It is
other glass fiber compositions, but using such alternate com- acceptable to use excess resin due to loss by adhering to mixing
positions shall be considered as variables for comparison to the containers, rollers, and other factors. A suggested amount of excess resin
standard. is 10 to 15 % by weight.
7.1.2.1 Note that this practice applies to E-CR glass fiber, 7.3.2 Follow with three plies of 1.5 oz/ft2 chopped strand
which is a type of E glass fiber. If the E glass fiber material is mat and resin. Roll after each ply to distribute and wet-out the
of the E-CR type that information shall be identified in the test chopped strand mat. Rolling with a serrated roller is acceptable
report. after each ply to remove entrapped air but it shall be done in
7.1.3 Resin—Catalyzed and promoted in accordance with accordance with 7.3.4. The mat weight shall be within 65 % of
the resin manufacturer’s recommendation. 1.5 oz/ft2 upon weighing the full 26 by 33-in. cut (660 by
838-mm) piece, (or other full dimension used, 7.2.1.).
NOTE 2—It is acceptable to add fillers, such as antimony trioxide for
improved fire performance or thixotropes for viscosity control, but it is NOTE 4—Cut chopped strand mat so that the 26-in. dimension is across
possible that this will detract from the corrosion resistance of the test the width of the roll and the 33-in. dimension is along the machine
laminate. direction of the mat. Mat weight variation will most commonly occur
across the width of the mat. If a wide roll of mat, 52 in. (1320 mm) or
7.2 Dimensions and General Properties—The laminates greater, is used, place the two plies of mat in the laminate such that the
shall conform to the required dimensions and general proper- center cut of one ply is placed over the outside edge of the second ply. If
ties of 7.2 and be fabricated in accordance with 7.3. narrower width mat is used, reverse the second ply 180° in the machine

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C581 − 20
direction and lay it on top of the first ply to minimize weight variations. 8. Procedure
7.3.3 Follow with a 10-mil (0.25-mm) surfacing mat as in 8.1 Measurement of Specimens—Immediately following the
7.3.1. curing period, measure the thickness of the specimens to the
7.3.4 Remove the air by rolling over the surface with a nearest 0.001 in. (0.025 mm) at the geometric center of each of
serrated metal or plastic roller. Take care not to expel enough the intended 1 by 3 in. (25.4 by 76.2 mm) specimens that will
resin to raise the glass content above the permissible maxi- be cut for flexural tests after the completed exposures. Measure
mum. The laminate is considered within the range of allowable the weight of the specimens to the nearest 0.01 g. These
levels of resin and glass if the thickness of the laminate is thickness and weight measurements shall also be used for
within 0.120 and 0.140 in. (3.05 and 3.56 mm), as described in comparison against thickness and weight measurements after
7.2.2. the completed exposures.
7.3.5 After the lay-up is completed, cover the laminate with
8.2 Exposure—Following the curing period, as specified in
a plastic release film to prevent air inhibition or to provide a
7.3.6, prior to immersion, record a brief description of the color
uniform smooth glossy surface, or both. Carefully smooth
and surface appearance of the coupons and the color and the
down to remove entrapped air.
clarity of the test solution. The total number of coupons per
NOTE 5—It is acceptable to use any convenient method for the container is not limited except by the ability of the container to
application of the release film. Regardless of how it is applied, it is critical hold the coupons without touching each other or the container.
that any entrapped air between the film and the laminate be entirely The coupons must always be completely immersed. Coupons
removed. One method of application is done by previously wrapping the
film around a metal rod. Starting at one edge of the laminate, slowly unroll
shall be vertical, parallel, and spaced a minimum of 0.25 in.
the film from the rod, keeping a bead of resin ahead of the rod as you cross (6.35 mm) apart. There shall be a minimum of 0.50 in. (12.7
the laminate. Any entrapped air remaining can be removed by rubbing a mm) between coupon edges and the container or the liquid
tongue depressor across the release film surface. Carefully pull the film surface. Place the closed container in a constant temperature
taut and fasten at the edges to prevent wrinkling of the film. Placing stops oven adjusted to the required temperature or in a suitably
(neoprene has been found to be suitable) around the edges of the laminate
and passing a heavy metal roller over the laminate helps to insure uniform adjusted liquid bath. Examine the coupons after 30, 90, 180
controlled thickness. days, and one year of immersion or other time intervals as
required to determine the rate of attack.
7.3.6 Cure as recommended by the resin manufacturer. The
cure schedule shall be reported. 8.2.1 Discard the test solution and replace it with fresh
solution as often as necessary to maintain original composition
7.3.7 Trim edges as required.
and concentration. As a minimum, solutions known to be stable
7.4 Record of Standard Laminate Construction—Record the need to be replaced at the end of each test period.
properties of the standard laminate as follows:
8.3 Cleaning and Examination After Exposure—Clean the
7.4.1 Hardness—Determine Barcol hardness on the strip as coupon and dry by blotting with a paper towel. Cold tap water
described in 7.2.4 in accordance with Test Method D2583. is normally used for specimen cleaning. If other cleaning
7.4.2 Laminate Conditions—Visually examine the laminate. agents are used, verify that they do not attack the resin being
The laminate shall meet Acceptance Level I of Table 1 of tested.
Practice D2563. 8.3.1 Note any indication of surface attack on a coupon, any
7.4.3 If the laminate meets the requirements of this discoloration of the test solution, and the formation of any
specification, retain the laminate sections for preparation of test sediment.
specimens. 8.3.2 After final blotting, immediately measure the coupon
NOTE 6—The major criteria for accepting a laminate is thickness and thickness to the nearest 0.001 in. (0.025 mm) in the geometric
not glass content. If glass content is desired, cut eight 1 by 1 in. specimens center of each intended 1 by 3 in. (25 by 76.2 mm) specimen.
from the center of the laminate and test in accordance with Test Method Measure the coupon to the nearest 0.01g. The Barcol hardness
D2584. can then be checked, taking an average of ten readings on each
7.5 Individual Test Specimens: coupon, a minimum of 0.50 in. (12.7 mm) from the edge.
7.5.1 Specimens for immersion in test solutions shall be 8.3.3 After washing and measuring thickness, weight, and
approximately 4 by 5 in. (101.6 by 127 mm), cut from the Barcol hardness, place the coupons in an air-tight polyethylene
standard laminate. bag for conditioning or shipping as described in 8.4.1.
7.5.2 Identity of specimens shall be maintained by suitable 8.4 Flexural Testing—Determine the flexural strength and
means. modulus for: (1) two sets of three specimens immediately
7.5.3 Cut edges and drilled holes, if used for suspension, following the curing period, and (2) one set of three specimens
shall be sanded smooth and coated with paraffinated resin. after each inspection, for each solution, and each test tempera-
7.5.4 The number of specimens required is dependent on the ture. Calculation of flexural strength and modulus after expo-
number of test solutions to be employed, the number of sure shall use the coupon thickness determined at the time of
different temperatures at which testing is performed, and the flexural testing as measured in 8.3.2. The two pretested sets
number of test intervals. In addition, at least two 4 by 5 in. shall be taken from the center of the laminate as described in
(101.6 by 127 mm) specimens shall be available for test (see 7.2.1. The flexural strengths for these two sets shall be
8.4) following the curing period, prior to immersion. averaged together for use in calculating the retained flexural

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C581 − 20
strength in 9.2. The flexural modulus values shall also be E1 = flexural modulus of specimen after curing period, and
averaged for use in 9.2. E2 = flexural modulus of specimen after test period.
8.4.1 Flexural tests shall be conducted in accordance with
9.2.1 Calculate flexural strength and modulus properties in
Procedure A of Test Methods D790, except for the conditioning
accordance with Section 12 of Test Methods D790.
parameters specified in this document. Coupons being tested at
9.2.2 Construct graphs showing the average percentage of
the exposure location shall be placed in the conditioning
retained flexural strength and the average flexural modulus of
environment for a minimum of 2 h immediately following the
the specimens broken at a given examination period after
“cleaning and examination” described in 8.3. The coupon shall
immersion in a particular test solution at a given temperature,
be tested during the same day after removing the coupon from
plotting the percentage of retained flexural strength and flex-
the test environment. For testing at a different location, the
ural modulus as the vertical axis, and the test period, in days,
clean, dry coupons shall be placed in a vapor tight bag for
as the horizontal axis.
shipment.
9.3 Percent Weight and Thickness Change—Calculate to the
NOTE 7—In cases of volatile chemical exposure, special methods of
specimen handling will probably be required.
nearest 0.01 % the percent weight and thickness change of the
specimen during immersion for each examination period.
8.4.2 Three 1 by 3 in. (25 by 76.2 mm) (see Fig. 1) are cut
from each 4 by 5 in. coupon. After cutting, the specimen edges 9.4 Calculate the percent weight and thickness change, and
shall be routed or sanded to provide a nick-free edge. Test tabulate or graph these values as a function of the test period,
specimens shall be the full thickness of the exposure coupon. in days.
10. Interpretation of Results
9. Calculation
10.1 Mechanical Properties of the Specimen—Because of
9.1 Barcol Hardness Change—Tabulate or construct a graph
the chemical nature of certain types of plastic materials, the
showing the actual hardness readings of the specimens exposed
rate of change with time is of more significance than the actual
at a given temperature, and the test period, in days.
value at any one time. A plot of the test results will indicate
9.2 Retained Flexural Strength and Modulus—Calculate to whether a particular specimen will approach constant flexural
the nearest 1.0 %, the percentage retention of flexural strength strength, flexural modulus, or hardness with time or will
and flexural modulus of the specimen during immersion for continue to change as the test progresses.
each examination period, taking the flexural strength and
10.2 Appearance of Specimen—Visual inspection of the
flexural modulus after curing as 100 %:
exposed specimen for surface cracks, loss of gloss, etching,
Retained flexural strength, % 5 @ S 2 /S 1 # 3 100 (1) blistering, pitting, softening, changes in thickness, or other
where: irregularities, is very important, for these conditions indicate
some degradation of the laminate by a chemical environment.
S1 = flexural strength of specimen after curing period, and
S2 = flexural strength of specimen after test period. 10.3 Appearance of Immersion Medium—It is possible that
Retained flexural modulus, % 5 @ E 2 /E 1 # 3 100 (2)
discoloration of the test solution and the formation of sediment
will be significant factors. It is possible that an initial discol-
where: oration will indicate extraction of soluble components.
10.4 Weight and Thickness of Specimen—Weight and thick-
ness changes can indicate the extent of chemical degradation or
absorption of the test solution.
NOTE 8—Carry out all test exposures for the longest practical time to
assure valid results. It is particularly important to obtain 6 and 12-month
results in order to determine whether the properties are stable over a
period of time. Short-term results (less than six months) can be unreliable
when evaluating resins.

11. Report
11.1 Report the following information:
11.1.1 Company and individual preparing standard lami-
nates.
11.1.2 Complete identification of material tested including
resin, nonvolatile content, accelerator, catalyst, reinforcement,
surfacing mat, and filler, such as fire-retardant additive or
thixotropes.
11.1.2.1 As this practice applies to E-CR glass fiber, a type
of E glass fiber, if the E glass fiber material is of the E-CR type
that information shall be identified in the test report.
11.1.3 Cure cycle including room temperature gel time, time
FIG. 1 Specimen Cutting Guide at room temperature before testing or before post-cure if

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C581 − 20
required, post-cure time, and temperature. Any special post- 11.1.8.5 Weight and thickness before and after exposure.
curing techniques such as boiling water or steam for FDA-type 11.1.8.6 Flexural strength and flexural modulus of coupons
applications shall also be reported. and percent retention of flexural strength and flexural modulus.
11.1.4 Glass content of standard laminate, if run in accor-
11.1.9 Graph showing percent retention of flexural strength
dance with Note 6.
and flexural modulus plotted against test periods.
11.1.5 Hardness, flexural strength of control coupons.
11.1.6 Color and surface appearance of specimens before
testing. 12. Precision and Bias
11.1.7 Test conditions; immersion medium, temperature, 12.1 No precision statement can be made for this practice,
and the like. since controlled round-robin test programs have not been run.
11.1.8 Total duration of test in days, and examination The test results of this practice are obtained to assign bias
periods, in days. For each examination period, the data listed in statements to the subjective results since there are no standards.
11.1.8.11 through 11.1.8.6 are required. The bias of the quantitative results are covered by Test
11.1.8.1 Pretesting samples conditioning (if different than Methods D790.
standard).
11.1.8.2 Appearance of specimens after immersion (surface
13. Keywords
cracks, loss of gloss, etching, pitting, softening, and the like).
11.1.8.3 Appearance of immersion medium (discoloration, 13.1 chemical resistance; glass-fiber-reinforced; glass-
sediment, and the like). reinforced plastic (GRP); laminate; liquid service; reinforced
11.1.8.4 Barcol hardness of the specimens before and after thermosetting plastic (RTP); reinforced thermosetting resins;
exposure. thermosetting resins

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (C581 – 15)
that may impact the use of this standard. (February 15, 2020)

(1) Subsection 1.1: Addition of indentation for formatting. (3) Subsection 7.2.3: Removal of extra spacing around paren-
(2) Subsection 7.2.3: Updated preweighing to pre-weighing for theses.
grammatical correctness.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: C582 − 09 (Reapproved 2016)

Standard Specification for


Contact-Molded Reinforced Thermosetting Plastic (RTP)
Laminates for Corrosion-Resistant Equipment1
This standard is issued under the fixed designation C582; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope 2. Referenced Documents


1.1 This specification covers composition, thickness, fabri- 2.1 ASTM Standards:2
cating procedures, and physical property requirements for glass C581 Practice for Determining Chemical Resistance of
fiber reinforced thermoset polyester, vinyl ester, or other Thermosetting Resins Used in Glass-Fiber-Reinforced
qualified thermosetting resin laminates comprising the materi- Structures Intended for Liquid Service
als of construction for RTP corrosion-resistant tanks, piping, D638 Test Method for Tensile Properties of Plastics
and equipment. This specification is limited to fabrication by D695 Test Method for Compressive Properties of Rigid
contact molding. Plastics
D790 Test Methods for Flexural Properties of Unreinforced
NOTE 1—The laminates covered by this specification are manufactured
during fabrication of contact-molded RTP tanks, piping, and other and Reinforced Plastics and Electrical Insulating Materi-
equipment. als
NOTE 2—There is no known ISO equivalent to this standard. D883 Terminology Relating to Plastics
1.2 The values stated in inch-pound units are to be regarded D2583 Test Method for Indentation Hardness of Rigid Plas-
as standard. The values given in parentheses are mathematical tics by Means of a Barcol Impressor
conversions to SI units that are provided for information only D2584 Test Method for Ignition Loss of Cured Reinforced
and are not considered standard. Resins
D3681 Test Method for Chemical Resistance of “Fiberglass”
1.3 The following safety hazards caveat pertains only to the (Glass–Fiber–Reinforced Thermosetting-Resin) Pipe in a
test method portion, Section 8, of this specification: This Deflected Condition
standard does not purport to address all of the safety concerns, E84 Test Method for Surface Burning Characteristics of
if any, associated with its use. It is the responsibility of the user Building Materials
of this standard to establish appropriate safety, health, and
environmental practices and determine the applicability of 3. Definitions
regulatory limitations prior to use. 3.1 Definitions used in this specification are in accordance
1.4 This international standard was developed in accor- with Terminology D883 unless otherwise indicated. The ab-
dance with internationally recognized principles on standard- breviation for reinforced thermoset plastic is RTP.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 3.2 polyester—resins produced by the polycondensation of
mendations issued by the World Trade Organization Technical dihydroxyderivatives and dibasic organic acids or anhydrides,
Barriers to Trade (TBT) Committee. wherein at least one component contributes ethylenic unsatu-
ration yielding resins that can be compounded with styryl
monomers and reacted to give highly crosslinked thermoset
copolymers.
1
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced
2
Plastic Piping Systems and Chemical Equipment. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2016. Published November 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1965. Last previous edition approved in 2009 as C582 – 09. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C0582-09R16. the ASTM website.

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C582 − 09 (2016)
3.3 vinyl ester—resins characterized by reactive unsatura- 0.125-in. (3.175-mm) thick, flat laminates with all-mat glass content of 25
tion located predominately in terminal positions that can be to 30 %.
NOTE 5—Maximum flame spread designation by Test Method E84
compounded with styryl monomers and reacted to give highly relates to measurement and description of the properties of materials,
crosslinked thermoset copolymers. products, or systems in response to heat and flame under controlled
NOTE 3—These resins are handled in the same way as polyesters in laboratory conditions and should not be considered or used for the
fabrication of RTP components. description or appraisal of the fire hazard of materials, products, or
systems under actual fire conditions. However, results of this test may be
3.4 contact molding—a method of fabrication wherein the used as elements of a fire risk assessment that takes into account all the
glass-fiber reinforcement is applied to the mold, in the form of factors that are pertinent to an assessment of the fire hazard or a particular
chopped strand mat or woven roving, by hand or from a reel, end use.
or in the form of chopped strands of continuous-filament glass 4.1.3 Grade—In Arabic numerals, shall designate the mini-
from a chopper-spray gun. The resin matrix is applied by mum physical property levels of a laminate at 73.4 6 3.6°F (23
various methods, including brush, roller, or spray gun. Con- 6 2°C).
solidation of the composite laminate is by rolling.
NOTE 6—The five Arabic grade numbers designate minimum physical
property levels of a laminate obtained from tests of representative
4. Classification production process samples. They are not arbitrarily selected values.
4.1 Laminates shall be classified according to type, class, 4.1.4 Thickness—Nominal, shall be designated by Arabic
and grade. number in decimal hundredths of an inch. (See Table 1 and
4.1.1 Type—In Roman numerals, shall designate the rein- Table 2 for standard thicknesses.)
forcement structure comprised of specific plies of glass fiber in
specific sequences. NOTE 7—Table 1 and Table 2 are for reference purposes and do not
preclude other laminate-type constructions, such as nonwoven biaxial or
4.1.1.1 Type I—A standard all-mat or chopped-roving unidirectional fabric, which may be agreed upon between the buyer and
construction, or both, as shown in Table 1. the seller, or may be added to this specification if they have been fully
4.1.1.2 Type II—A standard mat or chopped-roving and identified and characterized, as shown in Appendix X2.
woven-roving construction, or combination thereof, as shown 4.1.5 Classification Requirements for Different Laminates—
in Table 2. Laminate designation from Table 3 shall consist of the abbre-
4.1.1.3 Other types, such as standard mat or chopped roving viation RTP followed by (1) type in Roman numerals; (2) class
with alternating layers of nonwoven biaxial or unidirectional in capital letters followed by FS( ) if required; (3) grade
reinforcement in the structured plies. may be qualified in consisting of five Arabic numbers to designate minimum levels
accordance with Appendix X2. of physical properties and (4) thickness designated by Arabic
4.1.2 Class—In capital letters, shall designate the generic number in decimal inches (or ALL, if properties apply to all
resin: “P” for polyester and “V” for vinyl ester. The letters thicknesses).
“FS” followed by parenthesis, “FS( ),” shall designate fire 4.1.5.1 Examples:
retardancy, if specified, with maximum flame spread in the (1) RTP I 1 ALL, designates Type I polyester laminate,
parentheses in accordance with Test Method E84. non-fire-retardant Grade 13211, having the following mini-
NOTE 4—Fire retardancy by Test Method E84 is determined for mum physical property levels (see Table 3):

TABLE 1 Standard Laminate Composition Type IA


Calculated Corrosion Structural PliesE Drafting
ThicknessBC BarrierD Number and Sequence of Plies Symbols
in. (mm) 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

0.18 (4.6) V M M M M V, 4M
0.23 (5.8) V M M M M M V, 5M
0.27 (6.9) V M M M M M M V, 6M
0.31 (7.9) V M M M M M M M V, 7M
0.35 (8.9) V M M M M M M M M V, 8M
0.40 (10.2) V M M M M M M M M M V, 9M
0.44 (11.2) V M M M M M M M M M M V, 10M
0.48 (12.2) V M M M M M M M M M M M V, 11M
0.53 (13.5) V M M M M M M M M M M M M V, 12M
0.57 (14.5) V M M M M M M M M M M M M M V, 13M
0.61 (15.5) V M M M M M M M M M M M M M M V, 14M
0.66 (16.8) V M M M M M M M M M M M M M M M V, 15M
0.70 (17.8) V M M M M M M M M M M M M M M M M V, 16M
0.74 (18.8) V M M M M M M M M M M M M M M M M M V, 17M
A
Glass content, weight, % = 25 to 30, all thickness.
B
Calculated thickness for design purposes is determined as follows:
V = Surfacing mat − 0.010 in./ply (0.25 mm/ply) when saturated with resin.
M = 1 1⁄2 oz/ft2 (459 g/m2) mat − 0.043 in./ply (1.1 mm/ply) when saturated with resin.
C
The thickness shall be not less than 90 % of the calculated thickness shown.
D
Corrosion barrier (Plies 1, 2, and 3) shall gel before structural plies are added.
E
Structural lay-up may be interrupted at intervals long enough to exotherm if required by the laminate manufacturing procedure and 6.3.1.

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TABLE 2 Standard Laminate Composition Type II
Calculated Glass Corrosion Structural PliesD
ThicknessAB Content BarrierC Number and Sequence of Plies Drafting
(weight, Symbols
in. (mm) %) 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21

0.22 (5.6) 28 to 33 V M M M R M V, 2M, MRM


0.29 (7.4) 30 to 35 V M M M R M R M V, 2M, 2(MR)M
0.37 (9.4) 30 to 35 V M M M R M R M R M V, 2M, 3(MR)M
0.41 (10.4) 30 to 35 V M M M R M R M R M M V, 2M, 3(MR)M,
M
0.49 (12.5) 34 to 38 V M M M R M R M R M M R M V, 2M, 3(MR)M,
MRM
0.57 (14.5) 34 to 38 V M M M R M R M R M M R M R M V, 2M, 3(MR)M,
2(MR)M
0.64 (16.3) 37 to 41 V M M M R M R M R M M R M R M R M V, 2M, 3(MR)M,
3(MR)M
0.69 (17.5) 37 to 41 V M M M R M R M R M M R M R M R M M V, 2M, 3(MR)M,
3(MR)M,M
0.76 (19.3) 37 to 41 V M M M R M R M R M M R M R M R M M R M V, 2M, 3(MR)M,
3(MR)M,
MRM
A
Calculated thickness for design purposes is determined as follows:
V = Surfacing mat − 0.010 in./ply (0.25 mm/ply) when saturated with resin.
M = 1 1⁄2 oz ⁄ft2 (459 g/m2) mat = 0.043 in./ply (1.1 mm/ply) when saturated with resin.
R = 241⁄2 oz/yd2 (832 g/m2) 5 × 4 woven roving = 0.033 in./ply (0.84 mm/ply) when saturated with resin.
B
The thickness shall be not less than 90 % of the calculated thickness shown.
C
Corrosion barrier (Plies 1, 2, and 3) shall gel before structural plies are added.
D
Structural lay-up may be interrupted long enough to exotherm following an “M” ply, if required by the laminate manufacturing procedure. Location of exotherm plies may
be shifted within the laminate body. No plies may be omitted. Refer to 6.3.1.

TABLE 3 Classification System for Hand Lay-up Laminates Using Minimum Property ValuesA
Classification Order
RTP followed by:

(1) Type I II III IV V


(2) Class P V ... ... ... followed by FS ( ), if
Polyester Vinylester specified with flame
spread in parentheses in
accordance with Test
Method E84
Physical and Mechanical Properties
(3) Grade 1 2 3 4 5 6 7 8 9 0
1st Digit: Tensile strength, 9 11 13 15 17.5 20 ... ... ... ...
ultimate psi × 103
(MPa) (62) (76) (90) (104) (121) (138) ... ... ... ...
2nd Digit: Tensile modulus, 0.85 0.95 1.05 1.15 1.3 1.5 1.75 2.0 ... ...
tangent psi × 103
(MPa) (5 863) (6 552) (7 242) (7 932) (8 966) (10 346) (12 070) (13 794) ... ...
3rd Digit: Flexural strength, 16 18 20 22 24 ... ... ... ... ...
ultimate psi × 103
(MPa) (110) (124) (138) (152) (166) ... ... ... ... ...
4th Digit: Flexural modulus, 0.7 0.85 1.0 1.15 1.3 1.5 ... ... ... ...
psi × 106
(MPa) (4 828) (5 863) (6 897) (7 932) (8 966) (10 346) ... ... ... ...
5th Digit: Glass content, by 25 28 30 34 37 40 44 ... ... ...
weight, %
A
Table will be completed as new resins and higher strength laminates become available.

Tensile strength, ultimate—9000 psi (62 MPa). (2) RTP II P FS(25) 55433.30, designates Type II, poly-
Tensile modulus—1 050 000 psi (7242 MPa). ester fire-retardant resin laminate with a maximum flame
Flexural strength, ultimate—18 000 psi (124 MPa). spread of 25, Grade 55433 having the following minimum
Flexural modulus—700 000 psi (4828 MPa). physical property levels (see Table 3):
Glass content—25 %. Tensile strength, ultimate—17 500 psi (121 MPa).
Thickness—“ALL” thicknesses. Tensile modulus—1 300 000 psi (8966 MPa).

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Flexural strength, ultimate—22 000 psi (152 MPa). 5.2.3 Woven Roving, shall be “E” or “ECR” type glass, 241⁄2
Flexural modulus—1 000 000 psi (6897 MPa). oz/yd2 (832 g/m2), 5 by 4 square weave fabric having a sizing
Glass content—30 %. compatible with the resin.
Thickness—0.30 in. (7.62 mm). 5.2.4 Roving, used in chopper guns for spray-up application,
shall be “E” or “ECR” type glass with sizing compatible with
5. Materials the resin.
5.1 Resin Matrix System: 5.2.5 Other Reinforcements, such as nonwoven biaxial or
unidirectional fabric. These products shall be a commercial
5.1.1 The resin shall be determined to be acceptable for the
grade of “E” or “ECR” type glass fiber with a sizing that is
service either by test, see 8.6, or by verified case history.
compatible with the resin.
5.1.2 Catalyst/Promoter System, shall be as recommended
or approved by the resin producer. 5.3 Laminates:
5.1.3 Diluents, such as added styrene, fillers, dyes, 5.3.1 Laminate construction shall be in accordance with the
pigments, or flame retardants shall be used only when agreed tabulated lay-up sequence for the specified type.
upon between the fabricator and the buyer. When such items 5.3.2 Type I, laminate structure is detailed in Table 1.
are required, limits for each shall be agreed upon between the 5.3.3 Type II, laminate structure is detailed in Table 2.
fabricator and the buyer. A thixotropic agent may be added to
the resin for viscosity control. 6. Laminate Fabrication
NOTE 8—The addition of fillers, dyes, pigments, flame retardants, and 6.1 Apply the catalyzed resin to a mold or mandrel properly
thixotropic agents may interfere with visual inspection of laminate quality. prepared with a parting agent or film suitable for the lay-up
NOTE 9—Chemical resistance can be significantly affected by the resin. Next apply the specified surface mat, rolling so as to
catalyst/promoter system, diluents, dyes, fillers, flame retardants, or draw the resin through the mat for thorough wet-out and
thixotropic agent used in the resin. deaeration.
5.1.4 Resin Pastes, used where necessary to fill crevices 6.2 Apply resin and two plies of 11⁄2-oz (42.6-g) mat. As an
formed by joining subassemblies before overlay shall not be alternative, a minimum of two passes of chopped roving
subject to the limitations of 5.1.3. Pastes shall be made with (minimum fiber length 1 in. (25.4 mm) and resin may be
thixotropic agents. applied by the spray-up process equivalent in weight and
5.1.5 Ultraviolet Absorbers, may be added to the exterior thickness to 3 oz/ft2 (918 g/m2) of chopped mat. Each pass of
surface for improved weather resistance when agreed upon chopped roving or ply of chopped-strand mat shall be thor-
between the fabricator and the buyer. oughly rolled out. This section of the laminate shall be allowed
5.2 Fiber Reinforcement: to exotherm prior to application of subsequent plies of rein-
5.2.1 Surfacing Mat (veil) is a thin mat of fine fibers used forcement.
primarily to produce a smooth surface on a reinforced plastic. 6.3 Continue lay-up in the sequence of plies, tabulated for
5.2.1.1 Veil shall be determined to be acceptable for the the specified laminate type. Roll each ply for thorough wet-out
service either by Test Methods C581 or D3681, or by a verified and deaeration.
case history. 6.3.1 Interruption of laminate construction for exotherm
5.2.1.2 Requirements of acceptable surface veils are: shall follow instructions noted on Table 1 and Table 2 for the
(a) Resin compatibility, particular laminate type. The final ply of reinforcement before
(b) Uniform fiber distribution, interruption for exotherm shall be 11⁄2-oz/ft2 (459-g ⁄m2) mat
(c) Single filaments (not bundled), or chopped roving equivalent. The initial ply of the following
(d) The thickness shall be a minimum of 10 mils per ply lamination shall be 11⁄2-oz/ft2 mat or chopped roving equiva-
when saturated with resin, and lent.
(e) Minimum fiber length shall be 0.5 in. 6.4 The outer surface of the fabricated laminate shall be
NOTE 10—The chemical resistance of the RTP laminate is provided by smooth and free of exposed glass fibers. The final ply shall be
the resin. In combination with the cured resin, the surfacing veil helps mat or chopped roving equivalent. A surfacing mat is not
determine the thickness of the resin-rich layer, reduces microcracking, and required unless specified. Surface resin may require the addi-
provides a nonwicking chemically resistant layer. tion of paraffin or may be sealed with overlaid film, as required
Additional desirable considerations in choosing a veil for a specific
application include: or approved by the resin producer, to ensure proper surface
(a) Drapability (surfacing veil should conform to mold shape), cure.
(b) Dry and wet tensile strength, 6.4.1 When pigmentation is specified, the pigment shall be
(c) Binder solubility (if used), incorporated only in the resin used to lay-up the final laminate
(d) Wetability,
(e) Surfacing veil shall wet-out completely without trapping air during
ply.
laminating, and 6.5 All edges of reinforcement material except surfacing
(f) Surfacing veil should not inhibit resin cure.
mat shall be lapped 1-in. (25.4-mm) minimum. Lapped edges
5.2.2 Chopped-Strand Mat, shall be “E” or “ECR” type of adjacent layers shall be staggered. Surfacing mat shall be
glass fiber, 11⁄2 oz/ft2 (459 g/m2), with sizing and binder butted together or have overlaps no more than 1⁄2 in. (12.7 mm).
compatible with the resin. Gaps are not permitted.

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7. Physical and Mechanical Properties 8.5 Hardness—Test Method D2583.
7.1 The composition and sequence requirements for Type I 8.6 Chemical Resistance—Test Method C581.
and II laminates are shown in Table 1 and Table 2. 8.6.1 Exposure tests under plant operating conditions shall
7.2 The mechanical property requirements for Type I and II employ Test Method C581 standard test laminate samples.
laminates are shown in Table 4.
NOTE 11—Thicker laminates shall not be used for such tests, as results
7.3 Physical properties of each type and grade of laminate will vary significantly compared to exposure of standard samples in Test
shall be established on flat laminates prepared under shop Method C581.
conditions. In Type II laminates the woven roving is to be laid 8.7 Surface Flame-Spread Classification—Test Method
square, and test specimens are to be cut parallel to the warp E84.
rovings.
7.3.1 Test specimens cut from fabricated equipment usually 9. Workmanship and Finish
are not parallel to warp rovings. Interpretation of mechanical
property data obtained from such specimens is discussed in 9.1 The finished laminate shall conform to visual accep-
Appendix X1. tance criteria of Table 5.

8. Test Methods 9.2 The surface exposed to the chemical environment (pro-
cess side) shall be smooth, resin-rich, and fully cured. The
8.1 Tensile Strength and Tangent Modulus of Elasticity— exterior surface shall also be fully cured.
Test Method D638.
9.2.1 The degree of cure shall be measured by a Barcol
8.1.1 Specimens shall be in accordance with Type III, Fig. 1
hardness test in accordance with Test Method D2583. At least
of Test Method D638 for all laminate thicknesses.
80 % of the random readings shall exceed at least 90 % of the
8.2 Flexural Strength and Tangent Modulus of Elasticity— resin manufacturer’s recommended hardness for the cured
Test Methods D790, Method I, Procedure A, and Table 1, 1/d resin.
= 16 to 1. 9.2.2 Potential air-inhibited, undercured surfaces (both in-
8.2.1 Specimens shall be the full thickness of the laminate terior secondary lamination and exterior non-mold surfaces)
as fabricated. shall be tested using an acetone sensitivity test. Four to five
8.2.2 The loading nose shall be applied to the inner face of drops of acetone rubbed with a finger on the laminate surface,
the laminate specimen. free of mold release, wax, dust, or dirt, until it evaporates, will
8.3 Glass Content—Test Method D2584. not result in surface softness or tackiness.
8.3.1 The residual, undisturbed glass-fiber plies from the
ignition shall be separated carefully and counted to confirm 10. Keywords
standard lay-up sequence. 10.1 contact molded; corrosion-resistant equipment; glass-
8.4 Thickness shall be measured with a ball-foot microm- fiber-reinforced; laminate; reinforced thermosetting plastic
eter. (RTP); thermoset polyester resin; thermoset vinyl ester resin

TABLE 4 Standard Laminate Properties


Calculated Thickness,A TensileB Mechanical Properties, min, psi (MPa)C
in. (mm) −6
Ultimate Stress × Modulus × 10 FlexuralD Edge CompressionE
Type
10−3 (MPa) (MPa) Ultimate Stress × Modulus × 10 −6
Ultimate Stress × 10−
10−3 (MPa) (MPa) 3
(MPa)

ALL I 9.0 0.85 16.0 0.7 16


(62) (5862) (110) (4828) (110)
0.22 (5.6) II 12.0 0.9 19.0 0.8 16
(83) (6207) (131) (5518) (110)
0.30 (7.6) II 13.5 1.1 20.0 0.9 18
(93) (7587) (138) (6207) (124)
0.37 (9.4) and up II 15.0 1.2 22.0 1.0 20
(104) (8276) (152) (6897) (138)
A
The thickness shall be not less than 90 % of the calculated thickness shown.
B
Test Method D638.
C
Barcol hardness should be 90 % (minimum) of cast resin hardness.
D
Test Method D790.
E
Test Method D695.

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TABLE 5 Visual Acceptance Criteria
Visual Observation Surface Inspected
Process Side Nonprocess Side

Cracks None None


Crazing (fine resin-rich surface cracks) None Maximum dimension 1 in. (25.4 mm). Maximum density
5/ft2 (0.1 m2).A
Blisters (rounded elevations of the None Maximum 1⁄4 -in. (6.4-mm) diameter by 1⁄8 in. (3.2 mm)
laminate surface over bubbles) high. Maximum 2/ft2 (2/0.1 m2).A
Wrinkles and solid blisters Maximum deviation, 20 % of wall thickness, but not exceeding Maximum deviation, 20 % of wall thickness, but not
1⁄8 in. (3.2 mm).A exceeding 3⁄16 in. (4.8 mm).A
Pits (craters in the laminate surface) Maximum dimensions, 1⁄8 -in. (3.2-mm) diameter by 1⁄32 in. (0.8 Maximum dimension 1⁄8 -in. (3.2-mm) diameter by 1⁄16 in.
mm) deep. Maximum number 10/ft2 (10/0.1 mm2).A (1.6 mm) deep. Maximum density 10/ft2 (10/0.1 m2).A
Surface porosity, pin holes, or pores in Maximum dimensions, 1⁄16 -in. (1.6-mm) diameter by 1⁄32 in. (0.8 Maximum dimension 1⁄16 -in. (1.6-mm) diameter by 1⁄16 in.
the laminate mm) deep. Maximum number 20/ft2 (20 ⁄0.1 m2) by 1⁄16 in. (1.6 deep. Maximum number 20/ft2 (20/0.1 m2). Must be
mm). Must be resin-rich.A resin-rich.A
Chips (small piece broken from edge or Maximum dimensions, 1⁄8 -in. (3.2-mm) diameter by 1⁄32 in. (0.8 Maximum dimension 1⁄4 -in. (6.4-mm) diameter by 1⁄16 in.
surface) mm) deep. Maximum number 1/ft2 (1/0.1 m2).A (1.6 mm) deep. Maximum number 5/ft2 (5/0.1 m2).A
Dry spot (non-wetted reinforcing) None Maximum dimensions 2 in.2 (13 cm2) per ft2 (0.1 m2).A
Entrapped air (bubbles or voids or Maximum diameter 1⁄16 in. (1.6 mm), 10/in.2 (10 ⁄6.5 cm2) Maximum diameter 1⁄16 in. (1.6 mm). 10/in.2 (10 ⁄6.5 cm2)
delaminations in the laminate) maximum density. Maximum diameter 1⁄8 in. (3.2 mm), 2/in.2 maximum density. Maximum diameter 1⁄8 in. (3.2 mm),
(2/6.5 cm2) maximum density. Maximum depth of 1⁄32 in. (0.8 2/in.2 (2/6.5 cm2) maximum density. Maximum diameter
mm).AB 3⁄16 in. (4.8 mm), 2/ft2 (2/0.1 m2). Maximum density.AB

Exposed glass None None


Burned areas None None
Exposure of cut edges NoneC NoneC
Scratches None over 0.005 in. deep and 4 in. long Maximum length 12 in. (3.5 mm). Maximum depth 0.010
in. (0.25 mm) 2/ft2 (2/0.1 m2), maximum density.A
Foreign matter None 1⁄8-in. (3.2-mm) diameter, maximum density 1/ft2 (1 ⁄0.1

m2). 3⁄16 -in. (4.8-mm) diameter, maximum density 1/ft2


(1/0.1 m2).AD
A
Maximum 5 % of total surface area affected.
B
Entrapped air or bubbles described are allowed, provided the surface cannot easily be broken with a pointed object, such as a knife blade.
C
Cut edges must be covered with resin.
D
Foreign matter must not penetrate the surface and must not contribute to entrapped air or other defects not allowed.

APPENDIXES

(Nonmandatory Information)

X1. INTERPRETATION OF DATA FROM ANISOTROPIC LAMINATES

X1.1 General—Mechanical properties of laminates contain- applied load and the direction of the roving strands. For 5 by 4
ing alternative plies of woven roving and chopped strand mat square weave roving, the approximate relationship is shown in
are dependent upon relationship between the direction of the Fig. X1.1.

X2. QUALIFICATION OF LAMINATE STRUCTURE FOR TYPE, CLASS, AND GRADE DESIGNATION

X2.1 General—The RTP laminate structures other than X2.2.1.2 Laminates having essentially unidirectional fiber
those covered by this specification may be characterized for reinforcement shall be 25 by 25-in. (635 by 635-mm) size to
designation as standard type, class, and grade by means of the provide sufficient laminate for testing in two directions.
following procedure. X2.2.1.3 The degree of cure of the surface exposed to the
chemical environment (process side) shall be measured by a
X2.2 Laminate Preparation:
Barcol hardness test in accordance with Test Method D2583.
X2.2.1 Under shop fabrication conditions, lay up 12 by At least 80 % of the random readings shall exceed at least 90 %
25-in. (305 by 635-mm) flat laminates of the proposed laminate of the resin manufacturer’s recommended hardness for the
structure in nominal thicknesses of 3⁄16, 5⁄16, 1⁄2, and 3⁄4 in. (4.8, cured resin.
8, 12.8, and 19.2 mm). X2.2.1.4 Cured laminates shall be flat within the limits of
X2.2.1.1 Orientation of reinforcing fibers of fabrics shall be 1⁄8-in./ft (3.2-mm/0.1 m2) deviation from a plane surface.
such as to produce maximum properties in the 25-in. (635-mm)
direction of the laminate. X2.3 Testing:

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Standard
Deviation
Note: At 45°, Tensile strength is 69 % of 0°. 11 %
Tensile modulus is 86 % of 0°. 2%
At 45°, Flexural strength is 62 % of 0°. 14 %
Flexural modulus is 72 % of 0°. 14 %
At 45°, Composition strength is 100 % of 0°. 11 %
Composition modulus is 73 % of 0°. 20 %

FIG. X1.1 Directional Properties of RTP Alternating Mat/Woven


Roving

X2.3.1 Tests shall be performed, and results certified, by a X2.4.1 The report shall describe laminate manufacture, date
recognized independent testing laboratory experienced in the of manufacture, resin used with batch number noted, identifi-
testing of RTP laminates. cation of reinforcements used, cure components, additives, and
X2.3.2 Determine mechanical and physical properties as all pertinent cure information.
required by Sections 7 and 8 of this specification. X2.4.2 The report shall contain the data obtained on all
X2.3.2.1 Unidirectional laminates, as described in X2.2.1.2, specimens, the laboratory that performed the tests, and the date
shall have properties determined both parallel to, and at 90° to, performed.
the direction of reinforcement.
X2.4 Report:

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D953 − 19

Standard Test Method for


Pin-Bearing Strength of Plastics1
This standard is issued under the fixed designation D953; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* D5947 Test Methods for Physical Dimensions of Solid


1.1 This test method covers the determination of the pin- Plastics Specimens
bearing strength of rigid plastics in either sheet form, molded D7290 Practice for Evaluating Material Property Character-
form, or in reinforced thermoset form. Procedures A and B are istic Values for Polymeric Composites for Civil Engineer-
applicable for thermoplastic materials in tension loading and ing Structural Applications
compression loading respectively. Procedure C is applicable E4 Practices for Force Verification of Testing Machines
for thermoset reinforced plastics. See the significance and use E177 Practice for Use of the Terms Precision and Bias in
section (Section 5) for cautions in using this test standard. ASTM Test Methods
E6 Terminology Relating to Methods of Mechanical Testing
1.2 Test data obtained by this test method is relevant and E691 Practice for Conducting an Interlaboratory Study to
appropriate for use in quality control and engineering design. Determine the Precision of a Test Method
1.3 The values stated in SI units are to be regarded as the 2.2 ISO Standards:
standard. The values given in parentheses are for information ISO 12815 Fibre-reinforced plastic composites—
only. Determination of plain-pin bearing strength3
1.4 This standard does not purport to address all of the 3. Terminology
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.1 Definitions—For definitions of technical terms used in
priate safety, health, and environmental practices and deter- this test method and associated with plastics issues refer to
mine the applicability of regulatory limitations prior to use. terminology contained in ASTM D883.

NOTE 1—This standard and ISO 12815 address the same subject matter,
3.2 Definitions of Terms Specific to This Standard:4
but differ in technical content. 3.2.1 pin-bearing area—the diameter of the hole multiplied
1.5 This international standard was developed in accor- by the thickness of the specimen.
dance with internationally recognized principles on standard- 3.2.2 pin-bearing strength—the pin-bearing stress at which
ization established in the Decision on Principles for the the pin-bearing hole is deformed 4 % of its diameter for
Development of International Standards, Guides and Recom- thermoplastics. For thermosets, the pin-bearing strength is the
mendations issued by the World Trade Organization Technical maximum pin-bearing stress at which the sample fails.
Barriers to Trade (TBT) Committee. 3.2.3 pin-bearing stress—the applied load in newtons (or
pounds-force) divided by the pin-bearing area in mm2 (or in2).
2. Referenced Documents
3.2.4 edge distance ratio—the distance from the center of
2.1 ASTM Standards:2 the pin-bearing hole to the edge of the specimen in the
D618 Practice for Conditioning Plastics for Testing direction of loading, divided by the diameter of the hole.
D883 Terminology Relating to Plastics 3.2.5 maximum pin-bearing stress—the maximum load in
newtons (or pounds-force) sustained by the specimen, divided
1
by the bearing area.
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset- 4. Summary of Test Method
ting Plastics.
Current edition approved Nov. 1, 2019. Published December 2019. Originally 4.1 This test standard is intended to test the pin-bearing
approved in 1948. Last previous edition approved in 2018 as D953 - 18. DOI: strength of thermoplastic material using procedures A, B and
10.1520/D0953-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
Standards volume information, refer to the standard’s Document Summary page on 4th Floor, New York, NY 10036, http://www.ansi.org.
4
the ASTM website. Attention is also directed to Terminology E6.

*A Summary of Changes section appears at the end of this standard


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D953 − 19
reinforced thermoset plastics using procedure C. In procedures no more than 61 % of the applied load as determined in
A and B, the sample with a pin-bearing hole will be tested in accordance with Practices E4.
tension and compression respectively. While using procedure A 6.2 Tension Loading Fixture for Procedure A—A three-plate
and B, the load at which the hole deformation reaches 4 % of fixture of hardened steel similar to that shown in Fig. 1.
hole diameter, that load shall be considered as maximum
pin-bearing load to calculate the pin-bearing strength. In 6.3 Extension Indicator—A suitable instrument reading in
procedure C, the sample shall be tested in compression and the 0.0025 mm (0.0001 in.) for indicating the movement of the free
maximum failure load of the sample shall be used as maximum end of the specimen with relation to the bearing pin in the
pin-bearing load to calculate the pin-bearing strength. As tension loading fixture. A dial gauge fitted with accessories for
reinforced thermoset plastics are much stiffer than this purpose is shown in Fig. 2.
thermoplastics, the pin-bearing failure happens much before 6.4 Compression Loading Fixture for Procedure B—A type
the hole deformation reaches 4 % of the hole diameter. Using of support with a suitable bearing pin similar to Fig. 3.
procedure C, it is allowed to test reinforced thermoset samples 6.5 Compression Indicator—A suitable instrument reading
with over-sized holes for any engineering design purposes. to 0.0025 mm (0.0001 in.) for indicating the movement of the
Using the maximum pin-bearing load obtained by using an free end of the specimen with relation to the bearing pin in the
appropriate procedure, the pin-bearing strength of the material compression loading fixture. A schematic of the dial gauge
will be determined. assembly for this purpose is shown in Fig. 4.
5. Significance and Use 6.6 Compression Loading Fixture for Procedure C—The
fixture as shown in Fig. 5 (A) is made up of two properly
5.1 This pin-bearing strength test for plastics is intended to aligned steel angle uprights welded to a steel base plate. The
apply in the specification of various thermoplastic or thermo- welding of the angle uprights has to be on the outside only and
setting products in sheet form where rivets, bolts, or similar not for the surfaces against which the specimen makes contact
fastenings are to be used in joining members or sections. It also
is intended to apply wherever sheet materials of the classes
indicated are required to sustain edgewise loads that are
applied by means of pins or rods of circular cross section which
pierce the sheet perpendicular to the surface.
5.2 The purpose of the test using procedures A and B is to
determine the pin-bearing strength of thermoplastic material
and to plot the pin-bearing stress versus the deformation of the
hole. The allowable deformation of the hole in the material
shall be such as to produce no looseness of joints.
5.3 The purpose of procedure C is to determine the ultimate
pin-bearing strength of reinforced thermoset material. This test
procedure enables the user to test the part in any direction that
is intended to carry the pin-bearing loads. The sample size used
in this procedure will cover thermoset reinforced plastics that
are commonly used in infrastructure applications.
5.4 While it is a known fact that higher strength materials 1—Hardened spacer plate.
2—6.3-mm (-in.) steel bolts in reamed holes.
will generally give higher bearing strengths, there is no 3—Hardened side plate.
satisfactory method to estimate pin-bearing strength from 4—Extensometer span.
tensile or compressive properties of the material. 5—Hardened steel pin in reamed hole.
6—Test specimen.
5.5 Before proceeding with this test method, reference shall
be made to the specification of the material being tested. Any
test specimen preparation, conditioning, dimensions or testing NOTE 1—Critical dimensions are as follows:
Thickness of
parameters or combination thereof covered in the relevant Type
Bearing Hole Bearing Pin Diameter, mm
Spacer Plate,
Diameter, mm (in.) (in.)
ASTM materials specification shall take precedence over those mmA (in.)
in this test method. If there are no relevant ASTM material I 3.175 + 0.025 3.150 + 0.000 3.2
− 0.000 − 0.025
specifications then the default conditions apply. (0.125 + 0.0010 (0.124 + 0.0000 (1⁄8 )
− 0.0000) − 0.0010)
6. Apparatus II 6.350 + 0.025 6.325 + 0.000 6.3
− 0.000 − 0.025
6.1 Testing Machine—A properly calibrated universal test- (0.250 + 0.0010 (0.249 + 0.0000 (1⁄4 )
− 0.0000) − 0.0010)
ing machine that is capable to be operated at a speed of 1.3 6 A
The spacer plate shall be shimmed to a thickness of 0.025 to 0.125 mm (0.001
0.3 mm (0.05 6 0.01 in.)/min, except that in cases of certain to 0.005 in.) greater than the specimen under test.
types of materials where it is necessary to operate at a slower
speed. The percentage of error of the testing machine shall be FIG. 1 Steel Tension Loading Fixture

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D953 − 19

1—Test specimen.
2—Hardened steel pin.
3—Hardened thrust bushing.

NOTE 1—Critical dimensions are as follows:


Minimum
Clear-
Bearing Hole
Bearing Pin Diameter, ance Be-
Type Diameter,
mm (in.) tween
mm (in.)
Bushings,
mm (in.)
I 3.175 + 0.025 3.150 + 0.000 2.8
− 0.000 − 0.025
(0.125 + 0.0010 (0.124 + 0.0000 (7/64)
− 0.0000) − 0.0010)
II 6.350 + 0.025 6.325 + 0.000 6.0
− 0.000 − 0.025
(0.250 + 0.0010 (0.249 + 0.0000 (15/64)
− 0.0000) − 0.0010)

FIG. 3 Steel Compression Loading Fixture


1—Spacer plate.
2—Dial gauge.
3—Double foot ring mounted on spindle of dial gauge.
4—Bearing pin.
5—Yoke mounted on specimen.
6—Test specimen. 7.2 The test specimens for procedure C shall conform to the
7—Plan view of yoke. dimensions shown in Fig. 7. The test specimen shall be a 76.2
mm by 76.2 mm (3 in. by 3 in.) sample machined from a part
FIG. 2 Tension Loading Assembly
that mostly nearly conforms to the production requirements of
the material under consideration. The specimen shall be clearly
marked to identify the orientation of the material. The pin-
bearing hole shall be located at a distance of 15.88 mm (0.625
with so the sample can be supported flush to the surface of the
in.) from the one edge of the sample in the direction of the
angle and align without any angularity. This fixture will
loading. The hole shall be drilled undersized and reamed to size
support and align the sample normal to the loading ram. It is
as indicated in Fig. 7. The hole shall be clean and smooth with
allowed to use C-clamps to provide lateral support to the
sharp edges but not polished. The reaming operation shall be
sample against the fixture as shown in Fig. 5 (B). For quality
done in the drill press by hand without the use of a jig. The
assurance purposes, the nominal bearing pin diameter shall be
sample with pin-bearing hole shall be carefully machined at the
the same as the thickness of the sample.
mid-section of the hole to present half of the hole as shown in
Fig. 7.
7. Test Specimens
7.1 The test specimens for Procedures A and B shall 7.3 The dimensions given in Fig. 7 applies to holes up to
conform to the dimensions shown in Fig. 6. A size of test 25.4 mm (1 in.). For pin-bearing holes bigger than 25.4 mm (1
specimen shall be chosen that most nearly conforms to in.) an edge distance (B) of 3 times the diameter of the
production requirements of the material and the type of loading pin-bearing pin shall be considered.
under consideration. It is permitted to machine the specimen 7.4 Oversized Holes for Engineering Designs—To deter-
from sheet or molded to finished size. The bearing hole shall be mine the pin-bearing strength of oversized holes for engineer-
located as shown in Fig. 6. It shall be drilled undersized and ing design purpose, it is allowed to use the compression fixture
reamed to size as indicated. The hole shall be clean and smooth and the compression sample, prepared as described in 7.2
with sharp edges but not polished. The reaming operation shall except that it is not required to clean or ream the hole. While
be done in the drill press by hand without the use of a jig. determining the pin-bearing stress of an oversized hole, note
NOTE 2—The thicker specimens with the larger pin-bearing hole are
likely to give the more precise results, although it is advantageous to use that the values obtained for a particular combination of hole
the thinner specimens with the smaller pin-bearing hole in testing certain size, pin size, thickness, and material is acceptable only for that
relatively brittle plastics because they are less likely to fail prematurely. combination.

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D953 − 19

1—Test specimen. 6—Dial gauge.


2—Bearing pin. 7—Pedestal support.
3—Thrust bushings. 8—Clamp for cheek blocks.
4—Hanger for dial gauge. 9—Hard maple cheek blocks to stabilize test specimen.
5—Spring-supported thrust member of transfer deforma-
tion of specimen to dial gauge foot.

FIG. 4 Compression Loading Assembly

FIG. 5 Compression Loading Fixture for Procedure C (With Picture of Sample Under Pin-Bearing Load)

8. Number of Test Specimens 8.2 Ten specimens, five perpendicular to and five parallel
8.1 At least five specimens shall be tested for each sample in with the principal axis of anisotropy, shall be tested for each
the case of isotropic materials. sample in case of anisotropic materials.

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D953 − 19

Type Dimensions, mmA (in.) Ream Hole


A B C D to

I 11.913 ± 0 .127 19.050± 0 .127 120.6 3.2 3.200 ± 0 .025


(0.469 ± 0 .005) (0.750 ± 0 .005) (43⁄4 ) (1⁄8 ) (0.126 ± 0 .001)
II 11.913 ± 0 .127 19.050 ± 0 .127 120.6 6.4 6.375 ± 0 .025
(0.469 ± 0 .005) (0.750 ± 0 .005) (43⁄4 ) (1⁄4 ) (0.251 ± 0 .001)

A
All fractional dimensions shall be held to ±0.40 mm (1⁄64 in.) tolerance.

Edge distance ratio = B/hole diameter

FIG. 6 Dimensions of Pin-Bearing Strength Test Specimens

Dimensions, mm (in.)
A B Ream Hole to
76.2 ± 1.588 14.732 ± 0.0635 D ± 0.0635
(3 ± 0.0625) (0.625 ± 0.0025) (D ± 0.0025)

FIG. 7 Dimensions of Compression Pin-Bearing Samples for Procedure C

NOTE 3—If the intent of the testing is to obtain the characteristic value ture and humidity tolerances shall be in accordance with
in accordance with Practice D7290, the sample numbers have to be a Section 7 of Practice D618 unless specified differently by
minimum of ten samples per direction of principal axis.
contract or material specification.
8.3 Specimens that break at some obvious flaw that is not
naturally formed by the material processing method shall be 9.2 Test Conditions—Conduct tests at the same temperature
discarded and retests made, unless such flaws constitute a and humidity used for conditioning with tolerances in accor-
variable the effect of which is being studied. dance with Section 7 of Practice D618 unless otherwise
specified by contract or the relevant ASTM material specifica-
9. Conditioning tion.
9.1 Conditioning—Condition the test specimens in accor-
10. Measurement of Dimensions
dance with Procedure A of Practice D618, unless otherwise
specified by contract or the relevant ASTM material specifica- 10.1 Measure the width and thickness of the conditioned
tion. Conditioning time is specified as a minimum. Tempera- test specimen to the nearest 0.025 mm (0.001 in.) at the bearing

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D953 − 19
hole. Also, measure the pin diameter, diameter of the pin- until the maximum load is recorded. Record load vs. position
bearing hole and the distance from the center of the pin-bearing readings throughout the test.
hole to the edge of the specimen in the direction of the
principal stress to the nearest 0.025 mm (0.001 in.). All 13. Calculation
measurements to be made using the applicable test methods in 13.1 Plot the load - deflection curve for each specimen.
accordance with Test Method D5947.
13.2 For Procedures A and B, use a template as described in
the Appendix to determine the load at 4 % hole deformation.
11. Speed of Testing
For Procedure C, use the ultimate (maximum) load for pin-
11.1 The mean rate of crosshead travel in the testing of bearing strength calculations.
specimens shall not exceed 1.3 6 0.3 mm (0.05 6 0.01 13.3 Calculate the pin-bearing strength as follows:
in.)/min. In any case the crosshead movement shall be slow
enough so that deflection gauge readings can be made accu- S b 5 P/ ~ td! (1)
rately. where:
Sb = pin-bearing strength, MPa (or psi),
12. Procedure P = pin-bearing load at 4 % hole deformation for thermo-
12.1 The choice of either Procedure A for tension loading plastics using Procedure A and B, N (or lbf). Use
(12.2) or Procedure B for compression loading (12.3) is maximum load for reinforced thermoset plastics, N (or
optional, but note that Procedure B gives higher pin-bearing lbf).
strength values than Procedure A on the same material. Test d = pin-bearing hole diameter, mm (or in.), and
specimens according to both Procedures A and B if a complete t = specimen thickness, mm (or in.).
specification of pin-bearing strength is required. 13.4 Calculate the arithmetic mean of the observations and
12.2 Procedure A for Tension Loading—Mount the speci- report the result to three significant figures.
men to be tested in the tension loading fixture and attach a 13.5 Calculate the standard deviation of each batch of test
deformation indicator. If a dial gauge (Fig. 2) is used, adjust the results and record to two significant figures.
yoke so that contact is made with the specimen at the level
indicated in Fig. 1. Exception is taken in the case of those 14. Report
thermoplastic materials which exhibit extended plastic flow. 14.1 Report the following information:
Such specimens tend to “neck down” in the region of the 14.1.1 Complete identification of the material tested, includ-
pin-bearing hole, and it is necessary to mount the yoke 12.7 ing type, source, manufacturer’s code number, form, principal
mm (1⁄2 in.) below the normal position indicated in A, Fig. 1, so dimensions, and previous history,
that it will not slip during test. 14.1.2 Direction of cutting and loading specimens,
12.3 Procedure B for Compression Loading—Mount the 14.1.3 Conditioning procedure and environmental condi-
specimen to be tested in the compression loading fixture and tions under which the tests were conducted,
load through a flat, hardened compression plate. Adjust the 14.1.4 Length, width, and thickness of specimen, in milli-
clearance between the thrust bushings of the loading fixture metres (or inches),
such that their contact with the specimen is sufficient to support 14.1.5 Diameter of pin and diameter of pin-bearing hole, in
it in a vertical position without binding. Clamp the hardwood millimetres (or inches),
cheek blocks in place and attach the deformation indicator (see 14.1.6 Edge distance ratio,
Fig. 4). 14.1.7 Mean rate of crosshead motion in millimetres (or
inches) per minute,
12.4 Details Common to Procedures A and B—Take care in 14.1.8 Pin-bearing strength in Megapascals (or pounds-
aligning the long axis of the specimen with the center line of force per square inch), stating whether Procedure A for tension
the testing fixture. Load the specimen at the prescribed rate of loading or Procedure B for compression loading for thermo-
crosshead travel and take deformation readings. In case auto- plastic materials or Procedure C for reinforced thermoset
graphic recording is not available, record the load sustained by plastics was used,
the specimen for every 0.0127-mm (0.0005-in.) deformation 14.1.9 Average pin-bearing stress in Megapascals (or
up to a total deformation of 4 % of the pin-bearing hole pounds-force per square inch), stating whether Procedure A or
diameter. Continue the test until maximum load is sustained Procedure B or Procedure C was used,
and the corresponding deformation of the pin-bearing hole is 14.1.10 The test method number and published/revision
recorded. date.
12.5 Procedure C for Compression Loading—Mount the
specimen to be tested in the steel compression fixture against 15. Precision and Bias
the steel angle uprights as shown in Fig. 5. Clamp the sample 15.1 The precision of this test method is based on an
to the fixture to keep it in place during the testing. Place the intralaboratory study of ASTM D953—Test Method for Bear-
bearing pin in the half-circle of the specimen and center this ing Strength of Plastics using Procedure C, conducted in 2018.
assembly under the flat platen attachment of the test machine. A single laboratory participated in this study, testing a single 3⁄8
Load the specimen at the prescribed rate of crosshead travel in. pultruded material. Every “test result” represents the

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D953 − 19
average of ten individual determinations. The laboratory re- TABLE 2 Average Bearing Stress (psi)
ported three replicate test results for the study material in both Material Average Repeatability Repeatability
the crosswise and lengthwise direction. Except for the use of Standard Limit
Deviation
only one laboratory and one material, Practice E691 was x̄ Sr r
followed for the design and analysis of the data; the details are ⁄ in. Pultruded
38 41 733 666 1864
given in ASTM Research Report No. D20-1273.5 Material
(Lengthwise)
15.1.1 Repeatability Limit (r)—The difference between re- 3⁄8 in. Pultruded 34 267 473 1323
petitive results obtained by the same operator in a given Material
(Crosswise)
laboratory applying the same test method with the same
apparatus under constant operating conditions on identical test 15.1.2.1 Reproducibility can be interpreted as maximum
material within short intervals of time would in the long run, in difference between two results, obtained under reproducibility
the normal and correct operation of the test method, exceed the conditions, that is accepted as plausible due to random causes
following values only in one case in 20. under normal and correct operation of the test method.
15.1.1.1 Repeatability can be interpreted as maximum dif- 15.1.2.2 Reproducibility limits cannot be calculated from a
ference between two results, obtained under repeatability single laboratory’s results.
conditions, that is accepted as plausible due to random causes 15.1.3 The above terms (repeatability limit and reproduc-
under normal and correct operation of the test method. ibility limit) are used as specified in Practice E177.
15.1.1.2 Repeatability limits are listed in Tables 1 and 2. 15.1.4 Any judgment in accordance with statement 15.1.1
15.1.2 Reproducibility Limit (R)—The difference between would normally have an approximate 95 % probability of
two single and independent results obtained by different being correct, however the precision statistics obtained in this
operators applying the same test method in different laborato- ILS must not be treated as exact mathematical quantities which
ries using different apparatus on identical test material would, are applicable to all circumstances and uses. The limited
in the long run, in the normal and correct operation of the test number of laboratories reporting replicate results essentially
method, exceed the following values only in one case in 20. guarantees that there will be times when differences greater
TABLE 1 Average Bearing Stress (MPa) than predicted by the ILS results will arise, sometimes with
Material Average Repeatability Repeatability
considerably greater or smaller frequency than the 95 %
Standard Limit probability limit would imply. Consider the repeatability limit
Deviation as a general guide, and the associated probability of 95 % as
x̄ Sr r
⁄ in. Pultruded
38 287.74 4.59 12.85
only a rough indicator of what can be expected.
Material 15.2 Bias—At the time of the study, there was no accepted
(Lengthwise)
3⁄8 in. Pultruded 236.26 3.26 9.13
reference material suitable for determining the bias for this test
Material method, therefore no statement on bias is being made.
(Crosswise)
15.3 The precision statement was determined through sta-
tistical examination of 12 test results, from a single laboratory,
one 3⁄8 in. pultruded material.
5
Supporting data have been filed at ASTM International Headquarters and may 16. Keywords
be obtained by requesting Research Report RR:D20-1273. Contact ASTM Customer
Service at service@astm.org. 16.1 compression strength; pin-bearing strength; plastics

APPENDIX

(Nonmandatory Information)

X1. DETERMINATION OF PIN-BEARING LOAD USING PROCEDURES A AND B

X1.1 Pin-bearing strength has been defined as the pin- through the point, O, on the zero load axis, the distance
bearing stress at which the pin-bearing hole is deformed a betweenOandDshall be equal to 4 % of the bearing hole
given percentage (4 %) of the hole diameter, and is by diameter.
definition, sensitive to zero load errors. The following proce-
dure for determining pin-bearing strength has been found to X1.3 A template to facilitate the determination of point Bon
eliminate this ambiguity. It is insensitive to zero load errors, the curve is shown in Fig. X1.2. It is designed to fit the
and as a result improves the precision of the pin-bearing coordinate paper upon which the load-deformation curve is
strength measurements. drawn in such a way that a “4 % line” on the template is
established at a distance from the origin, O, equal to 4 % of the
X1.2 The method is best illustrated by Fig. X1.1. Given the pin-bearing hole diameter. It consists of a thin rigid sheet of
pin-bearing load − deflection curve, ABC, the tangent is deter- transparent plastic upon which the rectangular coordinates are
mined at a point, B, such that when the tangent is projected ruled. A strip of transparent plastic is mounted on the sheet so

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D953 − 19

FIG. X1.2 Template for Determining Point Bon Pin-Bearing Load-


FIG. X1.1 Illustration of Method of Determining Pin-Bearing
Deformation Curve
Strength from Pin-Bearing Load-Deformation Curve

as to rotate about point O. The strip is provided with a and a parallel straightedge. The template is then slid to right or
reference center line passing through the point of rotation. left while in superposition until the rotating arm can be made
tangent to the load-deformation curve at its intersection with
X1.4 In practice, the deformation axis of the template is the 4 % line. The intersection is the point Bon the curve in Fig.
superimposed on the zero load axis of the load-deformation X1.1; Bis projected horizontally to the load axis and the
curve. This can best be done with the aid of a drawing board pin-bearing load is read.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D953 - 18)
that may impact the use of this standard. (November 1, 2019)

(1) Changed the sentence in 6.6: The nominal bearing pin


diameter shall be the same as the thickness of the sample to
“For quality assurance purposes, the nominal bearing pin
diameter shall be the same as the thickness of the sample”.

Committee D20 has identified the location of selected changes to this standard since the last issue (D953 - 10)
that may impact the use of this standard. (November 1, 2018)

(1) Changed the title of the standard to “Standard Test Method (3) Changed language at several locations in accordance with
for Pin-Bearing Strength of Plastics.” ASTM D4968-17.
(2) Added Procedure C to the scope of the test standard to
include a test procedure for reinforced thermoset plastics

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of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D1494 − 17 An American National Standard

Standard Test Method for


Diffuse Light Transmission Factor of Reinforced Plastics
Panels1
This standard is issued under the fixed designation D1494; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* E2935 Practice for Conducting Equivalence Testing in


1.1 This test method covers the determination of the diffuse Laboratory Applications
light transmission factor of translucent reinforced plastics E691 Practice for Conducting an Interlaboratory Study to
building panels. Determine the Precision of a Test Method
2.2 ASTM Adjuncts:
1.2 The values stated in SI units are to be regarded as the
Test Cabinet for Diffuse Light Transmission Factor of
standard. The values given in the parentheses are for informa-
Reinforced Panels3
tion only.
1.3 The text of this standard references notes and footnotes 3. Terminology
which provide explanatory material. These notes and footnotes
3.1 General—Definitions are in accordance with Terminol-
(excluding those in Tables and Figures) shall not be considered
ogy D883 and abbreviations with Terminology D1600, unless
as requirements of this standard.
otherwise indicated.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Significance and Use
responsibility of the user of this standard to establish appro-
4.1 The purpose of this test method is to obtain the diffuse
priate safety, health, and environmental practices and deter-
light transmittance factor of both flat and corrugated translu-
mine the applicability of regulatory limitations prior to use.
cent building panels by the use of simple apparatus and by
NOTE 1—There is no known ISO equivalent to this standard. employing as a light source a combination of fluorescent tubes
1.5 This international standard was developed in accor- whose energy distribution closely approximates CIE Source C.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 5. Apparatus
Development of International Standards, Guides and Recom- 5.1 The apparatus for this test method shall consist of a
mendations issued by the World Trade Organization Technical transmissometer, Fig. 1, comprising essentially the following:
Barriers to Trade (TBT) Committee. 5.1.1 Light Source—The illumination shall consist of twelve
20-W fluorescent tubes which are assembled in three banks of
2. Referenced Documents four tubes each, according to the following schedule: daylight,
2.1 ASTM Standards:2 deluxe cool white, blue, and daylight.
D618 Practice for Conditioning Plastics for Testing 5.1.2 Photometer—The photometer shall consist of a pho-
D883 Terminology Relating to Plastics tocell and of a galvanometer. The photocell shall be of the
D1600 Terminology for Abbreviated Terms Relating to Plas- barrier-layer type and shall contain a visual correction filter.
tics The assembly preferably should be hermetically sealed into
plastic as a protection against moisture. The indicating galva-
1
nometer should contain one scale graduated from 0 to 100, and
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.24 on Plastic Building
a circuit with sufficient variable resistance so that the sensitiv-
Products. ity of the photometer can be adjusted over the range of 50 to
Current edition approved Dec. 1, 2017. Published January 2018. Originally 100 footcandles.
approved in 1957. Last previous edition approved in 2012 as D1494 – 12. DOI:
10.1520/D1494-17.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Detailed working drawings and a bill of materials for this equipment can be
Standards volume information, refer to the standard’s Document Summary page on obtained at a nominal charge from ASTM Headquarters, 100 Barr Harbor Drive, PO
the ASTM website. Box C700, West Conshohocken, PA 19428–2959. Order Adjunct: ADJD1494.

*A Summary of Changes section appears at the end of this standard


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D1494 − 17

Metric Equivalents
in. mm in. mm in. mm in. mm

1 32 0.8 ⁄
34 19.1 83⁄4 222 243⁄4 634
3⁄16 4.8 11⁄4 31.8 93⁄4 248 251⁄2 648
7⁄37 5.6 11⁄2 38.1 12 305 28 711
1⁄ 4 6.4 2 50.8 14 356 291⁄2 749
9⁄32 7.1 63⁄4 172 24 610 381⁄2 978
3⁄ 8 9.5

FIG. 1 Assembly Drawing of Transmissometer

5.1.3 Test Cabinet, constructed in accordance with the bottom of the test specimen to the bottom of the masking plate
following dimensions.3 shall be 233.0 6 0.8 mm (93⁄4 6 1⁄32 in.).
5.1.3.1 The transmitted area of the test specimen shall be
610.0 6 1.6 mm by 610.0 6 1.6 mm (24 6 1⁄16 in. by 24 6 6. Standardization of Transmissometer
1⁄16 in.).
6.1 Center the photocell beneath the 31.8-mm (11⁄4-in.)
5.1.3.2 The distance from the bottom of the fluorescent
diameter hole in the bottom masking plate. Place the galva-
tubes to the bottom of the test specimen shall be 203.0 6 0.8
nometer in a flat level position. Ensure that no current flows in
mm (8 6 1⁄32 in.).
the electrical circuit by opening the circuit. Adjust the position
5.1.3.3 A 4.8-mm (3⁄16-in.) thick, white, standard outdoor,
of the indicating needle on the galvanometer to read “0’’ by
translucent diffusing plate shall be placed between the light
means of the zero adjustment knob. Close the galvanometer
source and the test specimen so that the distance from the
circuit. Turn on the illumination in the transmissometer. Wait a
bottom of the diffusing plate to the bottom of the test specimen
minimum of 20 min to permit the transmissometer to reach
is 31.8 6 0.8 mm (11⁄4 6 1⁄32 in.).
equilibrium conditions. Adjust the galvanometer to read “100.”
5.1.3.4 The photocell shall be positioned below the center
The instrument is now ready to be used for measurements of
axis of the test specimen so that the distance from the bottom
diffuse light transmission factor.
of the specimen to the top of the cell is 283.0 6 0.8 mm
(111⁄8 6 1⁄32 in.).
7. Test Specimens
5.1.3.5 A masking plate containing a 31.8-mm (11⁄4-in.)
diameter hole in its center shall be placed between the test 7.1 The test specimens shall consist of translucent rein-
specimen and the photocell so that the distance from the forced plastic panels having a minimum length of 610 mm (24

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D1494 − 17
TABLE 1 Precision Values in the Units of Percent
Material Average SrA SRB IrC IRD
Sample #4 6.1 0.36 1.08 1.02 3.06
Sample #5 24.1 0.59 2.48 1.67 7.02
Sample #1 59.7 0.45 5.01 1.27 14.18
Sample #3 73.0 0.76 3.19 2.16 9.03
Sample #2 95.6 0.64 1.61 1.81 4.56
A
Sr is the within-laboratory standard deviation of the average.
B
SR is the between-laboratory standard deviation of the average.
C
Ir = 2.83 Sr; and
D
IR = 2.83 SR.

in.) and a width greater than 610 mm (24 in.), but not to the seven participating laboratories. Each test result is an
exceeding 711 mm (28 in.). individual determination. Each laboratory obtained three test
results for each material.
8. Conditioning
NOTE 2—The explanation of Ir and IR (11.2 through 11.2.3) are only
8.1 Conditioning—Condition the test specimens at 23 6 intended to present a meaningful way of considering the approximate
2°C (73 6 4°F) and 50 6 10 % relative humidity for not less precision of this test method. The data in Table 1 should not be vigorously
than 40 h prior to test in accordance with Procedure A of applied to acceptance or rejection of materials as these data specific to the
Practice D618, for those test methods where conditioning is round robin and may not be representative of other lots, conditions,
materials, or laboratories.
required. In cases of disagreement, the tolerances shall be
61°C (62°F) and 65 % relative humidity. 11.1.1 Users of this test method should apply the principles
outlined in Practice E691 to generate data specific to their
8.2 Test Conditions—Conduct tests in the Standard Labora- laboratory and materials or between specific laboratories. The
tory Atmosphere of 23 6 2°C (73 6 4°F) and 50 6 10 % principles of 11.2 through 11.2.3 then would be valid for such
relative humidity, unless otherwise specified in the test meth- data.
ods or in this specification. In cases of disagreement, the
tolerances shall be 61°C (62°F) and 65 % relative humidity. 11.2 Concept of Ir and IR—If Sr and SR have been
calculated from a large enough body of data, and for test
9. Procedure results that are the individual result from testing one specimen:
9.1 In making a measurement, place the test specimen in the 11.2.1 Ir: Repeatability The value below which the absolute
test cabinet so that it completely covers the 610 by 610-mm (24 difference between two individual test results obtained under
by 24-in.) space. The transmittance is read on the galvanometer repeatability conditions is likely to be expected to occur with a
in percent. probability of approximately 0.95 (95 %).
11.2.2 IR: Reproducibility The value below which the
10. Report absolute difference between two individual test results obtained
10.1 The report shall include the following: under reproducibility conditions is likely to be expected to
10.1.1 The source and identity of test specimens. occur with a probability of approximately 0.95 (95 %).
10.1.2 The percent transmission of the test specimen. 11.2.3 Equivalence testing on numerical data from two
10.1.3 The average thickness of the test specimen in inches sources shall be conducted in accordance with Practice E2935
expressed to the nearest 0.025 mm (0.001 in.) and comprising or any known method for judging the equivalence of two
at least ten individual measurements. means.
NOTE 3—Example, a t-test.
11. Precision and Bias4
11.3 Bias is systematic error which contributes to the
11.1 Table 1 is based on a round robin conducted in 1987 in difference between a test result and a true (or reference) value.
accordance with Practice E691, involving five materials tested There are no recognized standards on which to base an estimate
by seven laboratories. Because of the nonuniform nature of of bias for this test method.
large corrugated sheets, the five samples were sequentially sent
12. Keywords
4
Supporting data are available from ASTM Headquarters. Request RR:D20- 12.1 building panels; diffuse light transmission factor; rein-
1145. forced plastics

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D1494 − 17
SUMMARY OF CHANGES

Committee D20 has identified the location of the following changes to this standard since the last issue
(D1494-12) that may impact the use of this standard. (December 1, 2017)

(1) Revised 2.1, added reference to E2935. (4) Revised 11.2.1, 11.2.2, 11.2.3, new rewording.
(2) Revised 8.1 and 8.2, changed 6 2% to 5% per D618-13. (5) Added Note 3.
(3) Revised 8.2, corrected °C to °F.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D2143 − 15

Standard Test Method for


Cyclic Pressure Strength of Reinforced, Thermosetting
Plastic Pipe1
This standard is issued under the fixed designation D2143; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 3. Terminology
1.1 This test method covers the determination of the failure 3.1 Definitions of Terms Specific to This Standard:
characteristics of reinforced plastic pipe when subjected to 3.1.1 failure—the transmission of the test fluid through the
cyclic internal hydraulic pressure. It is limited to pipe in which pipe wall in any manner, whether it be wall fracture, localized
the ratio of outside diameter to wall thickness is 10:1 or more. leaking, or weeping at a distance greater than one diameter
from the end closure (specimens failing within one diameter of
1.2 The values stated in inch-pound units are to be regarded
the end closure shall be discarded).
as the standard. The values in parentheses are for information
only. 3.1.2 failure detector—a devise that measures the electrical
resistance between the test fluid and a conductive material,
1.3 This standard does not purport to address all of the wrapped around the circumference of the test specimen, and
safety concerns, if any, associated with its use. It is the which will indicate failure when 1) the resistance is lowered to
responsibility of the user of this standard to establish appro- a range from 10 to 20 meg-ohm or 2) for the case of municipal
priate safety, health, and environmental practices and deter- water, when the first drop of fluid has passed through the wall
mine the applicability of regulatory limitations prior to use. of the specimen.
NOTE 1—There is no known ISO equivalent to this standard. 3.1.3 localized leaking—failure that occurs as small frac-
1.4 This international standard was developed in accor- tures (one or more in a test specimen) that permit the test fluid
dance with internationally recognized principles on standard- to be transferred at a rate that is measured by the failure
ization established in the Decision on Principles for the detector.
Development of International Standards, Guides and Recom- 3.1.4 weeping—a general transmission of the test fluid
mendations issued by the World Trade Organization Technical through the pipe, without visible fracture, at a sufficient rate to
Barriers to Trade (TBT) Committee. be measured by the failure dectector, or in the case of larger
magnitudes of fluid transmission appear to be moisture con-
2. Referenced Documents densation on the specimen.
2.1 ASTM Standards:2 3.1.5 wall fracture—failure by a break in the pipe wall
D618 Practice for Conditioning Plastics for Testing causing immediate loss of test fluid and continued loss at
D2992 Practice for Obtaining Hydrostatic or Pressure De- essentially no pressure.
sign Basis for “Fiberglass” (Glass-Fiber-Reinforced
Thermosetting-Resin) Pipe and Fittings 4. Summary of Test Method
D3567 Practice for Determining Dimensions of “Fiberglass” 4.1 This test method consists of exposing pipe specimens to
(Glass-Fiber-Reinforced Thermosetting Resin) Pipe and cyclic internal pressures at several different pressure levels and
Fittings measuring the cycles to failure at these different levels. Test
temperatures are obtained by circulating salt water or munici-
pal water through the specimens.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
5. Significance and Use
and is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic
Piping Systems and Chemical Equipment. 5.1 The values obtained by this test method are applicable
Current edition approved May 1, 2015. Published June 2015. Originally
only to conditions that specifically duplicate the procedures
approved in 1963. Last previous edition approved in 2010 as D2143 – 00(2010).
DOI: 10.1520/D2143-15. used.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.2 After the regression characteristics of a pipe material
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on and manufacturing process have been determined by this test
the ASTM website. method, one pressure may be used for quality-control purposes.

*A Summary of Changes section appears at the end of this standard


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D2143 − 15
This pressure shall be one of the points used in the original an accumulator which acts as a fluid separator transferring the
determination and be agreed upon between the individuals pressurizing medium to the salt solution or municipal water.
concerned. The solenoid is operated with equal on and off times by an
5.3 This test method deals with cyclic internal pressure electric pulsator.
performance of a pipe and omits creep and nonrecoverable 6.1.2 Test Fluid—The test fluid shall be a 2 % aqueous
deformation measurements. sodium chloride solution when salt water or municipal water is
used.
5.4 For determination of the cyclic hydrostatic design basis 6.1.3 Temperature Bath—A thermostatically controlled bath
using data from this test method see Practice D2992. coupled into the test fluid, which maintains specimen tempera-
5.5 In the application of the following test requirements and ture to within 65°F (62°C). The circulation of this fluid is
recommendations it is assumed that test specimens of a given pumped on the off portion of the pressure cycle.
sample of pipe are truly representative of that material and 6.1.4 Pressure Gages—Pressure gages having a precision of
manufacturing process. In tests conducted to show the effect of not less than 1 % of full-scale deflection with a maximum
temperature and pressures on the life span of the pipe, great indicating hand. The pressure gage shall be selected such that
care must be taken to ensure that the specimens being tested are the final readings are in the mid-60 % range of the scale. The
representative of the group being studied. Departure from this gage should be equipped with a surge protection device.
assumption could introduce discrepancies that are greater than 6.1.5 Specimen Fittings—Any suitable closure that allows
those introduced by departure from the details of the procedure free end mounting, and does not contribute to end failures may
outlined in this test method. be used.
6.1.6 Specimen Support—Any support is acceptable as long
6. Apparatus as it does not contribute to the restraint of the specimen in
6.1 A schematic diagram of the apparatus is shown in Fig. 1 either the circumferential or axial direction.
and shall consist of the following: 6.1.7 Cycle Counter and Failure Detector—Each group of
6.1.1 Pressurizing System—A device capable of exerting specimens shall be outfitted with a cyclic counter and a failure
cyclic internal pressure of the salt water or municipal water to detector which automatically stops the cyclic count when the
the test specimens. Fig. 1 shows an oil pump leading to a specimen has failed.
four-way solenoid-operated valve which directs the fluid alter-
nately to the two pressure legs, each of which contains a 7. Test Specimens
spring-operated, manually adjustable, pressure relief valve and 7.1 Sample Size—See Practice D2992.

FIG. 1 Schematic Drawing of Cyclic Pressure Apparatus

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D2143 − 15
7.2 Specimen Size—For pipe sizes of 6 in. (150 mm) or less, 9.7 After each specimen fails, record the failure count as
the specimen length between the end closures shall be not less indicated by the failure detector.
than five times the outside diameter of the pipe, but in no case
10. Calculation
less than 12 in. (300 mm). For larger sizes, the minimum length
shall be not less than three times the outside diameter, but in no 10.1 Calculate the hoop stress in the pipe specimen as
case less than 30 in. (760 mm). follows:
7.3 Measurement of Dimensions—The physical dimensions S 5 P ~ D 2 t ! /2t
of the pipe shall be measured in accordance with Practice where:
D3567.
S = hoop stress, psi (MPa),
P = internal pressure, psi (MPa),
8. Conditioning D = average outside diameter, in. (mm), and
8.1 Precondition all specimens in the standard laboratory t = minimum wall thickness, in. (mm).
atmosphere as specified in Practice D618. 10.2 For the statistical calculation method, see Practice
8.2 The specimen shall be suitable for test when the D2992.
temperature of the test fluid, at both inlet and outlet, is
11. Report
maintained within 5°F (2.8°C) of the test temperature for a
period of 1 h. 11.1 Report the following information:
11.1.1 Complete identification of specimens, including ma-
8.3 Ambient temperature need not be controlled.
terial type, source, manufacturer’s name and code number, and
previous history,
9. Procedure 11.1.2 Pipe dimensions,
9.1 Attach the specimen with end closures into the system, 11.1.3 Test temperature and test fluid,
being careful to eliminate all air from the entire system. 11.1.4 Cyclic rate and cycles to failure of each specimen
9.2 With the valves to the specimens closed and the power tested and nature of the failure,
pump operating, adjust the pressure regulator to the desired 11.1.5 Correlation coefficient,
pressure. 11.1.6 Any unusual effects or observations during or prior to
the test,
9.3 Open the bypass needle valves, and with the circulating 11.1.7 Dates of test.
pump running, circulate the salt solution through the specimen
to obtain the desired test temperature for conditioning. 12. Precision and Bias
9.4 Close the bypass needle valve to permit only enough test 12.1 No precision and bias statement can be made for this
fluid to pass through to maintain the test temperature. Connect test method since a controlled round-robin test program has not
the failure detector units, reset these units to zero, and start the been run. A controlled round-robin program is not considered
main power pump. feasible due to the number of samples, the duration of time, and
the cyclic pressure apparatus specified by this test method.
9.5 Adjust the cycling rate to at least 25 6 2 cycles/min.
9.6 As additional specimens are added or removed from the 13. Keywords
system, maintain the maximum pressure condition desired by 13.1 cyclic pressure strength; fiberglass pipe; hydrostatic
readjusting the cyclic rate to at least 25 6 2 cycles/min. design basis; pressure design basis

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D2143-00(2010)) that may impact the use of this standard. (May 1, 2015)

(1) Revised specimen length requirements in 7.2 to be consis-


tent with Test Methods D1598 and D1599.

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D2143 − 15
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D2517 − 18

Standard Specification for


Reinforced Epoxy Resin Gas Pressure Pipe and Fittings1
This standard is issued under the fixed designation D2517; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* 2. Referenced Documents


1.1 This specification covers requirements and methods of 2.1 ASTM Standards:2
test for materials, dimensions and tolerances, hydrostatic-burst D396 Specification for Fuel Oils
strength, chemical resistance, and longitudinal tensile D543 Practices for Evaluating the Resistance of Plastics to
properties, for reinforced epoxy resin pipe and fittings for use Chemical Reagents
in gas mains and services for direct burial and insertion D618 Practice for Conditioning Plastics for Testing
applications. The pipe and fittings covered by this specification D883 Terminology Relating to Plastics
are intended for use in the distribution of natural gas, petro- D1598 Test Method for Time-to-Failure of Plastic Pipe
leum fuels (propane–air and propane–butane vapor mixtures), Under Constant Internal Pressure
manufactured and mixed gases where resistance to gas D1599 Test Method for Resistance to Short-Time Hydraulic
permeation, toughness, resistance to corrosion, aging, and Pressure of Plastic Pipe, Tubing, and Fittings
deterioration from water, gas, and gas additives are required. D1898 Practice for Sampling of Plastics (Withdrawn 1998)3
Methods of marking are also given. Design considerations are D2105 Test Method for Longitudinal Tensile Properties of
discussed in Appendix X1. “Fiberglass” (Glass-Fiber-Reinforced Thermosetting-
1.2 The values in SI units are to be regarded as the standard. Resin) Pipe and Tube
D2143 Test Method for Cyclic Pressure Strength of
1.3 The following safety hazards caveat pertains only to the Reinforced, Thermosetting Plastic Pipe
test method portion, Section 8, of this specification: This D2290 Test Method for Apparent Hoop Tensile Strength of
standard does not purport to address all of the safety concerns, Plastic or Reinforced Plastic Pipe
if any, associated with its use. It is the responsibility of the user D2412 Test Method for Determination of External Loading
of this standard to establish appropriate safety, health, and Characteristics of Plastic Pipe by Parallel-Plate Loading
environmental practices and determine the applicability of D2924 Test Method for External Pressure Resistance of
regulatory limitations prior to use. “Fiberglass” (Glass-Fiber-Reinforced Thermosetting-
NOTE 1—There is no known ISO equivalent to this standard. Resin) Pipe
D2992 Practice for Obtaining Hydrostatic or Pressure De-
1.4 A recommended inplant quality control program is
sign Basis for “Fiberglass” (Glass-Fiber-Reinforced
given in Appendix X2.
Thermosetting-Resin) Pipe and Fittings
1.5 This international standard was developed in accor- D2996 Specification for Filament-Wound “Fiberglass”
dance with internationally recognized principles on standard- (Glass-Fiber-Reinforced Thermosetting-Resin) Pipe
ization established in the Decision on Principles for the D3567 Practice for Determining Dimensions of “Fiberglass”
Development of International Standards, Guides and Recom- (Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
mendations issued by the World Trade Organization Technical Fittings
Barriers to Trade (TBT) Committee. D3839 Guide for Underground Installation of “Fiberglass”

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Plastic Piping Systems and Chemical Equipment. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Jan. 1, 2018. Published February 2018. Originally the ASTM website.
3
approved in 1966. Last previous edition approved in 2011 as D2517 – 06(2011). The last approved version of this historical standard is referenced on
DOI: 10.1520/D2517-18. www.astm.org.

*A Summary of Changes section appears at the end of this standard


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(Glass-Fiber Reinforced Thermosetting-Resin) Pipe Design Basis U, W, X, Y, and Z —Example: RTRP 11 HZ and
D3892 Practice for Packaging/Packing of Plastics fittings as defined in specification D5685-RTRF Types 1, 2, 3,
D5685 Specification for “Fiberglass” (Glass-Fiber- 4, and 5; Grade 1; Class A, C, F, and H; Category 1, 2, 3, 4, and
Reinforced Thermosetting-Resin) Pressure Pipe Fittings 5; and Pressure Rating Category D, E, F, G, H, I, and
F412 Terminology Relating to Plastic Piping Systems J—Example: RTRF 21A2D.
3. Terminology NOTE 2—The particular reinforced thermosetting resin included ini-
tially in this specification for gas pressure piping was selected on the basis
3.1 Definitions: of engineering test studies made by Battelle Memorial Institute, experi-
3.1.1 General—Definitions are in accordance with Termi- mental use in field installations, and technical data supplied by the
nology D883 or F412. Abbreviations are in accordance with manufacturers of the plastics materials used to make the pipe and fittings.
It is the intent of ASTM Committee D-20 on Plastics to consider for
Terminology D1600, unless otherwise indicated. The abbrevia- inclusion other resins and reinforcements in this specification when
tion for fiberglass pipe is RTRP and the abbreviation for evidence is presented to show that they are suitable for gas service.
fiberglass fittings is RTRF. Minimum requirements are an ASTM pipe specification and long-term
3.1.2 The gas industry technology used in this specification strength determined in accordance with Test Method D2992, Procedure B,
is in accordance with definitions given in The Department of in addition to the requirements of this specification.
Transportation of Natural and Other Gas by Pipeline Minimum
Safety Standards. 6. Requirements
3.1.3 Standards Reinforced Thermosetting Resin Pipe Ma- 6.1 Workmanship—The pipe and fittings shall be free of
terials Designation Code—The pipe material designation code visible cracks, holes, foreign inclusions, blisters, and other
shall consist of the abbreviation RTRP followed by type and injurious defects. The pipe and fittings shall be as uniform as
grade in arabic numerals, class by a capital letter and the long commercially practicable in color, opacity, density, and other
term steady pressure strength by a second capital letter. The physical properties.
fittings material designation shall consist of the abbreviation 6.2 Pipe Dimensions and Tolerances:
RTRF followed by type (method of manufacture), grade 6.2.1 Diameters—The outside diameter of the pipe shall be
(general type of resin), class (configuration of joining system), in accordance with Table 1 when measured in accordance with
and pressure rating. 8.4.1.
6.2.2 Wall Thickness—The wall thickness of the pipe shall
4. Classification
meet the requirements given in Table 1 when measured in
4.1 Pipe—The pipe covered in this specification is made by accordance with 8.4.1.
the filament winding process and is described in Specification 6.2.3 Lengths—The pipe shall be in lengths as specified on
D2996. Requirements of this pipe are based on short-term tests the purchase order when measured in accordance with 8.4.1.
defined in this specification.
NOTE 3—Either threaded adaptors or bonded joints are acceptable.
4.2 Fittings—This specification covers a) reinforced epoxy Jointers of up to 5 % of the shipment are acceptable to meet the length
resin fittings described in specification D5685 and made of the requirements. No section less than 1.5 m (5 ft) long can be used to make
type of materials covered in Section 5, and b) metal fittings a joint and only one jointer can be used in a length.
which have been designed and tested in accordance with the 6.3 Fittings Dimensions and Tolerances— The fittings di-
provisions of The Department of Transportation Title 49 of The mensions shall enable the pipe and fittings to be joined and
Code of Federal Regulations Part 192 – Transportation of shall be measured in accordance with 8.4.2.
Natural Gas and Other Gas by Pipeline: Minimum Federal
NOTE 4—Subcommittee D20.23 is working towards development of
Safety Standards, which are capable of being joined to the pipe dimensional requirements for fittings; however, it will be some time
and will provide a suitable gas distribution system. before the requirements are available. Therefore, the method of measuring
is provided only to have a standard method of measuring fittings
5. Materials dimensions for inspection purposes.
5.1 The resins and reinforcements used to make pipe shall 6.4 Short-Term Rupture Strength (Burst Pressure)—The
be as specified in 5.1.1. minimum hoop stress at burst for pipe covered by this
5.1.1 This specification covers glass fiber reinforced epoxy specification shall be as listed in Table 2 when tested in
resin pipe and fittings as defined in Specification D2996 as accordance with 8.5. The minimum burst requirements for
RTRP Type 1; Grade 1; Classes A, C, F, and H; and Hydrostatic fittings covered by this specification shall be 4.82 MPa (700

TABLE 1 Pipe Dimensions, mm (in.)


Nominal Outside Diameter Tolerance Minimum Wall Thickness

2 60.325 (2.375) +1.524, −0.457 (+0.060, −0.018) 1.524 (0.060)


3 88.900 (3.500) +1.524, −0.457 (+0.060, −0.018) 1.524 (0.060)
4 114.300 (4.500) +1.524, −0.457 (+0.060, −0.018) 1.780 (0.070)
6 168.275 (6.625) +1.678, −0.711 (+0.066, −0.028) 2.540 (0.100)
8 219.075 (8.625) +2.184, −1.016 (+0.086, −0.040) 3.227 (0.125)
10 273.050 (10.750) +2.743, −1.219 (+0.108, −0.048) 3.830 (0.150)
12 323.850 (12.750) +3.251, −1.422 (+0.128, −0.056) 4.215 (0.175)

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D2517 − 18
TABLE 2 Minimum Physical Property Requirements for Pipe sampling plan be agreed upon by the purchaser and the
65.6°C manufacturer (see Practice D1898).
Test 23°C (150°F)
Physical Property Method (73.4°F) 8.2 Conditioning—Unless otherwise specified, condition the
specimens prior to test at 23 6 2°C (73.4 6 3.6°F) and 50 6
Short-term rupture strength (burst) D1599 40 000 35 000 5 % relative humidity for not less than 48 h, in accordance with
min, hoop stress, psi
Static hydrostatic hoop stress 105 h D2992 15 000 14 000
Procedure A of Practice D618 for those tests where condition-
(estimated), min, psi ing is required and in all cases of disagreement.
Hydrostatic collapse min, psig D2924 14.7 11.0
Longitudinal tensile strength, min, psi D2105 8 900 8 300
8.3 Test Conditions—Conduct the tests in the Standard
Parallel plate crush strength, min D2412 45 41 Laboratory Atmosphere of 23 6 2°C (73.4 6 3.6°F), unless
pipe stiffness at 5% deflection, psi otherwise specified.
8.4 Dimensions and Tolerances:
8.4.1 Wall Thickness and Diameter—Determine in accor-
psi) internal pressure or 27.5 MPa (4000 psi) hoop tensile dance with Practice D3567.
stress, whichever is greater, when tested in accordance with 8.5 8.4.2 Liner Thickness—When the test specimens contain a
at temperatures of 23°C (73.4°F) and 65.6°C (150°F), and liner, determine the average liner thickness in accordance with
calculated using the equation listed in Test Method D1599 for Practice D3567.
hoop stress. The calculations shall use the fittings wall thick- 8.5 Short-Term Hydrostatic Failure Strength (Minimum
ness and diameter at a point where the wall thickness is at a Hoop Stress)—Determine in accordance with Test Method
minimum and which is also in the section of the fittings which D1599. Fittings shall be tested with pipe nipples bonded in the
is not reinforced by the pipe. sockets.
6.5 Crush Strength—The minimum stiffness at 5 % deflec- 8.6 Apparent Tensile Properties—The apparent tensile
tion of the pipe shall be as shown in Table 2 when tested in strength shall be determined in accordance with Procedure B of
accordance with Test Method D2412. Test Method D2290.
6.6 Chemical Resistance—The pipe shall not change more 8.7 Chemical Resistance—Determine the resistance to the
than 612 % in apparent tensile strength when measured in following chemicals in accordance with Procedure II of Test
accordance with 8.7. Method D543, except use ring specimens cut from pipe for this
NOTE 5—A suitable chemical resistance test for fittings is not available
purpose:
at the present time and will be added when available. Chemical Concentration, %
Fuel Oil No. 1 (Specification D396) 100
6.7 Longitudinal (Tensile Strength)—The minimum longi- t-butyl mercaptan 5 in fuel oil
tudinal tensile strength for pipe covered by this specification Antifreeze agents (at least one shall be used):
Methanol 100
shall be as listed in Table 2 when tested in accordance with Test Isopropanol 100
Method D2105. Ethylene glycol 100
6.8 Hydrostatic Collapse—The minimum factor for pipe Cut specimens from the pipe in accordance with 8.6; test five
covered by this specification shall be as listed in Table 2 when specimens with each reagent. Coat specimen edges with
tested in accordance with Test Method D2924. adhesive prior to immersion. Completely immerse the speci-
mens in the chemicals for 72 h. Upon removal from the
7. Adhesive Requirements chemicals, wipe the specimens with a clean dry cloth, condi-
7.1 Adhesives used to join reinforced epoxy resin pipe shall tion in the testing room for a period not to exceed 2 h, and then
be suitable for use with the pipe and fittings and meet the test in tension in accordance with 8.6.
requirements listed in 7.2 and 7.3. 8.8 Adhesive Test—The ultimate shear strength for adhe-
NOTE 6—It is recommended that the working (pot) life of the adhesive
sives used to bond pipe and fittings together shall be deter-
be agreed upon between the purchaser and the manufacturer. mined in accordance with the following procedure; it is
applicable to all adhesives covered by this specification.
7.2 Adhesive Test—All adhesives covered by this specifica-
8.8.1 Principle—Laboratory shear specimens are made by
tion shall have a minimum ultimate shear strength of 10.3 MPa
bonding together two 3 by 13 by 75-mm (1⁄8 by 1⁄2 by 3-in.),
(1500 psi) when tested in accordance with 8.8.
reinforced thermosetting plastic laminates using the supplied
7.3 Packaging—Each adhesive kit shall contain the neces- adhesive kits. This specimen is then cured in accordance with
sary components and instruction sheets, which shall include instructions supplied with the adhesive. After curing, the
cure times and pot life. specimen is pulled apart in a universal testing machine.
8.8.2 Test Specimen—The test specimen shall be made using
8. Test Methods longitudinally reinforced epoxy resin laminates that are made
8.1 Sampling—Take a sample of the pipe and fittings of the same materials as the pipe with dimensions of 5 by 13
sufficient to determine conformance with this specification. by 75 mm (1⁄8 by 1⁄2 by 3 in.). Each specimen shall have a
About 15 m (50 ft) of pipe or tubing are required to make the bonding surface on one end made by milling off 5 mils of the
tests prescribed. The number of fittings required varies, de- surface for a length of 2 mm (3⁄4 in.). Test a minimum of five
pending upon the size and type of fitting. It is suggested that a test specimens.

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8.8.3 Procedure: where:
8.8.3.1 Clean the milled surfaces of two 75-mm (3-in.) long s = estimated standard deviation,
laminates using solvent supplied with adhesive. X = value of a single observation,
8.8.3.2 Mix the adhesive components in accordance with n = number of observations, and
instructions supplied with the adhesives. X̄ = arithmetical average of the set of observations.
8.8.3.3 Wet the cleaned surface of the laminates with the
mixed adhesive. 9. Packaging and Marking
8.8.3.4 Press the adhesive-coated areas of the laminates 9.1 Pipe—All required marking shall be legible and so
together, maintaining alignment of edges and clamp so that the applied without indentation as to remain legible under normal
specimen is held together using uniform pressure. Pressure handling and installation practices. These markings shall con-
used shall be sufficient to yield specimens with adhesive line sist of the manufacturer’s name or trademark, the nominal pipe
thicknesses that do not exceed 0.9 mm (1⁄32 in.). size, and the standard reinforced plastic pipe identification at
8.8.3.5 Note the time when assembly is completed. each end of the pipe. In addition to the above, the pipe shall
8.8.3.6 Check the temperature in the room and determine bear an appropriate code number which will ensure identifica-
the cure time from instructions supplied with the adhesive. tion of the pipe as to the month and year of production and raw
8.8.3.7 When the required amount of time has elapsed, materials used in the production of said pipe. The manufacturer
remove the specimen from the clamping fixture, and place it in shall maintain such additional records as are necessary to
grips of the universal testing machine. Good alignment in the confirm identification of all coded pipe. Marking shall include
grips is essential. Set speed control at 5.1 to 6.4 mm (0.20 to the designation ASTM D2517.
0.25 in.)/min and start the testing machine. Record the break- 9.2 Fittings—All fittings shall be marked on the body or
ing load. hub. The marking shall consist at least of the manufacturer’s
8.8.4 Calculation—Calculate the ultimate shear strength of name or trademark, or both, and the symbol for the type of
the adhesive using the following equation and report to three material and size. Marking shall include the designation ASTM
significant figures: D2517.
σ 5 P/A (1) 9.3 Adhesives—All adhesive containers shall be marked on
where: the container. The marking shall consist of the manufacturer’s
σ = ultimate shear stress, MPa (or psi), name or trademark, or both, manufacturing date, shelf life, and
P = ultimate load, N (or lbf), and storage requirements.
A = bond area, mm2 (or in.2). 9.4 All packing, packaging, and marking provisions of
For each series of tests, calculate the arithmetic mean of all Practice D3892 shall apply to this specification.
values obtained to three significant figures and report as the
10. Keywords
“average value.” Calculate the standard deviation as follows
and report to two significant figures: 10.1 filament wound; compression molded; configuration of
1
joining system; rupture srength; crush strength; chemical
s 5 @~ ( X 2 2 nX̄ ! / ~ n 5 1 ! #
2 2
(2) resistance; apparent tensile properties; adhesive

APPENDIXES

(Nonmandatory Information)

X1. DESIGN

X1.1 General X1.2 Internal Pressure


X1.1.1 The design of a plastic piping system for gas must X1.2.1 The design stresses for natural gas are based on the
include consideration of the effect of the environment while 100 000-h hydrostatic strength of the pipe of 75°F obtained in
under stress, as well as internal and external loads. The accordance with Procedure B of Practice D2992. The
combined effects of time, stress, and environment must be 100 000-h strengths of the plastics included in the applicable
investigated as an overall basis for selecting a specific kind and ASTM specifications are as follows:
size of plastic pipe. The selection of design stresses for RTRP Long-Term (100 000-h)
is the prerogative of the Department of Transportation (DOT) Plastic Pipe Material Designation Strength at 23°C (73°F)
Office of Pipeline Safety. The AGA Plastic Pipe Committee and RTRP (glass fiber reinforced epoxy resin pipe) 15 000 psi

members of Committee D-20 are cooperating with DOT to Strengths for other RTRP materials will be added when these
provide assistance in selecting safe design stress levels for the materials are included in the applicable ASTM specifications.
various kinds of plastic pipe. The design stresses are obtained by multiplying the 100 000-h

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D2517 − 18
strength by design factors or service factors in accordance with flexible conduit (as defined by Marston and Spangler)4 to
the class of location as described in Chapter IV of the ASME support relatively large earth loads without excessive deflec-
Code for Pressure Piping B31, ASME B 31.8, Gas Transmis- tion by mobilizing lateral passive soil forces. Proper installa-
sion and Distribution Piping System and The Department of tion technique ensures that the necessary passive soil pressure
Transportation Minimum Federal Safety Standards for Gas at the sides of the pipe will be developed and maintained. It is
Lines (Part 192 Title 49 Code of Federal Regulations). also recognized that the internal pressures may be valuable in
minimizing the deflection caused by earth loads. However, the
X1.3 External Loads magnitude of this latter effect is somewhat subjective, and
therefore installation procedures defined in Test Method D3839
X1.3.1 It is recognized that certain minimum requirements are recommended instead of more specific information.
exist for the support of earth loads from backfill and other
external forces. Proper installation techniques can be used with
4
Spangler, M. G., “Secondary Stresses in Buried High Pressure Lines,” The
Iowa State College Bulletin, Engineering Report 23 of the Iowa Engineering
Experiment Station, 1954–1955.

X2. RECOMMENDED IN-PLANT QUALITY CONTROL PROGRAM FOR REINFORCED EPOXY RESIN PIPE INTENDED
FOR USE IN NATURAL GAS SERVICE

X2.1 Introduction TABLE X2.1 Pipe Tests

X2.1.1 The following in-plant quality control program cov- Property Test Method Test Frequency

ering material, performance requirements, and marking shall


Visual ... all
be used in manufacture to provide reasonable assurance that Dimensions:
the RTRP pipe and fittings for use with the type of RTRP Diameter D3567 900 m (3000 ft) or once/3h
Wall thickness D3567 1500 m (5000 ft) or once/lotA
supplied under this code meets the requirements of the appli-
Mechanical properties:
cable standard. The pipe and fittings producers shall maintain Burst pressure D1599 5000 ft
records on all aspects of this program and supply these to the Short-term static (20 D1598 (D2143) 24 h
h) or cyclicB
purchaser, if requested.
A
Whichever is most frequent.
X2.2 Material B
A cyclic pressure test made in accordance with the procedure in Test Method
D2143 may be substituted for the static test requirements if it has been demon-
X2.2.1 The pipe and fittings manufacturer shall use only strated that the results of the two methods are equivalent.
those raw materials that are allowed by the applicable standard
and shall so certify.
X2.3 Pipe Tests
X2.3.1 Product Quality Control (See Note X2.1)—The tests X2.5 Records
in Table X2.1 shall be made per size per processing unit at the
denoted frequencies and the test results recorded and filed for X2.5.1 A code number shall be included in the marking on
inspection, upon request. the pipe. If required, on the directional fittings, the code
number may be used to identify in the records the following:
NOTE X2.1—When the pipe fails to meet the specification (or standard)
requirement in any test, additional tests shall be made on the pipe X2.5.2 The compound,
produced back to the previous acceptable results to select the pipe
produced in the interim that does pass the requirement. Pipe that does not X2.5.3 The date of manufacture,
meet the requirement shall be rejected.
X2.5.4 The shift,
X2.4 Test Methods
X2.5.5 The test results required in this in-plant quality
X2.4.1 The test methods may be those generally used by the
control program, and
manufacturer, but in case of question, those given in the
applicable ASTM standard shall be used. X2.5.6 The manufacturer.

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D2517 − 18
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue,
D2517–06(2011), that may impact the use of this standard.(January 1, 2018)

(1) Revised 5.1.1. (2) Revised Table 2.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D2924 − 12 (Reapproved 2017)

Standard Test Method for


External Pressure Resistance of “Fiberglass”
(Glass-Fiber-Reinforced Thermosetting-Resin) Pipe1
This standard is issued under the fixed designation D2924; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 3. Terminology
1.1 This test method covers determination of the resistance 3.1 Definitions:
of fiberglass pipe to external pressure. It classifies failures as 3.1.1 Definitions are in accordance with Terminology D883
buckling, compressive, and leaking. Both glass-fiber- or F412 and abbreviations are in accordance with Terminology
reinforced thermosetting-resin pipe (RTRP) and glass-fiber- D1600, unless otherwise indicated.
reinforced polymer mortar pipe (RPMP) are fiberglass pipes. 3.2 Definitions of Terms Specific to This Standard:
NOTE 1—For the purposes of this standard, polymer does not include 3.2.1 aggregate, n—a siliceous sand conforming to the
natural polymers.
requirements of Specification C33, except that the require-
1.2 The values stated in inch-pound units are to be regarded ments for gradation shall not apply.
as standard. The SI units given in parentheses are for informa-
tion only. 3.2.2 buckling failure pressure— the external gage pressure
at which buckling occurs. Buckling is characterized by a sharp
NOTE 2—There is no known ISO equivalent to this standard. discontinuity in the pressure-volume change graph and subse-
1.3 This standard does not purport to address all of the quent fracture in the test specimen appearing as an axially
safety concerns, if any, associated with its use. It is the oriented crack. Buckling is an elastic instability type of failure
responsibility of the user of this standard to establish appro- and is normally associated with thin-wall pipe.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3.2.3 compressive failure pressure—the maximum external
1.4 This international standard was developed in accor- gage pressure that the specimen will resist without transmis-
dance with internationally recognized principles on standard- sion of the testing fluid through the wall. Compressive failure
ization established in the Decision on Principles for the pressure will not be associated with a sharp discontinuity in the
Development of International Standards, Guides and Recom- pressure-volume change graph nor lead to a fracture appearing
mendations issued by the World Trade Organization Technical as a sharp axially oriented crack. It will appear as a fracture
Barriers to Trade (TBT) Committee. which is the result of reaching the compressive strength limits
of the material and is normally associated with thick-wall pipe.
2. Referenced Documents Failure is usually identified by a sudden drop in pressure.
2.1 ASTM Standards:2
3.2.4 fiberglass pipe, n—a tubular product containing glass
C33 Specification for Concrete Aggregates
D618 Practice for Conditioning Plastics for Testing fiber reinforcements embedded in or surrounded by cured
D883 Terminology Relating to Plastics thermosetting resin; the composite structure may contain
D1600 Terminology for Abbreviated Terms Relating to Plas- aggregate, granular, or platelet fillers, thixotropic agents,
tics pigments, or dyes; thermoplastic or thermosetting liners or
F412 Terminology Relating to Plastic Piping Systems coatings may be included.
3.2.5 leaking pressure—the external gage pressure at which
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics the test fluid is transmitted through the pipe wall. It is
and is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic characterized in this test by continuous volume change indica-
Piping Systems and Chemical Equipment.
Current edition approved Sept. 1, 2017. Published September 2017. Originally
tions with no pressure increase.
approved in 1970. Last previous edition approved in 2012 as D2924 – 12. DOI:
3.2.6 reinforced polymer mortar pipe (RPMP), n—a fiber-
10.1520/D2924-12R17.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or glass pipe with aggregate.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 3.2.7 reinforced thermosetting resin pipe (RTRP), n—a fi-
the ASTM website. berglass pipe without aggregate.

*A Summary of Changes section appears at the end of this standard


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4. Summary of Test Method
4.1 This test method consists of loading a specimen to
failure in a short time interval by means of incrementally
increasing external fluid pressure at a controlled constant
temperature. Fluid is also maintained inside the pipe, and
changes in the inside volume are monitored with a bleed hole
and fluid level tube. On Cartesian coordinates, pressure versus
change in volume is plotted and the failure pressure selected as
indicated by the graph. Scaling constants are presented for
extending the results to other diameters.
5. Significance and Use
5.1 The values obtained by this test method are applicable
only to conditions that specifically duplicate the procedures
used.
5.2 After a scaling constant is determined for one diameter,
this may be used for calculating the external failure pressures
of other diameters as long as the resin and reinforcement (if
used), the wall thickness-to-diameter ratio, and the reinforce-
ment pattern (if reinforcement is used) are the same.
NOTE 3—Based upon tests conducted on one size of pipe, a scaling
constant is calculated according to 10.1 or 10.2. The appropriate constant
is used to calculate failure pressure for other pipe diameters, but it can
only be applied if the same resin and reinforcement are used, the wall
thickness to diameter ratios are similar, and the reinforcement pattern is
constant.
5.3 In the application of the following test requirements and
recommendations, care must be exercised to ensure that the FIG. 1 Apparatus Showing Specimen Loading with Both Hoop
specimens tested are truly representative of the group being and Axial Loads
studied.
6. Apparatus (see Figs. 1 and 2)
6.6 Temperature Regulator—When temperatures other than
6.1 Test Chamber—An external chamber capable of with-
ambient are being studied, a temperature-regulating system
standing pressures to be encountered. It may be either the type
will be employed that will maintain the temperature of the
that applies both hoop and axial loads as shown in Fig. 1 or the
testing fluid and specimen at a specified amount 62°C.
type that applies hoop load only as shown in Fig. 2. In either
event, the report shall state which type loading was used for
7. Test Specimens
test.
7.1 Number of Specimens—A minimum of five specimens
6.2 Weight Change Indicator—The specimen shall be in-
shall be used for determining the external pressure resistance.
strumented to measure changes in weight by use of a balance
Any specimens that are tested and fall outside the specified
accurate to within 60.1 g.
time limits shall be discounted and replaced with equivalent
6.2.1 Transparent Tube—Connected to the test specimen so
specimens, so that a minimum of five valid specimens are
that the volume changes of the specimen result in changes in
tested.
the level of fluid in the tube. A scale shall be affixed to the tube
so variations in fluid level can be recorded. Absolute measure- 7.2 Specimen Size—The inside and outside diameters of the
ment of volume change is not required. pipe specimens shall be as fabricated, with the permissible
exception of that portion of the pipe within 2 in. (50 mm) of the
6.3 Pressurizing System—A device capable of exerting ex-
end closures. The minimum specimen length exposed to
ternal fluid pressure to the specimen at a specified constant
external pressure shall be the greater of:
rate. A Bourdon-tube pressure gage or recording gage with an
accuracy of6 1 % of full scale should be used, and the L 5 10~ D !
anticipated failure pressure should be in the middle two thirds or Roark’s formula for long tube length:3
of the gage range. Care should be exercised so the gage is
placed where it will give a true reading of the external pressure
on the test specimen.
L 5 4.90r Πr
t
6.4 Test Fluid—Water or hydraulic oil.
6.5 Timer—Any time-measuring device that can measure 3
Roark, Raymond J., Roark’s Formulas for Stress and Strain, McGraw-Hill
the duration of test with accuracy of 1 s. Book Company, New York, NY, Sixth Edition, 1989, p. 690.

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increasing weight of displaced fluid with a small increase in
pressure indicates failure. Record the time to failure.
9.3 After the specimen has failed, remove it from the
external pressure chamber and observe and record appearance.
9.4 Make a graph showing external pressure versus weight
of fluid displaced. A sharp change in slope indicates either a
buckling pressure or a pressure at which the pipe wall
transmitted fluid. Either condition is classified as failure.

10. Calculation
10.1 For specimens that failed by buckling, calculate a
buckling scaling constant as follows:
K 5 P⁄E□ ~ r ⁄ t ! 3

where:
K = buckling scaling constant,
P = external collapse pressure, psi (or MPa),
E = circumferential modulus of elasticity,
r = mean wall radius (do not include unreinforced liner in
reinforced wall), in. (or mm), and
t = minimum wall thickness (do not include unreinforced
liner in reinforced wall), in. (or mm).
10.2 For specimens that failed by collapse, calculate a
compressive failure scaling constant as follows:
C 5 P c ~ D 2 t ! /2t

where:
FIG. 2 Apparatus Showing Specimen Loading with Hoop Load C = compressive failure scaling constant,
Only Pc = pressure at failure, psi (or MPa),
D = the average outside diameter of the specimen, in. (or
where: mm), and
L = length of test specimen exposed to external pressure, in. t = minimum pipe wall thickness (do not include liner in
(or mm), filament reinforced wall), in. (or mm).
D = average outside diameter of pipe, in. (or mm), 10.3 Calculate the average failure pressure for all five
r = mean wall radius (do not include unreinforced liner), in. specimens tested.
(or mm), and
t = minimum wall thickness (do not include unreinforced 10.4 Calculate the average scaling constant for all five
liner), in. (or mm). specimens tested.

8. Conditioning 11. Report


8.1 All samples shall be conditioned for a minimum of 2 h 11.1 Report the following information:
in the fluid in which they will be tested. The temperature of the 11.1.1 Complete identification of the specimens, including
fluid shall be uniform and stabilized to within 62°C of the test material type, source, manufacturer’s name, pipe trade name,
temperature during conditioning. and previous history,
11.1.2 Pipe Dimensions—Record dimensions of each speci-
9. Procedure
men including nominal size, length exposed to external
9.1 Mount the specimen in the test chamber and fill both pressure, minimum wall thickness, and average outside diam-
internal and external volumes with the test fluid. Take care to eter. The wall thickness and outside diameter shall be rein-
expel all air from the inside of the specimen as any gaseous forced dimensions only. Unreinforced thickness shall also be
fluid escaping through the measuring tube during the test will recorded.
disqualify the test. Fit the specimen with a tube to direct the 11.1.3 Test temperature and test fluid, (water or oil),
fluid into a suitable basin for collecting and weighing. Condi- 11.1.4 Type of loading used (hoop only or both hoop and
tion the system at a temperature in accordance with Section 8. axial),
9.2 Increase the pressure at an incremental rate. The incre- 11.1.5 Failure pressures for each specimen tested and the
ment shall be chosen to allow at least 10 readings before average,
failure. After the fluid has stopped flowing from the tube, 11.1.6 Type of failure (buckling, compressive, or leaking),
record the pressure and weight of the fluid displaced. Rapidly 11.1.7 Time to failure of each specimen tested,

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11.1.8 Scaling constant (see 10.1 for buckling failures, 10.2 suspect at a probability level of 0.95. They are expressed as
for compressive failures, no scaling permitted for leaking percentages of the mean value.
failures), and 12.2.1 Hoop Load Method—For individual values within a
11.1.9 Date of test. set of five, the precision is 68.4 %. Between averages of five
12. Precision and Bias determinations, the precision is 64.9 %.
12.1 The precision of this test method was determined from 12.2.2 Axial and Hoop Load Method—For individual values
the results of one laboratory performing one set of tests by each within a set of five, the precision is 613.1 %. Between
loading method on each of six pipe sizes and conditions. averages of five determinations, the precision is 67.6 %.
12.2 The following values of precision have been calculated 12.3 There are presently no definite means of establishing a
from the above test program. true value, so no bias statement can be made.
NOTE 4—These values were developed using Procedure A. The samples
were conditioned at 23 6 2° (73.4 6 3.6°F) and 50 6 5 % relative 13. Keywords
humidity for not less than 40 h prior to test in accordance with Procedure
A of Practice D618. 13.1 external pressure resistance; fiberglass pipe; pipe; re-
The critical differences indicate the maximum deviation of inforced polymer mortar pipe (RPMP); reinforced
results beyond which measured values should be considered thermosetting-resin pipe (RTRP)

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D2925 − 14 (Reapproved 2019)

Standard Test Method for


Beam Deflection of “Fiberglass” (Glass-Fiber-Reinforced
Thermosetting Resin) Pipe Under Full Bore Flow1
This standard is issued under the fixed designation D2925; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This test method covers measurement of the deflection 2.1 ASTM Standards:2
as a function of time of a specimen of fiberglass pipe supported C33/C33M Specification for Concrete Aggregates
on a flat non-arced support as a simple beam under full bore D883 Terminology Relating to Plastics
flow of water at elevated temperatures. Both glass-fiber- D1600 Terminology for Abbreviated Terms Relating to Plas-
reinforced thermosetting-resin pipe (RTRP) and glass-fiber- tics
reinforced polymer mortar pipe (RPMP) are fiberglass pipes. D3567 Practice for Determining Dimensions of “Fiberglass”
(Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
NOTE 1—For the purposes of this standard, polymer does not include Fittings
natural polymers.
F412 Terminology Relating to Plastic Piping Systems
1.2 This test method can be used to determine deflection at
varying conditions by substituting other test media. 3. Terminology
1.3 Deflections observed using this test method are repre- 3.1 General—Definitions are in accordance with Terminolo-
sentative only of piping supported as a simple beam under full gies D883 and F412 and abbreviations are in accordance with
bore flow which has one diameter of pipe overhanging at each Terminology D1600, unless otherwise indicated.
support. 3.2 Definitions of Terms Specific to This Standard:
1.4 The values stated in SI units are to be regarded as the 3.2.1 aggregate—a siliceous sand conforming to the re-
standard. The values given in parentheses are provided for quirements of Specification C33/C33M, except that the re-
information purposes only. quirements for gradation shall not apply.
3.2.2 fiberglass pipe—a tubular product containing glass
NOTE 2—There is no known ISO equivalent to this standard.
fiber reinforcement embedded in or surrounded by cured
1.5 This standard does not purport to address all of the thermosetting resin; the composite structure may contain
safety concerns, if any, associated with its use. It is the aggregate, granular or platelet fillers, thixotropic agents,
responsibility of the user of this standard to establish appro- pigments, or dyes; thermoplastic or thermosetting liners may
priate safety, health, and environmental practices and deter- be included.
mine the applicability of regulatory limitations prior to use.
3.2.3 reinforced thermosetting resin pipe (RTRP)—a fiber-
1.6 This international standard was developed in accor-
glass pipe without aggregate.
dance with internationally recognized principles on standard-
3.2.4 reinforced polymer mortar pipe (RPMP)—a fiberglass
ization established in the Decision on Principles for the
pipe with aggregate.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical 4. Significance and Use
Barriers to Trade (TBT) Committee.
4.1 In the absence of deflection measurements from actual
installed-above-ground piping, this test method may be used to
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic
2
Piping Systems and Chemical Equipment. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Aug. 1, 2019. Published August 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1970. Last previous edition approved in 2014 as D2925 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2925-14R19. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D2925 − 14 (2019)
evaluate the influence of span length on mid-span deflections at water at all times. Any recirculation shall be vented to
differing temperatures under full bore flow. atmosphere. A schematic drawing of the test setup is shown on
NOTE 3—A flat bearing area, small contact area, and narrow bearing
Fig. 2.
width may induce high localized support interaction stresses, and con- 5.3 Flexible Connections for the ends of the pipe test
straints imposed by the supports may also adversely influence deflections specimens, installed so as to produce negligible moment on the
and performance of the pipe.
ends of the pipe.
5. Apparatus 5.4 A Device for Measuring the Deflection of the pipe
5.1 Rigid Support with edges rounded to a 6-mm ( ⁄ -in.) 14 specimen to the nearest 0.025 mm (0.001 in.) with negligible
radius, consisting of two uprights of a convenient height. The constraint on the specimen. A recommended device is a
uprights are to be spaced at a predetermined distance over cathetometer as shown on Fig. 1.
which deflection is to be determined as shown on Fig. 1. The 5.5 Time-Interval Measuring Device graduated in minutes
uprights shall have lateral guides, a saddle, groove, or inden- or seconds.
tation on the top to keep the pipe specimen from rolling off 5.6 Temperature and Pressure Gages and suitable control
when placed in position. devices to maintain standard test conditions.
5.1.1 The support space distance shall be estimated for a
maximum allowable sag of 12.7 mm (1⁄2 in.) at test conditions. 6. Test Specimens
This estimate may be made by solving Eq 1 for L, using y = 6.1 The test specimens shall be sections of fiberglass pipe
12.7 mm (1⁄2 in.) and assuming an elastic modulus, E = cut to a precalculated span length plus two pipe diameters 6 13
1 000 000 psi, unless a more accurate value is available. mm (60.5 in.), essentially straight and of a diameter and wall
5.2 Source of Hot Water and a Feed System maintained at thickness to be specified.
conditions such that when this source is coupled to the pipe 6.2 At least three specimens shall be tested for any given
specimen and the water is fed into the specimen, the water pipe size.
emerging from the specimen shall be maintained continuously
at the controlled temperature within 62°C (3.6°F). The water 7. Test Temperature
shall be fed into the specimen at a head not exceeding 1.5 m 7.1 The test temperature selected should be the maximum
(5 ft) and allowed to flow through it under such conditions that recommended service temperature for the piping unless it is
the pipe specimen is filled with the controlled temperature desired to test the effects of temperature variation.

FIG. 1 Schematic of Test Specimen Support

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FIG. 2 Schematic of Test Set-up for Beam Deflection Test on Pipe

8. Procedure 9. Calculation
8.1 Measure the total wall thickness, liner thickness, and 9.1 Calculate EI values from the data obtained, as follows:3
diameter of the pipe specimen in accordance with Practice EI 5 22.5wL4 /y (1)
D3567.
where:
8.2 Place the test specimen on the upright supports so that
there is an overhang of one pipe diameter 613 mm (60.5 in.) w = combined weight of pipe and fluid at test temperature,
on each end. lb/ft,
L = span length, ft,
8.3 Connect the test specimen to the water supply and outlet y = maximum measured deflection, in.,
system by means of supported flexible connectors. E = apparent elastic modulus of pipe, psi,
8.4 Fill the pipe test specimen with water at ambient I = 0.0491 (D4 − d4), cross-section moment of inertia of
temperature and determine initial deflection. pipe, in.4,
D = average outer diameter of pipe, in., and
8.5 Circulate the test media (water) through the test speci- d = average inner diameter of pipe, in.
men until a steady-state temperature (see 5.2) is attained at the
designated test temperature. Then take the initial elevated 10. Report
temperature deflection reading. 10.1 The report shall include the following:
8.6 Measure the position of the base point and the point of 10.1.1 Test laboratory and supervisor of tests,
maximum deflection at 15-min intervals for 1 h and then at 1-h 10.1.2 Dates of test,
intervals for 4 h. 10.1.3 Complete identification of the sample, including
8.7 Continue to measure the position of the base point and material, manufacturer, type, source, and previous history,
the point of maximum deflection at suitable time intervals until 10.1.4 Pipe dimensions, including nominal pipe size, mini-
1000 h have elapsed or until the total maximum deflection mum and average wall thickness, liner thickness, and the
exceeds the allowable design limit of 12.7 mm (1⁄2 in.). If a minimum and average outside diameter of each specimen,
change of deflection less than 0.025 mm (0.001 in.) occurs in 10.1.5 Number of specimens tested,
two consecutive 24-h periods after 1000 h elapsed time, the test 10.1.6 Calculated weight of pipe filled with water at test
may be terminated. If the change in deflection is greater than temperature, pounds per foot,
0.025 mm (0.001 in.) in two consecutive 24-h periods after 10.1.7 Type of support used and dimensions of support
1000 hour elapsed time, the test should be continued until the (width and saddle radius),
design limit of 12.7 mm (1⁄2 in.) is reached or until a change of 10.1.8 Span length between supports used in test,
deflection less than 0.025 mm (0.001 in.) occurs in two
consecutive 24-h periods. Record this equilibrium time and 3
Crocker, Sabin, Piping Handbook, McGraw-Hill Book Co., NY, Fourth Edition,
maximum deflection. 1945, p. 745.

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D2925 − 14 (2019)
10.1.9 Temperature of inlet and outlet water at equilibrium, 12. Keywords
10.1.10 Table of deflection in inches versus time in hours, 12.1 beam deflection; fiberglass pipe; fullbore flow; elastic
and modulus
10.1.11 Calculated EI values.
10.1.12 Temperature of environment outside the pipe.
11. Precision and Bias
11.1 Attempts to develop a precision and bias statement for
this method have not been successful. For this reason, data on
precision and bias cannot be given.4

4
Anyone wishing to participate in the development of precision and bias data
should contact the Chairman, Subcommittee D 20.23, ASTM International, 100 Barr
Harbor Drive, PO Box C700, West Conshohocken, PA, 19428-2959 .

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue, D2925 – 14,
that may impact the use of this standard. (August 1, 2019)

(1) Reapproved without changes.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D2992 − 18

Standard Practice for


Obtaining Hydrostatic or Pressure Design Basis for
“Fiberglass” (Glass-Fiber-Reinforced Thermosetting-Resin)
Pipe and Fittings1
This standard is issued under the fixed designation D2992; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* practice may not be applicable for evaluating stresses induced


by loadings where the longitudinal stress exceeds 50 % of the
1.1 This practice establishes two procedures, Procedure A
HDS.
(cyclic) and Procedure B (static), for obtaining a hydrostatic
design basis (HDB) or a pressure design basis (PDB) for 1.5 The values stated in inch-pound units are to be regarded
fiberglass piping products, by evaluating strength-regression as the standard. The values in parentheses are given for
data derived from testing pipe or fittings, or both, of the same information purposes only.
materials and construction, either separately or in assemblies. NOTE 3—There is no known ISO equivalent to this standard.
Both glass-fiber-reinforced thermosetting-resin pipe (RTRP)
1.6 This standard does not purport to address all of the
and glass-fiber-reinforced polymer mortar pipe (RPMP) are
safety concerns, if any, associated with its use. It is the
fiberglass pipe.
responsibility of the user of this standard to establish appro-
NOTE 1—For the purposes of this standard, polymer does not include priate safety, health, and environmental practices and deter-
natural polymers. mine the applicability of regulatory limitations prior to use.
1.2 This practice can be used for the HDB determination for 1.7 This international standard was developed in accor-
fiberglass pipe where the ratio of outside diameter to wall dance with internationally recognized principles on standard-
thickness is 10:1 or more. ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
NOTE 2—This limitation, based on thin-wall pipe design theory, serves mendations issued by the World Trade Organization Technical
further to limit the application of this practice to internal pressures which, Barriers to Trade (TBT) Committee.
by the hoop-stress equation, are approximately 20 % of the derived
hydrostatic design stress (HDS). For example, if HDS is 5000 psi (34 500
kPa), the pipe is limited to about 1000-psig (6900-kPa) internal pressure, 2. Referenced Documents
regardless of diameter. 2.1 ASTM Standards:2
1.3 This practice provides a PDB for complex-shaped prod- D618 Practice for Conditioning Plastics for Testing
ucts or systems where complex stress fields seriously inhibit D883 Terminology Relating to Plastics
the use of hoop stress. D1598 Test Method for Time-to-Failure of Plastic Pipe
Under Constant Internal Pressure
1.4 Specimen end closures in the underlying test methods D1599 Test Method for Resistance to Short-Time Hydraulic
may be either restrained or free, leading to certain limitations. Pressure of Plastic Pipe, Tubing, and Fittings
1.4.1 Restrained Ends—Specimens are stressed by internal D1600 Terminology for Abbreviated Terms Relating to Plas-
pressure only in the hoop direction, and the HDB is applicable tics
for stresses developed only in the hoop direction. D2143 Test Method for Cyclic Pressure Strength of
1.4.2 Free Ends—Specimens are stressed by internal pres- Reinforced, Thermosetting Plastic Pipe
sure in both hoop and longitudinal directions, such that the D3567 Practice for Determining Dimensions of “Fiberglass”
hoop stress is twice as large as the longitudinal stress. This (Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
Fittings
F412 Terminology Relating to Plastic Piping Systems
1
This practice is under the jurisdiction of ASTM Committee D20 on Plasticsand
is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic Piping
2
Systems and Chemical Equipment. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 15, 2018. Published May 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1971. Last previous edition approved in 2012 as D2992 – 12. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2992-18. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D2992 − 18
F948 Test Method for Time-to-Failure of Plastic Piping 3.1.9 hydrostatic design basis (HDB)—a hoop stress devel-
Systems and Components Under Constant Internal Pres- oped for fiberglass pipe by this practice and multiplied by a
sure With Flow (Withdrawn 2018)3 service design factor to obtain an HDS.
2.2 ISO Standard: 3.1.10 hydrostatic design pressure (HDP)—the estimated
3 Preferred Numbers—Series of Preferred Numbers4 maximum internal hydrostatic pressure that can be applied
cyclically (Procedure A) or continuously (Procedure B) to a
3. Terminology piping component with a high degree of certainty that failure of
the component will not occur.
3.1 Definitions:
3.1.1 General—Definitions are in accordance with Termi- 3.1.11 hydrostatic design stress (HDS)—the estimated
nologies D883 and F412, and abbreviations are in accordance maximum tensile stress in the wall of the pipe in the hoop
with Terminology D1600, unless otherwise indicated. direction due to internal hydrostatic pressure that can be
applied cyclically (Procedure A) or continuously (Procedure B)
3.1.2 closure, free-end—a sealing device or mechanism with a high degree of certainty that failure of the pipe will not
fastened to the end of the test specimen so that internal pressure occur.
produces longitudinal tensile stresses in addition to hoop and
radial stresses in the test specimen. 3.1.12 long-term hydrostatic strength (LTHS)—the esti-
mated tensile stress in the wall of the pipe in the hoop direction
3.1.3 closure, restrained-end—a sealing device or mecha- due to internal hydrostatic pressure that, when applied
nism which relies on a rod through the test specimen or an cyclically, will cause failure of the pipe after a specified
external structure to resist the end thrust produced by internal number of cycles by Procedure A or a specified number of
pressure, thereby limiting the stresses in (straight) specimens to hours by Procedure B.
the hoop and radial directions only.
NOTE 6—The time for determination of LTHS or LTHP is specified by
3.1.4 failure—the transmission of the test fluid through the the product standard. Typically, the time is 150 × 106 or 657 × 106 cycles
body of the specimen in any manner, whether it be a wall for Procedure A and 100 000 or 438 000 h for Procedure B.
fracture, localized leaking, or weeping at a distance greater 3.1.13 long-term hydrostatic pressure (LTHP)—the esti-
than one diameter from the end closure. mated internal pressure of the piping product that, when
NOTE 4—For this practice, specimens which have not failed may be applied cyclically, will cause failure of the product after a
included as failures under the specific conditions given in 6.3, 9.3, and specified number of cycles by Procedure A or a specified
12.2. number of hours by Procedure B.
3.1.5 fiberglass pipe—a tubular product containing glass 3.1.14 pressure design basis (PDB)—an internal pressure
fiber reinforcement embedded in or surrounded by cured developed for fiberglass piping product by this practice and
thermosetting-resin; the composite structure may contain multiplied by a service design factor to obtain an HDP.
aggregate, granular or platelet fillers, thixotropic agents, 3.1.15 pressure rating (PR)—the estimated maximum pres-
pigments, or dyes; thermoplastic or thermosetting liners or sure in the pipe or fitting that can be exerted continuously with
coatings may be included. a high degree of certainty that failure of the piping component
3.1.6 reinforced polymer mortar pipe (RPMP)—a fiberglass will not occur.
pipe with aggregate. 3.1.16 service design factor—a number equal to 1.00 or less
3.1.7 reinforced thermosetting resin pipe (RTRP)—a fiber- that takes into consideration all the variables and degree of
glass pipe without aggregate. safety involved in a fiberglass piping installation so that when
3.1.8 hoop stress—the tensile stress in the wall of the piping it is multiplied by the HDB, an HDS and corresponding
product in the circumferential direction due to internal pres- pressure rating is obtained, or when it is multiplied by the PDB,
sure; hoop stress will be calculated by the ISO equation, as a pressure rating is obtained directly, such that in either case a
follows: satisfactory and safe piping installation results when good
quality components are used and the installation is made
S 5 P ~ D 2 t r ! /2t r (1)
properly.
where: 3.2 Definitions of Terms Specific to This Standard:
S = hoop stress, psi (kPa), 3.2.1 average outside diameter—a measurement obtained in
D = average reinforced outside diameter, in. (mm), accordance with Practice D3567 less any veil-reinforced and
P = internal pressure, psig (kPa), and nonreinforced exterior coating thicknesses.
tr = minimum reinforced wall thickness, in. (mm).
NOTE 5—Hoop stress should only be determined on straight hollow
3.2.2 minimum reinforced wall thickness—a measurement
cylindrical specimens. Product evaluation of more complex shapes may be obtained in accordance with Practice D3567, excluding veil-
based on pressure. reinforced and nonreinforced coating and lining thicknesses;
wall thickness of fittings is determined at the thinnest section of
the fitting body.
3
The last approved version of this historical standard is referenced on 4. Summary of Practice
www.astm.org.
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4.1 Procedure A consists of exposing a minimum of 18
4th Floor, New York, NY 10036, http://www.ansi.org. specimens of pipe or fittings, or both to cyclic internal

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pressures at a cycle rate of 25 cycles/min and at several actual anticipated product end-use conditions, from which a
different pressures. Elevated test temperatures are obtained by design basis for specific piping products and materials can be
circulating a hot liquid through the specimens or by testing in obtained. This practice defines an HDB for material in straight,
an air environment where the temperature is controlled. hollow cylindrical shapes where hoop stress can be easily
4.1.1 The cyclic LTHS or cyclic LTHP of a pipe or fitting is calculated, and a PDB for fittings and joints where stresses are
obtained by an extrapolation of a log-log plot of the linear more complex.
regression line for hoop stress or internal pressure versus 5.1.1 An alternative design practice based on initial strain
cycles to failure. versus time-to-failure relationships employs a strain basis HDB
4.1.2 The experimental basis for Procedure A shall be in instead of the stress basis HDB defined by this practice. The
accordance with Test Method D2143, which forms a part of strain basis HDB is most often used for buried pipe designs
this practice. When any part of the procedure is not in with internal pressures ranging from 0 to 250 psig (1.72 MPa).
agreement with Test Method D2143, the provisions of this
5.2 To characterize fiberglass piping products, it is neces-
practice shall be used.
sary to establish the stress versus cycles or time to failure, or
4.1.3 Joints between pipe and fitting specimens shall be
pressure versus cycles or time to failure relationships over
typical of those normally used for the kind of piping being
three or more logarithmic decades of time (cycles or hours)
tested.
within controlled environmental parameters. Because of the
4.2 Procedure B consists of exposing a minimum of 18 nature of the test and specimens employed, no single line can
specimens of pipe or fittings, or both, to constant internal adequately represent the data. Therefore, the confidence limits
hydrostatic pressures at differing pressure levels in a controlled shall be established.
environment and measuring the time to failure for each
pressure level. Test temperatures are obtained by immersing 5.3 Pressure ratings for piping of various dimensions at each
the specimens in a controlled-temperature water bath, by temperature may be calculated using the HDS determined by
testing in an air environment where the temperature is testing one size of piping provided that the same specific
controlled, or by circulating a temperature-controlled fluid process and material are used both for test specimens and the
through the specimen. piping in question.

NOTE 7—Testing in a water bath precludes the detection of weeping


5.4 Pressure ratings at each temperature for components
failure, (see 3.1.4) by either visual or electronic means. other than straight hollow shapes may be calculated using the
HDP determined by testing one size of piping provided that (1)
4.2.1 The static LTHS or static LTHP of a pipe or fitting is
the specific materials and manufacturing process used for the
obtained by an extrapolation of a log-log linear regression line
test specimens are used for the components, (2) for joints, the
for hoop stress or internal pressure versus time to failure.
joining materials and procedures used to prepare the test
4.2.2 The experimental basis for Procedure B shall be in
specimens are used for field joining, and (3) scaling of critical
accordance with either Test Method D1598 or Test Method
dimensions is related to diameter and pressure rating of the
F948, or both, which form a part of this practice. When any
component.
part of this practice is not in agreement with the selected
method, the provisions of this practice shall be used. NOTE 8—Scaling of fittings and joints should be further verified by
4.2.3 Joints between pipe and fitting specimens shall be short-time testing in accordance with Test Method D1599.
typical of those normally used for the kind of piping being 5.5 Results obtained at one set of environmental conditions
tested. shall not be used for other conditions, except that higher
4.3 The HDB category is obtained by categorizing the temperature data can be used for design basis assignment for
LTHS in accordance with Section 7 or Section 10. lower application temperatures. The design basis shall be
determined for each specific piping product. Design and
4.4 The PDB category is obtained by categorizing the LTHP processing can significantly affect the long-term performance
in accordance with Section 8 or Section 11. of piping products, and therefore shall be taken into consider-
4.5 Hydrostatic design stresses for pipe are obtained by ation during any evaluation.
multiplying the HDB values by a service design factor.
5.6 This practice is valid for a given pipe or fitting only so
4.6 Reconfirmation of HDB or PDB for Altered long as the specimens are truly representative of that material
Constructions—When a product already has an HDB or PDB and manufacturing process.
determined in accordance with this practice and a change of 5.6.1 Changes in materials or manufacturing processes will
process or material is made, a reconfirmation of the original necessitate a reevaluation as described in Section 12.
HDB or PDB shall be attempted in accordance with Section 12.
At least six specimens must be tested and meet the specified PROCEDURE A
criteria.
6. Long-Term Cyclic Hydrostatic Strength or Long-Term
5. Significance and Use Cyclic Hydrostatic Pressure
5.1 This practice is useful for establishing the hoop stress or 6.1 Select either free-end or restrained-end closures based
internal pressure versus time-to-failure relationships, under on the tensile stresses induced by internal pressure and the type
selected internal and external environments which simulate of joint in the intended piping system (see 1.4).

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D2992 − 18
6.2 Obtain a minimum of 18 failure stress-cycle points for as one specimen, using the normal joining procedures to join them
each selected temperature in accordance with Test Method together, with the fitting being at one end of the specimen. If the fitting
fails first, it can be cut off, and the test can be continued using the unfailed
D2143 except as follows: pipe with a mechanical end closure replacing the fitting. Should the pipe
6.2.1 Determine the average outside diameter and the mini- fail first, it can be recorded and repaired and the test continued until the
mum reinforced wall thickness in accordance with Practice fitting fails. If this recommendation is followed, it may enable the tester to
D3567. obtain failure points for both the pipe and the fitting while testing only one
specimen.
NOTE 9—Because of the need to cut the specimen, this determination
may be made on the failed test specimen. A corrected hoop stress is then 7. Cyclic Hydrostatic Design Basis
calculated for use in the analysis.
7.1 Calculate the cyclic LTHS at the specified time (150×
6.2.2 Elevated test temperatures are obtained by circulating 106 or 657 × 106 cycles) as described in Annex A1.
a heated test liquid through the specimens or by testing in a hot
air environment. In either case the test liquid shall be main- 7.2 If Sxy > 0 (see A1.4) consider the data unsuitable.
tained within 65°F (3°C) of the selected temperature. 7.3 Calculate r in accordance with A1.4.3. If r is less than
the applicable minimum value given in Table A1.1, consider
NOTE 10—Where elevated test temperatures are maintained by applying
heat to the circulating test liquid, work to date indicates that the ambient the data unsuitable.
air temperature need not be controlled. 7.4 If required, determine the cyclic HDB category in
6.2.3 The stress or pressure values for test shall be selected accordance with Table 1.
to obtain a distribution of failure points as follows:
8. Cyclic Pressure Design Basis
Cycles to Failure Failure Points
1000 to 10 000 at least 3 8.1 Use the procedures in 7.1, 7.2, and 7.3, using pressure in
10 000 to 100 000 at least 3 place of stress.
100 000 to 1 000 000 at least 3
1 000 000 to 10 000 000 at least 3 8.2 If required, determine the cyclic PDB category in
After 15 000 000 at least 1
accordance with Table 2.
Total at least 18
PROCEDURE B
6.3 Analyze the test results by using, for each specimen, the
logarithm of the stress or pressure in Section 6 and the 9. Long-Term Static Hydrostatic Strength
logarithm of the cycles to failure, as described in Annex A1.
9.1 Select either free-end or restrained-end closures based
NOTE 11—It is the custom of those testing fiberglass pipe to plot stress on the tensile stresses induced by internal pressure and the type
or pressure on the vertical (y) axis and time or cycles on the horizontal (x) of joint in the intended piping system (see 1.4).
axis.
9.2 Obtain a minimum of 18 failure points for each selected
6.3.1 A specimen which leaks within one diameter of an end temperature in accordance with Test Method D1598 or Test
closure may be: (1) included as a failure point if it lies above Method F948 except as follows:
the 95 % lower confidence limit curve; (2) repaired and testing 9.2.1 Determine the average outside diameter and the mini-
resumed provided the new leak is more than one diameter from mum reinforced wall thickness in accordance with Practice
a test joint, or (3) discarded and no data point recorded. D3567 (Note 9).
6.3.2 Those specimens that have not failed after more than 9.2.2 The inside environment for the pipe or fitting, test
15 000 000 cycles may be included as failures in establishing specimens, or both, shall be water. The outside environment
the regression line. Use of such data points may result in a shall be air or a controlled temperature water bath (See 7).
lower or higher cyclic LTHS or cyclic LTHP. In either case, the
lower confidence value requirements of Section 6 must be
TABLE 1 Hydrostatic Design Basis Categories by Procedure A or
satisfied.
Procedure B
NOTE 12—Non-failed specimens may be left under test and the Hydrostatic Design Basis
regression line recalculated as failures are obtained. Category Range of Calculated Values

6.3.3 Determine the final line for extrapolation by the psiA (kPa) psi (kPa)

method of least squares using the failure points along with


2500 (17 200) 2400 to 3010 (16 500 to 20 700)
those nonfailure points selected by the method described in 3150 (21 700) 3020 to 3820 (20 800 to 26 300)
6.3.1 and 6.3.2. Do not use failure points for stresses or 4000 (27 600) 3830 to 4790 (26 400 to 33 000)
pressures that cause failure in less than 500 cycles on the 5000 (34 500) 4800 to 5990 (33 100 to 40 900)
6300 (43 400) 6000 to 7590 (41 000 to 52 900)
average; determine these points by averaging the number of 8000 (55 200) 7600 to 9590 (53 000 to 65 900)
cycles-to-failure of tests made at the same stress or pressure 10 000 (68 900) 9600 to 11 990 (66 000 to 82 900)
level, that is, a stress within 6200 psi (1380 kPa) or a pressure 12 500 (86 200) 12 000 to 15 290 (83 000 to 105 900)
16 000 (110 000) 15 300 to 18 990 (106 000 to 130 900)
within 620 psig (138 kPa). Include in the report all failure 20 000 (138 000) 19 000 to 23 990 (131 000 to 169 900)
points excluded from the calculation by this operation and 25 000 (172 000) 24 000 to 29 990 (170 000 to 209 900)
identify them as being in this category. 31 500 (217 000) 30 000 to 37 990 (210 000 to 259 900)
40 000 (276 000) 38 000 to 47 000 (260 000 to 320 000)
NOTE 13—Since this procedure is for pipe or fittings, or both, it is A
Standard stress levels chosen in accordance with ISO 3, Series R10.
recommended that the pipe specimen and fitting be tested at the same time

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D2992 − 18
TABLE 2 Pressure Design Basis Categories by Procedure A or within 6200 psi (1380 kPa) or a pressure within 620 psi (138
Procedure B kPa). Include in the report all failure points excluded from the
Pressure Design Basis Category Range of Calculated Values calculation by this operation and identify them as being in this
psi (bar)A (kPa) psi (kPa) category (Note 12).
91 (6.3) (630) 87 to 110 (605 to 760)
116 (8) (800) 111 to 143 (765 to 990)
10. Static Hydrostatic Design Basis
150 (10) (1000) 144 to 172 (995 to 1180) 10.1 Calculate the static LTHS at the specified time
180 (12.5) (1250) 173 to 220 (1190 to 1510)
230 (16) (1600) 221 to 287 (1520 to 1980) (100 000 or 438 000 h) as described in Annex A1.
300 (20) (2000) 288 to 345 (1990 to 2380)
360 (25) (2500) 346 to 438 (2390 to 3020)
10.2 If Sxy > 0 (see A1.4), consider the data unsuitable.
460 (31.5) (3150) 439 to 556 (3030 to 3830) 10.3 Calculate r in accordance with A1.4.3. If r is less than
580 (40) (4000) 557 to 695 (3840 to 4790)
725 (50) (5000) 696 to 876 (4800 to 6040) the applicable minimum value given in Table A1.1, consider
910 (63) (6300) 877 to 1110 (6050 to 7680) the data unsuitable.
1160 (80) (8000) 1115 to 1380 (7690 to 9580)
1450 (100) (10 000) 1390 to 1720 (9590 to 11 800) 10.4 If required, determine the static HDB category in
1800 (125) (12 500) 1730 to 2220 (11 900 to 15 300) accordance with Table 1.
A
Standard pressures chosen in accordance with ISO 3, Series R10.
11. Static Pressure Design Basis
11.1 Use the procedures in 10.1, 10.2, and 10.3, using
Other media may be used, but the environment shall be given
pressure in place of stress.
in the test report. The test liquid shall be maintained within
65°F (3°C) of the test temperature (Note 10). 11.2 If required, determine the static PDB category in
9.2.3 The stress or pressure values for test shall be selected accordance with Table 2.
to obtain a distribution of failure points as follows:
Hours to Failure Failure Points
12. Reconfirmation of HDB or PDB
10 to 1000 at least 4 12.1 When a piping product has an existing HDB or PDB
1000 to 6000 at least 3
After 6000 at least 3 determined in accordance with Procedure A or Procedure B,
After 10 000 at least 1 any change in material, manufacturing process, construction,
or liner thickness shall necessitate a screening evaluation
Total at least 18
(reconfirmation) as described in 12.2, 12.3, 12.4, and 12.5.
9.2.4 Maintain the internal test pressure in each specimen
within 61 % of this pressure. Measure the time to failure to 12.2 Calculate and plot the 95 % confidence limits and the
within 62 % or 40 h, whichever is smaller. 95 % prediction limits of the original regression line in
accordance with A1.4 using only data obtained prior to the
9.3 Analyze the test results by using, for each failure point, change.
the logarithm of the stress or pressure in pound-force per
square inch or pound-force per square inch gage (kilopascals) NOTE 15—Prediction limits define the bounds for single observations,
whereas confidence limits define the bounds for the regression line.
and the logarithm of the time-to-failure in hours as described in NOTE 16—For 95 % confidence limits, there is a 2.5 % probability that
Annex A1 (Note 9). the mean value for the regression line may fall above the UCL and a 2.5 %
9.3.1 A specimen which leaks within one diameter of an end probability that the mean value for the regression line may fall below the
closure may be: (1) included as a failure point if it lies above LCL. For 95 % prediction limits, there is a 2.5 % probability that
the 95 % lower confidence limit curve; (2) repaired and testing individual data points may fall above the UPL and a 2.5 % probability that
individual data points may fall below the LPL.
resumed provided the new leak is more than one diameter from
a test joint, or (3) discarded and no failure point recorded. 12.3 From the original regression line, select stress or
9.3.2 Those specimens that have not failed after more than pressure levels for at least two sets of specimens, each set
10 000 h may be included as failures in establishing the consisting of 3 or more specimens tested at the same stress or
regression line. Use of such data points may result in a lower pressure level, that is, a stress within 6200 psi (1380 kPa) or
or higher static LTHS or static LTHP. In either case, the lower a pressure within 620 psi (138 kPa), as follows:
confidence value requirements of 9.3.1 must be satisfied. 12.3.1 For Procedure A:
Cycles to Failure Failure Points
NOTE 14—Non-failed specimens may be left under test and the (Average of Set)
regression line recalculated as failures are obtained.
15 000 to 3000 at least 3
9.3.3 Determine the final line for extrapolation by the More than 1 500 000 at least 3
method of least squares using the failure points along with
those nonfailure points selected by the method described in Total at least 6
9.3.1 and 9.3.2. Do not use failure points for stresses or For the purposes of reconfirmation, it is permitted to include
pressures that cause failure in less than 0.3 h on the average; as failures those specimens which have not failed after
determine these points by averaging the times-to-failure of 1 800 000 cycles provided they exceed the existing HDB or
tests made at the same stress or pressure level, that is, a stress PDB regression line.

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D2992 − 18
12.3.2 For Procedure B: engineer after evaluating fully the service conditions and the engineering
properties of the specific plastic pipe material under consideration.
Hours to Failure Failure Points
(Average of Set)
Recommended service design factors will not be developed or issued by
ASTM.
10 to 200 at least 3
More than 1000 at least 3 14. Pressure Rating
Total at least 6 14.1 For data based on hoop stress calculate the pressure
For the purposes of reconfirmation, it is permitted to include rating from the HDS by means of the ISO equation in 3.1.8 for
as failures those specimens which have not failed after 1200 h each diameter and wall thickness of pipe made from the
provided they exceed the existing HDB or PDB regression line. specific materials and constructions tested.
12.4 Consider any changes in the material or manufacturing 14.2 For data based on internal pressure, establish the
process minor and permissible if the results of 12.2 meet the pressure rating directly from the HDP for products made from
following criteria. the specific materials and constructions tested.
12.4.1 The average failure point for each stress or pressure 15. Report
level falls on or above the 95 % lower confidence limit of the
original regression line. 15.1 Report the following information:
12.4.2 The earliest individual failure point at each stress or 15.1.1 Complete identification of the specimen including
pressure level falls on or above the 95 % lower prediction limit material type, source, manufacturer’s name and code number,
of the original regression line. and previous significant history, if any.
12.4.3 The failure points are distributed about the originally 15.1.2 Specimen dimensions including nominal size, aver-
determined regression line. No more than two thirds of the age and minimum reinforced wall thickness, and average
individual failure points may fall below the original regression outside diameter, and liner material and liner thickness if
line. product is lined.
15.1.3 Fitting dimensions, including all items listed in
12.5 Data meeting the criteria of 12.4 may be assumed to be 15.1.2 and the type of fitting.
part of the original data set and it is permitted to determine a 15.1.4 Procedure used, (Procedure A or Procedure B), and
new regression line and HDB or PDB using all failure points. the ASTM designation of the underlying test method.
Specimens which have not failed after 1200 hours or 1 800 000 15.1.5 End closure type, free-end, or restrained-end.
cycles are not suitable for establishing a new regression line; 15.1.6 Test temperature.
however, it is permitted to use these points for the purpose of 15.1.7 Test environment inside and outside of the pipe.
reconfirmation. 15.1.8 A table of stresses or pressures in pound-force per
12.6 If the data fails to satisfy the criteria of 12.4, the square inch or pound-force per square inch gage (kilopascals)
changes are considered major and a new regression line must and the number of cycles to failure (Procedure A) or time-to-
be established. While the new test program is being conducted, failure in hours (Procedure B) of all the specimens tested; the
an interim HDB or PDB for the material or process change may nature of the failures, and the part that failed, that is, fitting or
be taken as the lower of the following: pipe. Specimens that are included as failures after they have
12.6.1 The 95 % lower confidence limit of the value ob- been under stress or pressure for more than 15 000 000 cycles
tained by extrapolating the failure points of 12.3.1 to or more than 10 000 h shall be indicated.
657 000 000 cycles (50 years), or the failure points of 12.3.2 to 15.1.9 The estimated LTHS or LTHP.
438 000 h (50 years) by the procedure in Annex A1. 15.1.10 The value for r.
12.6.2 The 95 % lower confidence limit of the original 15.1.11 The HDB or HDP.
regression line at 50 years. 15.1.12 The source of the HDB or PDB (7.1 or 7.2 for
Procedure A or 10.1 or 10.2 for Procedure B), and the
13. Hydrostatic Design Stress or Hydrostatic Design
categorized value in accordance with Table 1 or Table 2.
Pressure
15.1.13 Any unusual behavior observed in the tests.
13.1 Obtain the HDS or HDP by multiplying the HDB or 15.1.14 Dates of tests.
PDB as determined by Procedure A or Procedure B by a service 15.1.15 Name of laboratory and supervisor of tests.
design factor selected for the application on the basis of two
general groups of conditions. The first group considers the 16. Precision and Bias
manufacturing and testing variables, specifically normal varia- 16.1 The precision and bias of this practice for obtaining the
tions in the material, manufacture, dimensions, good handling HDB or PDB are as specified in Test Methods D1598, D2143,
techniques, and in the evaluation procedures in this method. and F948. This practice includes a statistical basis for evalu-
The second group considers the application or use, specifically ating the suitability of the data in Sections 6 and 9.
installation, environment, temperature, hazard involved, life
expectancy desired, and the degree of reliability selected. 17. Keywords
NOTE 17—It is not the intent of this practice to give service design 17.1 closure; cyclic pressure; design basis; fiberglass pipe;
factors. The service design factor should be selected by the design reconfirmation; static pressure

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D2992 − 18

ANNEX

(Mandatory Information)

A1. LEAST SQUARES CALCULATIONS FOR LONG-TERM HYDROSTATIC STRENGTH OR LONG-TERM HYDROSTATIC
PRESSURE

A1.1 General 1
5
n (y i (A1.2)
A1.1.1 The analysis is based on the following relationship:
y 5 a1bx (A1.1) x̄ = arithmetic mean of all xivalues:
1
where: 5
n (x i (A1.3)
y = one variable,
x = other variable, A1.4.2 Relevant Sums-of-Squares:
b = slope of the line, and A1.4.2.1 Calculate the following sums-of-squares and
a = intercept on the y axis. cross-products:
1
A1.1.2 A linear functional relationship analysis (sometimes S xy 5 ( ~ x 2 x̄ !~ y 2 ȳ !
i i (A1.4)
n
called “covariance analysis”) is used, subject to tests for the
sign (that is, “+” or “−”) of the slope and the coefficient of A1.4.2.2 If Sxy > 0, consider the data unsuitable for evalu-
correlation for the quantity of data available. The relevant ating the material; otherwise calculate also:
equations are given together with example data and results, on 1
the basis of which any other statistical computing package may S xx 5
n ( ~ x 2 x̄ !
i
2
(A1.5)
be used subject to validation by agreement with the example
results to within the indicated limits. 1
S yy 5
n ( ~y i 2 ȳ ! 2
(A1.6)
A1.1.3 For the purposes of this annex, a design service life
A1.4.3 Correlation of Data:
of 50 years has been assumed.
A1.4.3.1 Calculate the coefficient of correlation, r, from the
A1.2 Procedure for Analysis of Data following relationship:
A1.2.1 Use a linear functional relationship analysis to 2
~ S xy! 2
r 5 (A1.7)
analyze n pairs of data values (as y and x) to obtain the ~ S xx 3 S yy!
following information: r 5 =r 2

A1.2.1.1 The slope of line, b,


A1.4.3.2 If the value of r is less than the applicable
A1.2.1.2 The intercept on the y axis, a, minimum value given in Table A1.1as a function of n, reject
A1.2.1.3 The correlation coefficient, r, and the data; otherwise, proceed to A1.4.4.
A1.2.1.4 The predicted mean and the lower 95 % confi-
NOTE A1.1—The r minimum value assumes a two-sided 0.01 level of
dence and prediction intervals on the mean value. significance.
A1.3 Assignment of Variables A1.4.4 Functional Relationships:
A1.4.4.1 To find a and b for the functional relationship line,
A1.3.1 Let x be log10 t, where t is the time, in hours (or y = a + bx (Eq A1.1), first set:
cycles), and let y be log10 V, where V is the stress (or pressure)
value. λ5 S D S yy
S xx
(A1.8)
A1.4 Functional Relationship Equations and Method of
and then let:
Calculation
b 5 2 =λ (A1.9)
A1.4.1 Basic Statistics and Symbols:
A1.4.1.1 The following basic statistics and symbols are and then:
used: a 5 ȳ 2 bx̄ (A1.10)
NOTE A1.2—Since y = log10 V and x = log10 t, hence V = 10y, t = 10x
n = number of pairs of observed data values (Vi, ti), and the implied relationship for V in terms of t is therefore:
yi = log10 of Vi, where Vi is the stress (or pressure) at failure
of Observation i; i = 1, . . . n, V 5 10~ a1b3log 10 t !
xi = log10 of ti, where ti is the time to failure in hours of A1.4.5 Calculation of Variances:
Observation i; i = 1, . . .n, A1.4.5.1 If tL is the applicable time to failure, then set:
ȳ = arithmetic mean of all yi values:
x L 5 log10t L (A1.11)

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D2992 − 18
TABLE A1.1 Minimum Values for the Coefficient of Correlation, r, TABLE A1.2 Student’s “t” Value (Two-Sided 0.05 Level of
for Acceptable Data fromnPairs of Data Significance)
n n–2 Minimum, r n n–2 Student’st(0.05)
Number of variables Degrees of freedom Number of variables Degrees of freedom
3 1 0.9999 3 1 12.706
4 2 0.9900 4 2 4.303
5 3 0.9587 5 3 3.182
6 4 0.9172 6 4 2.776
7 5 0.8745 7 5 2.571
8 6 0.8343 8 6 2.447
9 7 0.7977 9 7 2.365
10 8 0.7646 10 8 2.306
11 9 0.7348 11 9 2.262
12 10 0.7079 12 10 2.228
13 11 0.6835 13 11 2.201
14 12 0.6614 14 12 2.179
15 13 0.6411 15 13 2.160
16 14 0.6226 16 14 2.145
17 15 0.6055 17 15 2.131
18 16 0.5897 18 16 2.120
19 17 0.5751 19 17 2.110
20 18 0.5614 20 18 2.101
21 19 0.5487 21 19 2.093
22 20 0.5368 22 20 2.086
23 21 0.5256 23 21 2.080
24 22 0.5151 24 22 2.074
25 23 0.5052 25 23 2.069
26 24 0.4958 26 24 2.064
27 25 0.4869 27 25 2.060
32 30 0.4487 32 30 2.042
37 35 0.4182 37 35 2.030
42 40 0.3932 42 40 2.021
47 45 0.3721 47 45 2.014
52 50 0.3542 52 50 2.009
62 60 0.3248 62 60 2.000
72 70 0.3017 72 70 1.994
82 80 0.2830 82 80 1.990
92 90 0.2673 92 90 1.987
102 100 0.2540 102 100 1.984

A1.4.5.2 Calculate, in turn, the following sequence of sta-


tistics. For i = 1 to i = n, the best fit, ξi, for true x, the best fit, the total variance, σy, for future values, yL, for y at xL using
Yi, for true y and the error variance, σδ, for x using Eq A1.12, the formula:
Eq A1.13, and Eq A1.14, respectively: σ y 2 5 σ n 2 1σ ε 2 (A1.22)
ξ i 5 $ λx i 1 ~ y i 2 a ! b % /2λ (A1.12) A1.4.5.5 Calculate the estimated standard deviation, σy, for
Y i 5 a1bξ i (A1.13) yL using the equation:
2
σy 5 ~σ 1σ ε 2 ! 0.5 (A1.23)
σδ 2 5 $ ( ~ y 2 Y ! 1λ ( ~ x
i i
2
i 2 ξ i! 2
%/$λ~n 2 2!% (A1.14) n

A1.4.5.3 Calculate the following quantities: and the predicted value, yL, for y at xL using the relationship:
y L 5 a1bxL (A1.24)
τ 5 bσ δ 2 /2S xy (A1.15)
D 5 2λbσ δ
2
/nSxy (A1.16) where a and b have the values obtained in accordance with
Eq A1.9 and Eq A1.10.
B 5 2Dx̄ ~ 11τ ! (A1.17)
A1.4.6 Calculation and Confidence Intervals:
A1.4.5.4 Calculate the following variances: the variance, C, A1.4.6.1 Calculate the lower 95 % prediction interval,
of b using the formula: yL 0.95, predicted for yL using the equation:
C 5 D ~ 11τ ! (A1.18) y L 0.95 5 y L 2 t v σ y (A1.25)
the variance, A, of a using the formula: where:
H
A 5 D x̄ 2 ~ 11τ ! 1
S xy
b J (A1.19) yL = value obtained in accordance with Eq A1.24 when xL is,
as applicable, the value in accordance with Eq A1.11
the variance, σn, of the fitted line at xL using the formula: appropriate to a design life of, for example, 50 years
(that is, xL = 5.6415 (h)) or to a time at which it is
σ n 2 5 A12BxL 1CxL 2 (A1.20)
desired to predict with 95 % confidence the minimum
the error variance, σε, for y using the formula: value for the next observation of V,
σy = value obtained in accordance with Eq A1.23, and
σ ε2 5 2λσ δ2 (A1.21)

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D2992 − 18

tv = applicable value for Student’s t for v = n − 2 df, as V L 5 10Y L (A1.27)


given in Table A1.2 for a two-sided 0.05 level of where:
significance (that is, mean 62.5 %).
YL = value obtained in accordance with Eq A1.24.
A1.4.6.2 Calculate the corresponding lower 95 % prediction
limit for V using the relationship: A1.4.6.4 Setting σy 2 = σn2 in Eq A1.22 will produce a
confidence interval for the line rather than a prediction interval
V L 0.95 5 10Y L 0.95 (A1.26)
for a future observation.
A1.4.6.3 The predicted mean value of V at time tL, that is,
VL, is given by the relationship:

APPENDIXES

(Nonmandatory Information)

X1. DATA ANALYSIS

X1.1 Hoop Stress versus Cycles-to-Failure or Time-to- X1.1.2 The main limitation of the use of hoop stress is that
Failure: it can only be applied to simple tubular-shaped specimens.
X1.1.1 Hoop stress is a more convenient parameter to use Therefore, its application has been mainly limited to materials
when attempting to predict long-term hydrostatic strength of a and a few products such as pipe and simple fittings like
material. Its use reduces scatter in the data by compensating for couplings.
varying dimensions in the test specimens. It effectively nor-
malizes pressure for variations in specimen geometry, and X1.2 Internal Pressure versus Cycles-to-Failure or Time-to-
reduces the variable to a material parameter. For this particular Failure—The use of internal pressure rather than stress extends
reason it has been widely used for evaluating the long-term the application of this practice to the prediction of service life
hydrostatic properties of plastic materials. Essentially, once a for many products of complex geometries which do not permit
value for HDS has been determined for a particular material the calculation of hoop stress. The logarithm of internal
and construction, that value can be used to effectively predict pressure is used in place of the logarithm of hoop stress in the
the long-term working pressure of tubular products by com- calculations.
pensating for the various product geometries.

X2. EXAMPLE CALCULATION

X2.1 Basic Data—The example data given in Table X2.1, b = –3.31731 × 10–2
together with the example analysis given in this appendix, can a = 3.782188
be used to validate statistical packages procedures. Because of
rounding errors, it is unlikely that there will be exact X2.5 Calculated Variances:
agreement, but acceptable procedures should agree within D = 4.84225 x 10–6
60.1 % of the results given in X2.5. B = –1.46896 x 10–5
C(variance of b)= 5.01271 × 10–6
X2.2 Sums of Squares:
Sxx = 0.798109 A(variance of a)= 4.66730 × 10–5
Syy = 8.78285 x 10–4 σn2(error variance for) x = 4.046696 x 10–5
Sxy = –0.024836 σ ε2(error variance for) y = 1.1601 × 10–4

X2.3 Coeffıcient of Correlation: X2.6 Confidence Limits—For N= 32 and Student’s t of


r = 0.938083 2.0423, the estimated mean and confidence and prediction
X2.4 Functional Relationships: intervals are given in Table X2.2.
λ = 1.100457 × 10–3

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TABLE X2.1 Example Data for Example Calculation
Data Time, Stress, Log Time, Log Stress, Data Stress, Log Time, Log Stress,
Point h psi h f Point Time, h psi h f

1 9. 5500. 0.95424 3.74036 17 1301. 4700. 3.11428 3.67210


2 13. 5500. 1.11394 3.74036 18 1430. 4800. 3.15534 3.68124
3 17. 5500. 1.23045 3.74036 19 1710. 4800. 3.23300 3.68124
4 17. 5500. 3.74036 20 2103. 4800. 3.32284 3.68124

5 104. 5200. 2.01703 3.71600 21 2220. 4500. 3.34635 3.65321


6 142. 5200. 2.15229 3.71600 22 2230. 4400. 3.34830 3.64345
7 204. 5200. 2.30963 3.71600 23 3816. 4700. 3.58161 3.67210
8 209. 5200. 2.32015 3.71600 24 4110. 4700. 3.61384 3.67210

9 272. 5000. 2.43457 3.69897 25 4173. 4600. 3.62043 3.66276


10 446. 5000. 2.64933 3.69897 26 5184. 4400. 3.71466 3.64345
11 466. 5000. 2.66839 3.69897 27 8900. 4600. 3.94939 3.66276
12 589. 4800. 2.77012 3.68124 28 8900. 4600. 3.94939 3.66276

13 669. 4700. 2.82543 3.67210 29 10900. 4500. 4.03743 3.65321


14 684. 5000. 2.83506 3.69897 30 10920. 4500. 4.03822 3.65321
15 878. 4600. 2.94349 3.66276 31 12340. 4500. 4.09132 3.65321
16 1299. 4800. 3.11361 3.68124 32 12340. 4500. 4.09132 3.65321

TABLE X2.2 Confidence Limits


Lower Lower
Confidence Prediction
Time, h Mean Interval Interval

1 6056 5864 5704


10 5611 5487 5309
100 5198 5129 4933
1000 4816 4772 4575
10 000 4462 4398 4233
100 000 4133 4037 3909
438 000 3936 3820 3711

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D2992 - 12)
that may impact the use of this standard. (May 15, 2018)

(1) Eliminated instances of non-mandator language. (3) Revised Tables A1.1 and A1.2 to unify range of variables
(2) Revised Section 12 on Reconfirmation of HDB or PDB. considered.

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of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D2997 − 15

Standard Specification for


Centrifugally Cast “Fiberglass” (Glass-Fiber-Reinforced
Thermosetting-Resin) Pipe1
This standard is issued under the fixed designation D2997; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D618 Practice for Conditioning Plastics for Testing


1.1 This specification covers machine-made glass-fiber- D883 Terminology Relating to Plastics
reinforced thermosetting-resin pressure pipe manufactured by D1598 Test Method for Time-to-Failure of Plastic Pipe
the centrifugal casting process. Included are a classification Under Constant Internal Pressure
system and requirements for materials, mechanical properties, D1599 Test Method for Resistance to Short-Time Hydraulic
dimensions, performance, test methods, and marking. Pressure of Plastic Pipe, Tubing, and Fittings
D1600 Terminology for Abbreviated Terms Relating to Plas-
NOTE 1—The term “fiberglass pipe” as described in Section 3 applies to tics
both reinforced thermosetting resin pipe (RTRP) and reinforced polymer
D2105 Test Method for Longitudinal Tensile Properties of
mortar pipe (RPMP).
NOTE 2—Pipe covered by this specification has been found suitable for “Fiberglass” (Glass-Fiber-Reinforced Thermosetting-
conveying gases, petroleum products, or corrosive fluids. Resin) Pipe and Tube
NOTE 3—For the purposes of this standard, polymer does not include D2143 Test Method for Cyclic Pressure Strength of
natural polymers. Reinforced, Thermosetting Plastic Pipe
1.2 The values given in parentheses are for information D2412 Test Method for Determination of External Loading
only. Characteristics of Plastic Pipe by Parallel-Plate Loading
D2992 Practice for Obtaining Hydrostatic or Pressure De-
NOTE 4—There is no known ISO equivalent to this standard.
sign Basis for “Fiberglass” (Glass-Fiber-Reinforced
1.3 The following precautionary caveat pertains only to the Thermosetting-Resin) Pipe and Fittings
test method portion, Section 7, of this specification: This D3567 Practice for Determining Dimensions of “Fiberglass”
standard does not purport to address all of the safety concerns, (Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
if any, associated with its use. It is the responsibility of the user Fittings
of this standard to establish appropriate safety, health, and F412 Terminology Relating to Plastic Piping Systems
environmental practices and determine the applicability of
regulatory limitations prior to use. 3. Terminology
1.4 This international standard was developed in accor-
3.1 Definitions—Definitions are in accordance with Termi-
dance with internationally recognized principles on standard-
nologies D883 and F412 and abbreviations with Terminology
ization established in the Decision on Principles for the
D1600, unless otherwise indicated.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical 3.2 Definitions of Terms Specific to This Standard:
Barriers to Trade (TBT) Committee. 3.2.1 aggregate, n—a siliceous sand conforming to the
requirements of Specification C33, except that the require-
2. Referenced Documents ments for gradation shall not apply.
2.1 ASTM Standards:2 3.2.2 centrifugal casting, n—a manufacturing process used
C33 Specification for Concrete Aggregates to produce tubular goods by applying resin and reinforcement
to the inside of a mold that is rotated and heated, subsequently
1
This specification is under the jurisdiction of ASTM Committee D20 on polymerizing the resin system. The outside diameter (OD) of
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced the finished pipe is fixed by the inside diameter (ID) of the
Plastic Piping Systems and Chemical Equipment. mold tube. The inside diameter of the pipe is determined by the
Current edition approved May 1, 2015. Published June 2015. Originally
papproved in 1971. Last previous edition approved in 2007 as D2997 – 01(2007)ε1.
amount of material introduced into the mold.
DOI: 10.1520/D2997-15.
2
3.2.3 fiberglass pipe, n—a tubular product containing glass-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
fiber reinforcements embedded in or surrounded by cured
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on thermosetting resin; the composite structure may contain
the ASTM website. aggregate, granular or platelet fillers, thixotropic agents,

*A Summary of Changes section appears at the end of this standard


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D2997 − 15
pigments, or dyes; thermoplastic or thermosetting liners or TABLE 1 Hydrostatic Design Basis Categories
coatings may be included. Cyclic Test Method Static Test Method

3.2.4 liner, n—the inner portion of the wall at least 0.005 in. Hoop Stress, Hoop Stress,
Designation Designation
psi (MPa) psi (MPa)
(0.13 mm) in thickness, as determined in 7.4 which does not
contribute to the strength in the determination of the hydro- A 2500 (17.2) Q 5000 (34.5)
static design basis. B 3150 (21.7) R 6300 (43.4)
C 4000 (27.6) S 8000 (55.2)
3.2.5 reinforced polymer mortar pipe (RPMP), n—a fiber- D 5000 (34.5) T 10 000 (68.9)
glass pipe with aggregate. E 6300 (43.4) U 12 500 (86.2)
F 8000 (55.2) W 16 000 (110)
3.2.6 reinforced thermosetting resin pipe (RTRP), n—a fi- G 10 000 (68.9) X 20 000 (138)
berglass pipe without aggregate. H 12 500 (86.2) Y 25 000 (172)
X 31 500 (217)
3.2.7 reinforced wall thickness, n—the total wall thickness
minus the liner or exterior surface resin layer thickness, or
both.

4. Classification strength, tensile modulus, and pipe stiffness. Thus, a complete


4.1 General—Pipe meeting this specification is classified by pipe designation code shall consist of four letters, two
type, grade, class, and hydrostatic design basis, and by a numerals, two letters, and four numerals.
secondary cell classification system that defines the basic 4.1.6.1 Example—RTRP-21CA-1334. Such a designation
mechanical properties of the pipe. These types, grades, classes, would describe a centrifugally cast, glass-fiber-reinforced,
hydrostatic design basis categories, and cell classification epoxy pipe having a nonreinforced epoxy liner; a long-term
designations are as follows: cyclic pressure strength level exceeding 2500 psi (17.2 MPa);
4.1.1 Types:—Type II a short-term rupture strength exceeding 4000 psi (27.6 MPa); a
Centrifugally cast pipe. longitudinal tensile strength exceeding 16 000 psi (110 MPa);
4.1.2 Grades:—Grade 1 a longitudinal tensile modulus exceeding 1.5 × 106 psi (10 300
Glass-fiber-reinforced epoxy-resin pipe. MPa); and a pipe stiffness of 72 psi (496 kPa).
Grade 2—Glass-fiber-reinforced polyester-resin pipe. NOTE 7—Although the Form and Style for ASTM Standards manual
Grade 3—Glass-fiber reinforced polydicyclopentadiene- requires that the type classification be roman numerals, it is recognized
resin pipe. that few companies have stencil-cutting equipment for this style of type,
Grade 8—Glass-fiber-reinforced polyester-resin mortar and it is therefore acceptable to mark the product type in arabic numbers.
pipe.
Grade 9—Glass fiber reinforced epoxy resin mortar pipe. 5. Materials
4.1.3 Classes:—Class A 5.1 General—The resins, reinforcements, colorants, fillers,
No liner. and other materials, when combined as a composite structure,
Class B—Polyester-resin liner, nonreinforced. shall produce a pipe that shall be classified in accordance to
Class C—Epoxy-resin liner, nonreinforced. this specification based on performance.
Class D—Polydicyclopentadiene-resin liner, nonreinforced.
NOTE 5—For the purposes of this classification, polyester resin includes
6. Requirements
vinylester resins, but the purchaser should consult with the manufacturer 6.1 Workmanship—The pipe shall be free from all defects,
to determine which resin is applicable for the specific conditions in which including indentations, delaminations, bubbles, pinholes, for-
the pipe will be used.
eign inclusions, and resin-starved areas which, as a result of
4.1.4 Hydrostatic Design Basis—Two methods of classify- their nature, degree, or extent, detrimentally affect the strength
ing the hydrostatic design basis of the pipe are provided. Pipe and serviceability of the pipe. The pipe shall be as uniform as
meeting this specification shall be classified using either the commercially practicable in color, opacity, density, and other
cyclic test method or the static test method, or both, and the physical properties. The pipe shall be round and straight, and
designations are shown in Table 1. Appendix X1 explains how the bore of the pipe shall be smooth and uniform. All pipe ends
to use the design basis categories shown in Table 1. shall be cut at right angles to the axis of the pipe, and any sharp
4.1.5 Mechanical Properties—Table 2 presents a cell clas- edges removed.
sification system for identifying the mechanical properties of
6.2 Dimensions and Tolerances:
pipe covered by this specification.
6.2.1 Outside Diameter—The outside diameter and toler-
NOTE 6—All possible combinations covered by the preceding classifi- ances of pipe meeting this specification shall conform to the
cation system may not be commercially available. requirements in Table 3, when determined in accordance with
4.1.6 Designation Code—The pipe designation code shall 7.4.
consist of the abbreviation RTRP or RPMP, followed by the 6.2.2 Wall Thickness—The minimum wall thickness of pipe
type and grade in Arabic numerals, the class and static or cyclic furnished under this specification shall not at any point be less
hydrostatic design basis level in capital letters, and four Arabic than 87.5 % of the nominal wall thickness published in the
numbers identifying, respectively, the cell classification desig- manufacturer’s literature, current at the time of purchase, when
nations of the short-term rupture strength, longitudinal tensile measured in accordance with 7.4.

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D2997 − 15
TABLE 2 Physical Property Requirements
Designation Cell Limits
Order Mechanical Property
Number 0A 1 2 3 4 5 6

1 Short time rupture strength hoop tensile stress, min, psi — 4000 12 000 22 000 30 000 40 000 50 000
(MPa) (27.6) (82.7) (152) (207) (276) (345)
2 Longitudinal tensile strength, min, psi — 2000 8000 16 000 22 000 30 000 40 000
(MPa) (13.8) (55.2) (110) (152) (207) (276)
3 Longitudinal tensile modulus, min, psi × 106 — 0.6 1.3 1.5 1.9 2.5 3.0
(MPa) (4100) (9000) (10 300) (13 100) (17 200) (20 700)
4 Pipe stiffness at 5 % deflection, psi — 9 18 36 72 144 288
(kPa) (62) (124) (248) (496) (993) (1986)
A
0 = Unspecified.

TABLE 3 Outside Dimensions and Tolerances NOTE 8—For individual orders, only those additional tests and number
Nominal Pipe of tests specifically agreed upon between the purchaser and the seller need
in. (mm) be conducted.
Size, in.
7.4 Dimensions and Tolerances—Determine in accordance
1 1.315 ± 0.009 (33.401 ± 0.229)
1 1 ⁄2 1.900 ± 0.009 (48.260 ± 0.229)
with Practice D3567.
2 2.375 ± 0.012 (60.325 ± 0.305) 7.5 Long-Term Cyclic Pressure Strength—Determine in ac-
2 1 ⁄2 2.875 ± 0.012 (73.025 ± 0.305)
3 3.500 ± 0.012 (88.900 ± 0.305) cordance with Procedure A of Practice D2992.
4 4.500 ± 0.015 (114.300 ± 0.381) 7.6 Long-Term Static Pressure Strength—Determine in ac-
6 6.625 ± 0.025 (168.275 ± 0.635)
8 8.625 ± 0.025 (219.075 ± 0.635) cordance with Procedure B of Practice D2992.
10 10.750 ± 0.025 (273.050 ± 0.635)
12 12.750 ± 0.025 (323.850 ± 0.635)
7.7 Short-Term Rupture Strength—Determine in accordance
14 14.000 ± 0.035 (355.600 ± 0.889) with Test Method D1599.
7.8 Longitudinal Tensile Properties—Determine in accor-
dance with Test Method D2105.
6.2.3 Liner Thickness—Except for Class A unlined products,
all other classes shall have a minimum liner thickness of 0.005 7.9 Pipe Stiffness—Determine in accordance with Test
in. (5 mil), when measured in accordance with 7.4. Method D2412. The reported stiffness shall be based on 5 %
deflection.
6.3 Performance—Pipe meeting this specification shall be
categorized by a long-term static or cyclic hydrostatic design 8. Certification
basis shown in Table 1, when tested in accordance with 7.5 and 8.1 When agreed upon in writing by the purchaser and the
7.6. Additionally, the pipe shall meet the applicable cell limit seller, a certification shall be made the basis of acceptance of
requirements for short-term rupture strength, longitudinal ten- the material. This shall consist of a copy of the manufacturer’s
sile strength, tensile modulus, and pipe stiffness described in test report or a statement by the seller accompanied by a copy
Table 2, when tested in accordance with 7.7, 7.8, and 7.9. of the test results, that the material has been sampled, tested,
7. Test Methods and inspected in accordance with the provisions of the speci-
fication. Each certification so furnished shall be signed by an
7.1 Conditioning—Condition the test specimens at 23 6 authorized agent of the seller or the manufacturer.
2°C (73.4 6 3.6°F) and 50 6 10 % relative humidity for not
less than 48 h prior to test, in accordance with Procedure A of 8.2 When original identity cannot be established, certifica-
Practice D618, for those tests where conditioning is required, tion can only be based on the sampling procedure provided by
and in all cases of disagreement. the applicable specification.
7.2 Test Conditions—Conduct the tests in the Standard 9. Marking
Laboratory Atmosphere of 23 6 2°C (73.4 6 3.6°F) and 50 6 9.1 Each piece shall be marked at least once and at lengths
10 % relative humidity, unless otherwise specified in the test of at least every 15 ft. Each piece of pipe shall be marked with
specification. the following information in such a manner that it remains
7.3 Sampling—Samples of pipe to determine conformance legible under normal handling and installation practices:
of the material to be short-term rupture requirements shown in 9.1.1 Nominal pipe size (for example, 2 in.),
Table 2 shall be taken at random on a weekly basis or on each 9.1.2 Identification of fiberglass pipes in accordance with
production run, whichever is the most frequent. The rate of the designation code given in Section 5,
sampling for the other tests listed shall be in accordance with 9.1.3 This designation, D2997, with which the pipe
the accepted statistical practice and as agreed upon between the complies, and
purchaser and the seller. 9.1.4 Manufacturer’s name (or trademark).

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APPENDIX

(Nonmandatory Information)

X1. HYDROSTATIC DESIGN BASIS, CATEGORIES, SERVICE FACTORS, AND PRESSURE RATINGS

X1.1 Hydrostatic Design Basis TABLE X1.2 Hydrostatic Design Basis Categories by
Procedure B
X1.1.1 The hydrostatic design basis is the estimated long-
Hydrostatic Design
term hydrostatic strength on which service factors (1.0 or less) Basis Category,
Range of Calculated Values,
psi (MPa)
are applied to obtain a hydrostatic design stress. The long-term psi (MPa)
hydrostatic strength is obtained by Practice D2992. In Practice
D2992, either Procedure A using data obtained in accordance 5000 (34.5) 4800 to 5900 (33.1 to 40.7)
6300 (43.4) 6000 to 7500 (41.4 to 51.7)
with Test Method D2143 or Procedure B using data obtained in 8000 (55.2) 7600 to 9500 (52.4 to 65.5)
accordance with Test Method D1598 is used to determine the 10 000 (68.9) 9600 to 11 900 (66.2 to 82.0)
12 500 (86.2) 12 000 to 15 200 (82.7 to 105)
long-term hydrostatic strength extrapolated at 50 years.
16 000 (110) 15 300 to 18 900 (106 to 130)
X1.1.2 The long-term hydrostatic strength is the estimated 20 000 (138) 19 000 to 23 000 (131 to 159)
25 000 (172) 24 000 to 29 000 (166 to 200)
tensile stress in the wall of the pipe in the hoop orientation due 31 500 (217) 30 000 to 38 000 (207 to 262)
to internal hydrostatic pressure that will cause failure after 50
years (657 × 106 pressure cycles by Procedure A or 438 000 h
of static pressure by Procedure B). environment, temperature, hazard involved, life expectance
desired, and the degree of reliability selected.
X1.2 Hydrostatic Design Basis Categories
NOTE X1.1—It is not the intent of this specification to give service
X1.2.1 The hydrostatic design basis is obtained by catego- (design) factors. The service (design) factor should be selected by the
rizing the long-term strength in accordance with Table X1.1 or design engineer after evaluating fully the service conditions and the
Table X1.2. engineering properties of the specific pipe material under consideration.
Recommended service (design) factors will not be developed or issued by
X1.3 Service (Design) Factor ASTM.

X1.3.1 The service (design) factor is a number equal to 1.00 X1.4 Hydrostatic Design Stress
or less that takes into consideration all the variables and degree X1.4.1 The hydrostatic design stress is the estimated
of safety involved in a fiberglass pressure piping installation, maximum tensile stress in the wall of the pipe in the circum-
and is selected for the application on the basis of two general ferential orientation as a result of internal hydrostatic pressure
groups of conditions. that can be applied continuously with a high degree of certainty
X1.3.2 The first group considers the manufacturing and that failure will not occur. It is obtained by multiplying the
testing variables, specifically normal variations in the material, hydrostatic design basis as determined by Procedure A or
manufacture, dimensions, good handling techniques, and in the Procedure B by the service (design) factor.
evaluation procedures of this method. The second group X1.5 Pressure Rating
considers the application or use, specifically installation,
X1.5.1 The pressure rating is the estimated maximum pres-
TABLE X1.1 Hydrostatic Design Basis Categories by
sure that the medium in the pipe can exert continuously with a
Procedure A high degree of certainty that failure of the pipe will not occur.
Hydrostatic Design
Range of Calculated Values,
X1.5.2 The pressure rating for each diameter and wall
Basis Category, thickness of pipe and fitting is calculated from the hydrostatic
psi (MPa)
psi (MPa)
design stress for the specific pipe by means of the ISO formula:
2500 (17.2) 2400 to 3010 (16.5 to 20.8) S 5 P ~ D 2 t ! /2t
3150 (21.7) 3020 to 3820 (20.8 to 26.3)
4000 (27.6) 3830 to 4790 (26.4 to 33.0) where:
5000 (34.5) 4800 to 5900 (33.1 to 40.7)
6300 (43.4) 6000 to 7500 (41.4 to 51.7) S = hoop stress,
8000 (55.2) 7600 to 9500 (52.4 to 65.5) P = internal pressure,
10 000 (68.9) 9600 to 11 900 (66.2 to 82.0) D = average outside diameter, and
12 500 (86.2) 12 000 to 15 200 (82.7 to 105)
t = minimum reinforced wall thickness.

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SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue,
D2997–99(2007)ε1, that may impact this standard. (May 1, 2015)

(1) Removed reference to ASTM D2310. (3) Corrected instance of non-mandatory language in 4.1.4.
(2) Added Note 5, defining vinylester resins as a subset of (4) Humidity tolerances in Section 7 changed to comply with
polyester resins. most recent version of ASTM D618.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3262 − 20

Standard Specification for


“Fiberglass” (Glass-Fiber-Reinforced Thermosetting-Resin)
Sewer Pipe1
This standard is issued under the fixed designation D3262; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 2. Referenced Documents


1.1 This specification covers machine-made fiberglass pipe, 2.1 ASTM Standards:2
8 in. (200 mm) through 156 in. (4000 mm), intended for use in C33 Specification for Concrete Aggregates
gravity-flow systems for conveying sanitary sewage, storm D638 Test Method for Tensile Properties of Plastics
water, and some industrial wastes. Both glass-fiber-reinforced D695 Test Method for Compressive Properties of Rigid
thermosetting-resin pipe (RTRP) and glass-fiber-reinforced Plastics
polymer mortar pipe (RPMP) are fiberglass pipes. D883 Terminology Relating to Plastics
NOTE 1—For the purposes of this standard, polymer does not include D1600 Terminology for Abbreviated Terms Relating to Plas-
natural polymers. tics
1.2 Although this specification is suited primarily for pipes D2412 Test Method for Determination of External Loading
to be installed in buried applications, it is acceptable to apply Characteristics of Plastic Pipe by Parallel-Plate Loading
it to the extent applicable for other installations such as, but not D2584 Test Method for Ignition Loss of Cured Reinforced
limited to, jacking, tunnel lining and sliplining rehabilitation of Resins
existing pipelines. D2992 Practice for Obtaining Hydrostatic or Pressure De-
sign Basis for “Fiberglass” (Glass-Fiber-Reinforced
NOTE 2—There is no known ISO equivalent to this standard. Thermosetting-Resin) Pipe and Fittings
1.3 The values stated in inch-pound units are to be regarded D3567 Practice for Determining Dimensions of “Fiberglass”
as the standard. The values given in parentheses are for (Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
information only. Fittings
1.4 The following safety hazards caveat pertains only to the D3681 Test Method for Chemical Resistance of “Fiberglass”
test method portion, Section 8, of this specification. This (Glass–Fiber–Reinforced Thermosetting-Resin) Pipe in a
standard does not purport to address all of the safety concerns, Deflected Condition
if any, associated with its use. It is the responsibility of the user D3892 Practice for Packaging/Packing of Plastics
of this standard to establish appropriate safety, health, and D4161 Specification for “Fiberglass” (Glass-Fiber-
environmental practices and determine the applicability of Reinforced Thermosetting-Resin) Pipe Joints Using Flex-
regulatory limitations prior to use. ible Elastomeric Seals
1.5 This international standard was developed in accor- F412 Terminology Relating to Plastic Piping Systems
dance with internationally recognized principles on standard- F477 Specification for Elastomeric Seals (Gaskets) for Join-
ization established in the Decision on Principles for the ing Plastic Pipe
Development of International Standards, Guides and Recom- 2.2 AWWA Standard:
mendations issued by the World Trade Organization Technical Standard C-950, Glass-Fiber Reinforced Thermosetting
Barriers to Trade (TBT) Committee. Resin Pipe3

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Plastic Piping Systems and Chemical Equipment. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved March 1, 2020. Published March 2020. Originally the ASTM website.
3
approved in 1973. Last previous edition approved in 2016 as D3262 – 16. DOI: Available from American Water Works Association (AWWA), 6666 W. Quincy
10.1520/D3262-20. Ave., Denver, CO 80235, http://www.awwa.org.

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D3262 − 20
3. Terminology cially available. The purchaser should determine for himself or consult
with the manufacturer for the proper type, liner, grade, and stiffness of
3.1 Definitions: pipe to be used under the installation and operating conditions that will
3.1.1 General—Unless otherwise indicated, definitions are exist for the project in which pipe is to be used.
in accordance with Terminology D883 or Terminology F412,
4.2 Designation Requirements—The pipe materials designa-
and abbreviations are in accordance with Terminology D1600.
tion code shall consist of the standard designation, ASTM
3.2 Definitions of Terms Specific to This Standard: D3262, followed by type, liner, and grade indicated in Arabic
3.2.1 fiberglass pipe—tubular product containing glass fiber numerals, and pipe stiffness by a capital letter. Table 1 presents
reinforcements embedded in or surrounded by cured thermo- a summary of the designation requirements. Thus a complete
setting resin. material code shall consist of ASTM D3262, three numerals,
3.2.1.1 Discussion—The composite structure may contain and a capital letter.
aggregate, granular, or platlet fillers, thixotropic agents,
pigments, or dyes, and thermoplastic or thermosetting liners. NOTE 4—Examples of the designation codes are as follows: (1) ASTM
D3262-1-1-3-A for glass–fiber–reinforced aggregate and polyester resin
3.2.2 flexible joint —a joint that is capable of axial displace- mortar pipe with a reinforced thermoset liner and an unreinforced
ment or angular rotation, or both. polyester resin and sand surface layer having a minimum pipe stiffness of
3.2.3 liner—a resin layer, with or without filler or 9 psi (62 kPa). (2) ASTM D3262-4-2-6-C for glass–fiber–reinforced
epoxy resin pipe with an unreinforced thermoset liner, no surface layer,
reinforcement, or both, forming the interior surface of the pipe. having a minimum pipe stiffness of 36 psi (248 kPa).
3.2.4 qualification test—one or more tests used to prove the NOTE 5—Although the Form and Style for ASTM Standards manual
design of a product. Not a routine quality control test. requires that the type classification be roman numerals, it is recognized
that few companies have stencil-cutting equipment for this style of type,
3.2.5 reinforced polymer mortar pipe (RPMP)—fiberglass and it is therefore acceptable to mark the product type in Arabic numbers.
pipe with aggregate.
3.2.6 reinforced thermosetting resin pipe (RTRP)— 5. Materials and Manufacture
fiberglass pipe without aggregate.
5.1 General—The thermosetting resins, glass fiber
3.2.7 rigid joint— a joint that is not capable of axial reinforcements, fillers, and other materials, when combined as
displacement or angular rotation. a composite structure, shall produce piping products that meet
3.2.8 surface layer—a resin layer, with or without filler or the performance requirements of this specification.
reinforcement, or both, applied to the exterior surface of the
pipe structural wall. 5.2 Wall Composition—The basic structural wall composi-
tion shall consist of a thermosetting resin, glass-fiber
4. Classification reinforcement, and if used, an aggregate filler.
4.1 General—This specification covers fiberglass sewer 5.2.1 Resin—A thermosetting polyester or epoxy resin, with
pipe defined by raw materials in the structural wall (type) and or without filler.
liner, surface layer material (grade), and pipe stiffness. Table 1 5.2.2 Reinforcement—A commercial grade of glass fibers
lists the types, liners, grades, and stiffnesses covered. compatible with the resin used.
NOTE 3—All possible combinations of types, liners, grades, and 5.2.3 Aggregate—A siliceous sand conforming to the re-
stiffnesses may not be commercially available. It is acceptable to add quirements of Specification C33, except that the requirements
additional types, liners, grades, and stiffnesses as they become commer- for gradation shall not apply.

TABLE 1 General Designation Requirements for Fiberglass Sewer Pipe


Desig-
nation Property Cell LimitsA
Order

1 Type 1 2 3 4
glass-fiber-reinforced glass-fiber-resin-reinforced glass-fiber-reinforced glass-fiber-reinforced
thermosetting polyesterB resin thermosetting polyesterB resin thermosetting epoxy resin thermosetting epoxy resin
mortar (RPMP polyesterB ) (RTRP polyesterB ) mortar (RPMP epoxy) (RTRP epoxy)
2 Liner 1 2 3 4
reinforced thermoset liner non-reinforced thermoset liner thermoplastic liner no liner

3 Grade 1 2 3 4 5 6
polyesterB resin polyesterB resin polyesterB resin and epoxy resin surface epoxy resin surface no surface layer
surface layer— surface layer— sand surface layer layer—reinforced layer—non-reinforced
reinforced nonreinforced non-reinforced

4 Pipe stiffness A B C DA,B


psi (kPa) 9 (62) 18 (124) 36 (248) 72 (496)
A
This cell-type format provides the means of identification and specification of piping materials. This cell-type format, however, is subject to misapplication since
unobtainable property combinations can be selected if the user is not familiar with non-commercially available products. The manufacturer needs to be consulted.
B
For the purposes of this specification, polyester includes vinyl ester resins.

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5.3 Liner and Surface Layer—A liner or surface layer, or 6. Requirements
both, when incorporated into or onto the pipe, shall meet the 6.1 Workmanship—Each pipe shall be free from all defects
structural requirements of this specification. including indentations, delaminations, bubbles, pinholes,
5.4 Joints—The pipe shall have a joining system that shall cracks, pits, blisters, foreign inclusions, and resin-starved areas
provide for fluid tightness for the intended service condition. that, due to their nature, degree, or extent, detrimentally affect
Restrained or unrestrained and flexible or rigid joints are the strength and serviceability of the pipe. The pipe shall be as
acceptable depending on the specific configuration and design uniform as commercially practicable in color, opacity, density,
conditions. and other physical properties.
5.4.1 Unrestrained—Pipe joints capable of withstanding 6.1.1 The inside surface of each pipe shall be free of bulges,
internal pressure but not longitudinal tensile loads. dents, ridges, and other defects that result in a variation of
5.4.1.1 Coupling or Bell-and-Spigot Gasket Joints, with a inside diameter of more than 1⁄8 in. (3.2 mm) from that obtained
groove either on the spigot or in the bell to retain an on adjacent unaffected portions of the surface. No glass fiber
elastomeric gasket that shall be the sole element of the joint to reinforcement shall penetrate the interior surface of the pipe
provide watertightness. For typical joint detail see Fig. 1. wall.
5.4.1.2 Mechanical Coupling Joint, with elastomeric seals. 6.1.2 Joint sealing surfaces shall be free of dents, gouges,
5.4.1.3 Butt Joint, with laminated overlay. and other surface irregularities that will affect the integrity of
5.4.1.4 Flanged Joint, both integral and loose ring. the joints.
5.4.2 Restrained—Pipe joints capable of withstanding inter-
nal pressure and longitudinal tensile loads. 6.2 Dimensions:
5.4.2.1 Joints similar to those in 5.4.1.1 with supplemental 6.2.1 Pipe Diameters—The pipe shall be supplied in the
restraining elements. nominal diameters shown in Table 2 or Table 3. The tolerances
5.4.2.2 Butt Joint, with laminated overlay. shall be as shown in Table 2 or Table 3, when measured in
5.4.2.3 Bell-and-Spigot, with laminated overlay. accordance with 8.1.1.
5.4.2.4 Bell-and-Spigot, adhesive-bonded joint: Three types 6.2.2 Lengths—Pipe shall be supplied in nominal lengths of
of adhesive-bonded joints are permitted by this standard as 10, 20, 30, 40, and 60 ft (3.05, 6.10, 9.15, 12.19, and 18.29 m).
follows: The actual laying length shall be the nominal length 62 in.
(1) Tapered bell-and-spigot, an adhesive joint that is manu- (651 mm), when measured in accordance with 8.1.2. At least
factured with a tapered socket for use in conjunction with a 90 % of the total footage of any one size and stiffness,
tapered spigot and a suitable adhesive. excluding special-order lengths, shall be furnished in the
(2) Straight bell-and-spigot, an adhesive joint that is manu- nominal lengths specified by the purchaser. Random lengths, if
factured with an untapered socket for use in conjunction with furnished, shall not vary from the nominal lengths by more
an untapered spigot and a suitable adhesive. than 5 ft (1.53 m), or 25 %, whichever is less.
(3) Tapered bell and straight spigot, an adhesive joint that 6.2.3 Wall Thickness—The average wall thickness of the
is manufactured with a tapered socket for use with an unta- pipe shall not be less than the nominal wall thickness published
pered spigot and a suitable adhesive. in the manufacturer’s literature current at the time of purchase,
5.4.2.5 Flanged Joint, both integral and loose ring. and the minimum wall thickness at any point shall not be less
5.4.2.6 Mechanical Coupling, an elastomeric sealed cou- than 87.5 % of the nominal wall thickness when measured in
pling with supplemental restraining elements. accordance with 8.1.3.
5.4.2.7 Threaded joints. 6.2.4 Squareness of Pipe Ends—All points around each end
of a pipe unit shall fall within 61⁄4 in. (66.4 mm) or 60.5 %
NOTE 6—It is acceptable to add other types of joints as they become
commercially available.
of the nominal diameter of the pipe, whichever is greater, to a
NOTE 7—Restrained joints typically increase service loads on the pipe plane perpendicular to the longitudinal axis of the pipe, when
to greater than those experienced with unrestrained joints. The purchaser measured in accordance with 8.1.4.
is cautioned to take into consideration all conditions in the anticipated
service and to consult the manufacturer regarding the suitability of a 6.3 Chemical Requirements:
particular type and class of pipe for service with restrained joint systems. 6.3.1 Long-Term—Pipe specimens, when tested in accor-
5.5 Gaskets—Elastomeric gaskets used with this pipe shall dance with 8.2.1, shall be capable of being deflected, without
conform to the requirements of Specification F477, except that failure, at the 50 year strain level given in Table 4 when
composition of the elastomer shall be as agreed upon between exposed to 1.0 N sulfuric acid.
the purchaser and the supplier for the particular exposure to NOTE 8—See Appendix X1 for derivation of the minimum sewer pipe
oily or aggressive chemical environments. chemical requirements given in Table 4.

FIG. 1 Typical Joints

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TABLE 2 Nominal Inside Diameters (ID) and Tolerances Inside Diameter Control Pipe
Inch-Pound Series SI Series
Nominal Tolerance, in. Nominal Metric ID Range,B mm ToleranceB on
Diameter,A in. Diameter,B mm Minimum Maximum Declared ID, mm
8 ±0.25 200 196 204 ±1.5
10 ±0.25 250 246 255 ±1.5
12 ±0.25 300 296 306 ±1.8
14 ±0.25 400 396 408 ±2.4
15 ±0.25 500 496 510 ±3.0
16 ±0.25 600 595 612 ±3.6
18 ±0.25 700 695 714
20
21
±0.25
±0.25
800
900
795
895
816
918
J ±4.2

24 ±0.25 1000 995 1020

6
27 ±0.27 1200 1195 1220
30 ±0.30 1400 1395 1420
33 ±0.33 1600 1595 1620 ±5.0
36 ±0.36 1800 1795 1820
39 ±0.39 2000 1995 2020
42 ±0.42 (2200) 2195 2220
45
48
51
54
60
±0.45
±0.48
±0.51
±0.54
±0.60
2400
(2600)
2800
(3000)
3200
2395
2595
2795
2995
3195
2420
2620
2820
3020
3220
6 ±6.0

66
72
78
84
±0.66
±0.72
±0.78
±0.84
(3400)
3600
(3800)
4000
3395
3595
3795
3995
3420
3620
3820
4020
6 ±7.0

90 ±0.90 ... ... ... ...


96 ±0.96 ... ... ... ...
102 ±1.00 ... ... ... ...
108 ±1.00 ... ... ... ...
114 ±1.00 ... ... ... ...
120 ±1.00 ... ... ... ...
132 ±1.00 ... ... ... ...
144 ±1.00 ... ... ... ...
156 ±1.00 ... ... ... ...
A
Inside diameters other than those shown shall be permitted by agreement between the purchaser and the supplier.
B
Values are taken from International Standards Organization documents. Parentheses indicate non-preferred diameters.

NOTE 9—The calculations in Table 4 and Appendix X1 assume that the deflection Level B in accordance with Table 6, there shall be no
neutral axis is at the pipe wall midpoint. For pipe wall constructions that indication of structural damage as evidenced by interlaminar
produce an altered neutral axis position, 2y shall be substituted for t to
evaluate results and establish requirements. (y is the maximum distance
separation, separation of the liner or surface layer (if incorpo-
from the neutral axis to the pipe surface.) rated) from the structural wall, tensile failure of the glass fiber
reinforcement, and fracture or buckling of the pipe wall.
6.3.2 Control Requirements—Test pipe specimens periodi-
cally in accordance with 8.2.2, following the procedure of NOTE 11—This is a visual observation (made with the unaided eye) for
8.2.2.1, or alternatively, the procedure of 8.2.2.2. quality control purposes only and should not be considered a simulated
service test. Table 6 values are based on an in-use long-term deflection
6.3.2.1 When the procedure of 8.2.2.1 is used, the following limit of 5 % and provide an appropriate uniform safety margin for all pipe
three criteria must be met: (a) the average failure time at each stiffnesses. Since the pipe stiffness values (F/∆y) shown in Table 5 vary,
strain level must fall at or above the lower 95 % confidence the percent deflection of the pipe under a given set of installation
limit of the originally determined regression line, (b) all conditions will not be constant for all pipes. To avoid possible
specimen-failure times shall be greater than the lower 95 % misapplication, take care to analyze all conditions that might affect
performance of the installed pipe.
prediction limit of the originally determined regression line,
and (c) one third or more of the specimen-failure times must be 6.4.1 For other pipe stiffness levels, it is acceptable to
on or above the originally determined regression line. compute appropriate values for level A and level B deflections
(Table 6) as follows:
NOTE 10—Determine the lower 95 % confidence limit and the lower 95
% prediction limit in accordance with Annex A1.
6.3.2.2 When the alternative procedure of 8.2.2.2 is used,
Level A at new PS 5 S 72
new PS D 0.33

~9! (1)

failure shall not occur in any specimen. Level B at new PS 5 new Level A÷0.6
6.4 Stiffness—Each length of pipe shall have sufficient 6.4.2 For products that have use limits of other than 5 %
strength to exhibit the minimum pipe stiffness (F/∆y) specified long-term deflection, it is acceptable to proportionally adjust
in Table 5, when tested in accordance with 8.3. At deflection Level A and Level B deflections (Table 6) to maintain
Level A in accordance with Table 6, there shall be no visible equivalent in-use safety margins. For example, a 4 % long-
damage in the test specimen evidenced by surface cracks. At term limiting deflection would result in a 20 % reduction of

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TABLE 3 Nominal Outside Diameters (OD) and Tolerances
NOTE 1—The external diameter of the pipe at the spigots shall be within the tolerances given in the table, and the manufacturer shall declare his
allowable maximum and minimum spigot diameters. Some pipes are manufactured such that the entire pipe meets the OD tolerances while other pipes
meet the tolerances at the spigots, in which case, if such pipes are cut (shortened) it is possible that the ends will need to be calibrated to the tolerances.

Metric Ductile Iron Pipe Tolerance Upper, Tolerance Lower, International O.D., Tolerance Upper, Tolerance Lower,
Pipe Size, mm Equivalent, mm mm mm mm mm mm
200 220.0 +1.0 0.0 ... ... ...
250 271.8 +1.0 -0.2 ... ... ...
300 323.8 +1.0 -0.3 310 +1.0 -1.0
350 375.7 +1.0 -0.3 361 +1.0 -1.2
400 426.6 +1.0 -0.3 412 +1.0 -1.4
450 477.6 +1.0 -0.4 463 +1.0 -1.6
500 529.5 +1.0 -0.4 514 +1.0 -1.8
600 632.5 +1.0 -0.5 616 +1.0 -2.0
700 ... ... ... 718 +1.0 -2.2
800 ... ... ... 820 +1.0 -2.4
900 ... ... ... 924 +1.0 -2.6
1000 ... ... ... 1026 +2.0 -2.6
1200 ... ... ... ... +2.0 ...
1400 ... ... ... 1229 +2.0 -2.6
1600 ... ... ... 1434 +2.0 -2.8
1800 ... ... ... 1638 +2.0 -2.8
2000 ... ... ... 1842 +2.0 -3.0
2200 ... ... ... 2046 +2.0 -3.0
2400 ... ... ... 2250 +2.0 -3.2
2600 ... ... ... 2453 +2.0 -3.4
2800 ... ... ... 2658 +2.0 -3.6
3000 ... ... ... 2861 +2.0 -3.8
3200 ... ... ... 3066 +2.0 -4.0
3400 ... ... ... 3270 +2.0 -4.2
3600 ... ... ... 3474 +2.0 -4.4
3800 ... ... ... 3678 +2.0 -4.6
4000 ... ... ... 3882 +2.0 -4.8
... ... ... ... 4086 +2.0 -5.0

Level A and Level B deflections, while a 6 % limiting than the adjusted level B test deflection. In such cases, the
deflection would result in a 20 % increase in Level A and Level pipes may be damaged or fail prior to determining the pipe
B deflection values. However, minimum values for Level A stiffness at 5 % deflection. Therefore, it is permitted to set the
and Level B deflections shall be equivalent to strains of 0.6 and pipe stiffness test deflection equal to the adjusted level A
1.0 % respectively (as computed by Eq X1.4 in Appendix X1). deflection, but not greater than 5 %. See Note 12 for additional
6.4.3 For high stiffness pipes, 5 % deflection will likely be information and further clarification.
above the use limit and the adjusted level A test deflection. For
very high stiffness pipes, 5% deflection may also be greater NOTE 12—Depending upon the product modulus and allowable ring

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TABLE 4 Minimum Sanitary Sewer Pipe Chemical Requirements εSCV
Pipe Stiffness, Minimum Strain
psi (kPa) 6 min 10 h 100 h 1000 h 10 000 h 50 years

9 (62) 0.97 (t/d) 0.84 (t/d) 0.78 (t/d) 0.73 (t/d) 0.68 (t/d) 0.60 (t/d)
18 (124) 0.85 (t/d) 0.72 (t/d) 0.66 (t/d) 0.61 (t/d) 0.56 (t/d) 0.49 (t/d)
36 (248) 0.71 (t/d) 0.60 (t/d) 0.55 (t/d) 0.51 (t/d) 0.47 (t/d) 0.41 (t/d)
72 (496) 0.56 (t/d) 0.48 (t/d) 0.44 (t/d) 0.41 (t/d) 0.38 (t/d) 0.34 (t/d)

Where: t and d are the nominal total wall thickness and the mean diameter (inside diameter plus t) as determined in accordance with 8.1, and
εSCV = strain corrosion value.

TABLE 5 Minimum Stiffness at 5 % Deflection 7.2 Production Tests—Select one pipe at random from each
Nominal Pipe Stiffness, psi (kPa) lot and take one specimen from the pipe barrel to determine
Diameter, Designation conformance of the material to the workmanship, dimensional,
in. A B C D and stiffness requirements of 6.1, 6.2, and 6.4, respectively.

8 36 (248) 72 (496)
7.3 Qualification Tests—Sampling for qualification tests
10 18 (124) 36 (248) 72 (496) (see 7.5) is not required unless otherwise agreed upon between
12 and 9 (62) 18 (124) 36 (248) 72 (496) the purchaser and the supplier. Qualification tests, for which a
greater
certification and test report shall be furnished when requested
by the purchaser, include the following:
7.3.1 Long-term chemical test.
TABLE 6 Ring Deflection Without Damage or Structural Failure
7.3.2 Joint-tightness test (see 6.5).
Nominal Pipe Stiffness, psi
7.3.3 Beam strength test.
9 18 36 72
7.4 Control for Chemical Test—Perform sampling and test-
Level A 18 % 15 % 12 % 9% ing for the control requirements of the chemical test at least
Level B 30 % 25 % 20 % 15 % once annually, unless otherwise agreed upon between the
purchaser and the supplier.
bending strain, this will likely begin affecting pipes with stiffness between 7.5 For individual orders, conduct only those additional
200 and 400 psi. For example, a pipe with pipe stiffness of PS360 may tests and numbers of tests specifically agreed upon between the
have a use limit of 4.3 %, an adjusted level A deflection of 4.5 % and an
purchaser and the supplier.
adjusted level B deflection of 7.5 %. Therefore, the new pipe stiffness test
deflection would be 4.5 %. Another possible product with pipe stiffness of 8. Test Methods
PS900 may have a use limit of 2.8 %, an adjusted level A deflection of
2.7 % and an adjusted level B deflection of 4.5 %. Therefore, the new pipe 8.1 Dimensions:
stiffness test deflection would be 2.7 %. 8.1.1 Diameters:
6.5 Joint Tightness: 8.1.1.1 Inside Diameter—Take inside diameter measure-
6.5.1 All joints shall meet the laboratory performance re- ments at a point approximately 6 in. (152 mm) from the end of
quirements of Specification D4161. Unrestrained joints shall the pipe section using a steel tape or an inside micrometer with
be tested with a fixed end closure condition and restrained graduations of 1⁄16 in. (1 mm) or less. Make two 90° opposing
joints shall be tested with a free end closure condition. Rigid measurements at each point of measurement and average the
joints shall be exempt from angular deflection requirements of readings.
D4161. Rigid joints typically include butt joints with laminated 8.1.1.2 Outside Diameter—Determine in accordance with
overlay, bell-and-spigot joints with laminated overlay, flanged, Test Method D3567.
bell-and-spigot adhesive bonded and threaded. 8.1.2 Length—Measure with a steel tape or gage having
6.6 Beam Strength—The pipe shall have a minimum axial graduations of 1⁄16 in. (1 mm) or less. Lay the tape or gage on
tensile elongation at failure of 0.25% and meet the following or inside the pipe and measure the overall laying length of the
requirements. For pipe sizes up to 27 in., the pipe shall pipe.
withstand, without failure, the beam loads specified in Table 7, 8.1.3 Wall Thickness—Determine in accordance with Test
when tested in accordance with 8.4. For pipe sizes larger than Method D3567.
27 in., and alternatively acceptable for smaller sizes, adequate 8.1.4 Squareness of Pipe Ends—Rotate the pipe on a man-
beam strength is demonstrated by tension and compression drel or trunnions and measure the runout of the ends with a dial
tests conducted in accordance with 8.4.1 for pipe wall speci- indicator. The total indicated reading is equal to twice the
mens oriented in the longitudinal direction, using the minimum distance from a plane perpendicular to the longitudinal axis of
tensile and compressive strengths specified in Table 7. the pipe. When the squareness of the pipe ends is rigidly fixed
by tooling, it is acceptable to verify and reinspect the tooling at
7. Sampling intervals frequent enough to assure that the squareness of the
7.1 Lot—Unless otherwise agreed upon between the pur- pipe ends is maintained within tolerance.
chaser and the supplier, one lot shall consist of 100 lengths of 8.2 Chemical Tests—Test the pipe in accordance with Test
each type, grade, and size of pipe produced. Method D3681.

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TABLE 7 Beam Strength Test Loads
Nominal Beam Load (P) Minimum Longitudinal Tensile Strength, per Unit Minimum Longitudinal Compressive Strength,
Diameter, of Circumference per Unit of Circumference
in. lbf (kN) lbf/in. (kN/m) lbf/in. (kN/m)

8 800 (3.6) 580 (102) 580 (102)


10 1200 (5.3) 580 (102) 580 (102)
12 1600 (7.1) 580 (102) 580 (102)
14 2200 (9.8) 580 (102) 580 (102)
15 2600 (11.6) 580 (102) 580 (102)
16 3000 (13.3) 580 (102) 580 (102)
18 4000 (17.8) 580 (102) 580 (102)
20 4400 (19.6) 580 (102) 580 (102)
21 5000 (22.2) 580 (102) 580 (102)
24 6400 (28.5) 580 (102) 580 (102)
27 8000 (35.6) 580 (102) 580 (102)
30 ... ... 580 (102) 580 (102)
33 ... ... 640 (111) 640 (111)
36 ... ... 700 (122) 700 (122)
39 ... ... 780 (137) 780 (137)
42 ... ... 800 (140) 800 (140)
45 ... ... 860 (150) 860 (150)
48 ... ... 920 (161) 920 (161)
51 ... ... 980 (171) 980 (171)
54 ... ... 1040 (182) 1040 (182)
60 ... ... 1140 (200) 1140 (200)
66 ... ... 1260 (220) 1260 (220)
72 ... ... 1360 (238) 1360 (238)
78 ... ... 1480 (260) 1480 (260)
84 ... ... 1600 (280) 1600 (280)
90 ... ... 1720 (301) 1720 (301)
96 ... ... 1840 (322) 1840 (322)
102 ... ... 1940 (340) 1940 (340)
108 ... ... 2060 (360) 2060 (360)
114 ... ... 2180 (382) 2180 (382)
120 ... ... 2280 (400) 2280 (400)
132 ... ... 2520 (440) 2520 (440)
144 ... ... 2740 (480) 2740 (480)
156 ... ... 2964 (519) 2964 (519)

FIG. 2 Beam Strength—Test Setup

8.2.1 Long-Term—To find if the pipe meets the require- 8.2.2 Control Requirements—Test at least six specimens in
ments of 6.3.1, determine at least 18 failure points in accor- accordance with one of the following procedures and record
dance with Test Method D3681. the results:
8.2.1.1 Alternative Qualification Procedure—Test four 8.2.2.1 Test at least three specimens at each of the strain
specimens each at the 10 and 10 000-h minimum strains given levels corresponding to the 100- and 1000-h failure times from
in Table 4 and test five specimens each at the 100 and 1000-h the product’s regression line established in 8.2.1.
minimum strains given in Table 4. Consider the product 8.2.2.2 When the alternate method of 8.2.1.1 is used to
qualified if all 18 specimens are tested without failure for at qualify the product, test at least three specimens each at the 100
least the prescribed times given in Table 4 (that is, 10, 100, and 1000-h minimum strains given in Table 4 for at least 100
1000, or 10 000 h respectively). and 1000-h respectively.

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8.2.2.3 It is acceptable to use the control test procedures of during the test. Apply the beam load for the diameter of pipe
8.2.2.2 as an alternative to the reconfirmation procedure shown in Table 7 simultaneously to the pipe (see Fig. 2).
described in Test Method D3681 for those products evaluated Maintain the loads for not less than 10 min with no evidence of
by the alternative qualification procedure of 8.2.1.1. failure. The testing apparatus shall be designed to minimize
8.3 Stiffness—Determine the pipe stiffness (F/∆y) at 5 % stress concentrations at the loading points.
deflection or the adjusted level determined in accordance with 8.4.1 As an alternative to 8.4, adequate beam strength shall
6.4.3 for the specimen, using the apparatus and procedure of be shown by determining longitudinal tensile strength in
Test Method D2412, with the following exceptions permitted: accordance with Test Method D638, except the provisions for
8.3.1 Measure the wall thickness to the nearest 0.01 in. maximum thickness shall not apply, and longitudinal compres-
(0.25 mm). sive strength in accordance with Test Method D695, on pipe
8.3.2 Load the specimen to 5 % deflection or the adjusted wall specimens oriented in the longitudinal direction.
level determined in accordance with 6.4.3 and record the load.
Then load the specimen to deflection Level A in accordance 9. Packaging, Marking, and Shipping
with Table 6 or to the adjusted level A determined in accor-
dance with 6.4.1 and 6.4.2 and examine the specimen for 9.1 Mark each length of pipe that meets or is part of a lot
visible damage evidence by surface cracks. Then load the that meets the requirements of this specification at least once in
specimen to deflection Level B in accordance with Table 6 or letters not less than 1⁄2 in. (12 mm) in height and of bold-type
to the adjusted level B determined in accordance with 6.4.1 and style in a color and type that remains legible under normal
6.4.2 and examine for evidence of structural damage as handling and installation procedures. The marking shall in-
evidenced by interlaminar separation, separation of the liner or clude the nominal pipe size, manufacturer’s name or
surface layer (if incorporated) from the structural wall, tensile trademark, this ASTM specification number D3262, type, liner,
failure of the glass-fiber reinforcement, fracture, or buckling of grade, and stiffness in accordance with the designation code in
the pipe wall. Calculate the pipe stiffness at 5 % deflection or 4.2.
at the adjusted test deflection level determined in accordance 9.2 Prepare pipe for commercial shipment in such a way as
with 6.4.3. to ensure acceptance by common or other carriers.
8.3.3 For production testing, only one specimen shall be
tested to determine the pipe stiffness. 9.3 All packing, packaging, and marking provisions of
8.3.4 The maximum specimen length needs to be 12 in. (305 Practice D3892 shall apply to this specification.
mm) or the length necessary to include stiffening ribs if they
are used, whichever is greater. 10. Keywords
8.4 Beam Strength—Place a 20-ft (6.1-m) nominal length of 10.1 fiberglass pipe; pressure pipe; RTRP; RPMP; strain
pipe on saddles at each end. Hold the ends of the pipe round corrosion

ANNEX

(Mandatory Information)

A1. CALCULATIONS OF LOWER CONFIDENCE (LCL) AND LOWER PREDICTION (LPL) LIMITS

A1.1 The following equations are used: where all symbols are as defined in Annex A1 and Annex A3
of Practice D2992 except:
h LCL 5 ~ a1bf0 ! 2 ts Π~f0 2 F!2 1
U
1
N
f 0 5 logof stress ~ strain! level of interest
NOTE A1.1—Of the expected failures at stress (strain) f0, 97.5 % will
h LPL 5 ~ a1bf0 ! 2 ts Π~f0 2 F!2 1
U
1 11
N
occur after hLPL. The average failure time at stress (strain) f0 will occur
later than hLCL 97.5 % of the time.

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D3262 − 20
APPENDIXES

(Nonmandatory Information)

X1. STRAIN CORROSION PERFORMANCE REQUIREMENTS

X1.1 From Molin and Leonhardt, the expression for bend- NOTE X1.1—Products may have use limits of other than 5 % long-term
ing strain is given as: deflection. In such cases, it is acceptable to adjust the requirements
proportionally. For example, a 4 % long-term limiting deflection would
ε b 5 D f ~ t/d !~ δv/d ! (X1.1) result in a 50 year requirement of 80 % of Table 4, while a 6 % limiting
deflection would yield a requirement of 120 % of Table 4.
With the common acceptance that these pipes must be
capable of withstanding 5 % deflection long-term, the maxi- X1.3 Alternative Strain Corrosion Test Requirements:
mum installed bending strain may be expressed as:
X1.3.1 At 0.1 h (6 min), the required strain corrosion
ε b max 5 ~ 0.05!~ D f !~ t/d ! (X1.2)
performance is based on the Level B deflections from Table 6
Using the AWWA C950 long-term bending factor of safety
of 1.50, the minimum strain corrosion performance extrapo- as follows:
lated to 50 years must be:
ε scv $ ~ 0.075!~ D f !~ t/d ! (X1.3)
ε test $ Df F t
d1δV/2 GF δV
d1δV/2 G (X1.4)

X1.2 The shape factor, Df, is dependent on both the pipe or


stiffness and the installation (backfill material, backfill density,
compaction method, haunching, trench configuration, native- ε test $ Df ~ t/d ! ~ δV/d ! S 1
11δV/2d D 2
(X1.5)
soil characteristics, and vertical loading, for example). Assum-
ing conservatively, installations achieved by tamped compac- Df for parallel plate loading is 4.28. Making the other
tion with inconsistent haunching that will limit long-term substitutions yield:
deflections to 5 %, the following values of Df have been Pipe Stiffness Minimum Test Strain
selected to be realistic, representative, and limiting. Substitut- (psi) Level B δv/d (%) at 6 Minutes

ing these values in the above equation for εscvyields the


9 30 0.97 (t/d)
minimum required strain corrosion performance at 50 years 18 25 0.85 (t/d)
given in Table 4 and below: 36 20 0.71 (t/d)
72 15 0.56 (t/d)
Pipe Stiffness, Minimum εscv
(psi) Df Performance X1.3.2 The minimum strain values at 10, 100, 1000, and
10 000 h given in Table 4 are defined by a straight line
9 8.0 0.60 (t/d)
18 6.5 0.49 (t/d) connecting the points at 6 min and 50 years on a log-log plot.
36 5.5 0.41 (t/d)
72 4.5 0.34 (t/d)

X2. INSTALLATION

X2.1 This specification is a material performance and pur- and backfill, pipe characteristics, and care in the field construc-
chase specification only and does not include requirements for tion work. The purchaser of the fiberglass pipe specified herein
engineering design, pressure surges, bedding, backfill, or the is cautioned that he must properly correlate the field require-
relationship between earth cover load and the strength of the ments with the pipe requirements and provide adequate inspec-
pipe. Experience has shown, however, that successful perfor- tion at the job site.
mance of this product depends upon the proper type of bedding

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D3262 − 20

X3. RECOMMENDED METHODS OF DETERMINING GLASS CONTENT

X3.1 Determine glass content as follows: X3.1.2 As a process control, by weight of the glass fiber
X3.1.1 By ignition loss analysis in accordance with Test reinforcement applied by machine into the pipe structure.
Method D2584 or ISO 1172.

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3299 − 18

Standard Specification for


Filament-Wound Glass-Fiber-Reinforced Thermoset Resin
Corrosion-Resistant Tanks1
This standard is issued under the fixed designation D3299; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope ization established in the Decision on Principles for the


1.1 This specification covers cylindrical tanks fabricated by Development of International Standards, Guides and Recom-
filament winding for above-ground vertical installation, to mendations issued by the World Trade Organization Technical
contain aggressive chemicals at atmospheric pressure as clas- Barriers to Trade (TBT) Committee.
sified herein, and made of a commercial-grade polyester or 2. Referenced Documents
vinylester resin. Included are requirements for materials,
properties, design, construction, dimensions, tolerances, 2.1 ASTM Standards:2
workmanship, and appearance. C581 Practice for Determining Chemical Resistance of
Thermosetting Resins Used in Glass-Fiber-Reinforced
1.2 This specification does not cover the design of vessels Structures Intended for Liquid Service
intended for pressure above atmospheric or under vacuum C582 Specification for Contact-Molded Reinforced Thermo-
conditions, except as classified herein, or vessels intended for setting Plastic (RTP) Laminates for Corrosion-Resistant
use with liquids heated above their flash points. Equipment
1.3 The values stated in inch-pound units are to be regarded D618 Practice for Conditioning Plastics for Testing
as standard. The values given in parentheses are mathematical D883 Terminology Relating to Plastics
conversions to SI units that are provided for information only D1599 Test Method for Resistance to Short-Time Hydraulic
and are not considered standard. Pressure of Plastic Pipe, Tubing, and Fittings
1.4 Special design consideration shall be given to tanks D2150 Specification for Woven Roving Glass Fabric for
subject to environmental and/or mechanical forces such as Polyester-Glass Laminates (Withdrawn 1987)3
seismic, wind, ice, agitation, or fluid dynamic forces, to D2583 Test Method for Indentation Hardness of Rigid Plas-
operational service temperatures greater than 180°F (82°C) and tics by Means of a Barcol Impressor
to tanks with unsupported bottoms. D2584 Test Method for Ignition Loss of Cured Reinforced
Resins
1.5 The following safety hazards caveat pertains only to the D2996 Specification for Filament-Wound “Fiberglass”
test method portion, Section 11, of this specification: This (Glass-Fiber-Reinforced Thermosetting-Resin) Pipe
standard does not purport to address all of the safety concerns, D2997 Specification for Centrifugally Cast “Fiberglass”
if any, associated with its use. It is the responsibility of the user (Glass-Fiber-Reinforced Thermosetting-Resin) Pipe
of this standard to establish appropriate safety, health, and D3892 Practice for Packaging/Packing of Plastics
environmental practices and determine the applicability of D4024 Specification for Machine Made “Fiberglass” (Glass-
regulatory limitations prior to use. Fiber-Reinforced Thermosetting Resin) Flanges
NOTE 1—There is no known ISO equivalent to this standard. D5421 Specification for Contact Molded “Fiberglass”
1.6 This international standard was developed in accor- (Glass-Fiber-Reinforced Thermosetting Resin) Flanges
dance with internationally recognized principles on standard- F412 Terminology Relating to Plastic Piping Systems

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Plastic Piping Systems and Chemical Equipment. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Aug. 1, 2018. Published August 2018. Originally the ASTM website.
3
approved in 1974. Last previous edition approved in 2010 as D3299 – 10. DOI: The last approved version of this historical standard is referenced on
10.1520/D3299-18. www.astm.org.

*A Summary of Changes section appears at the end of this standard


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D3299 − 18
2.2 ANSI Standards: NOTE 3—The addition of a thixotropic agent may reduce the resistance
B 16.1 Cast Iron Pipe Flanges and Flanged Fittings, Class of many resin systems to certain corrosive chemical environments. It is the
responsibility of the fabricator, using a thixotropic agent in the resin
25, 125, 250, and 8004 required for 7.1.1 and 7.1.2, to ascertain its compatibility with the
corrosive environment when this has been reported to him by the
3. Terminology purchaser.
3.1 General—Definitions are in accordance with Terminolo- 5.1.1.2 Resin pastes used to fill crevices before overlay shall
gies D883 and F412, unless otherwise indicated. not be subject to the limitations of 5.1.1.
3.2 filament-wound—as applied to tanks, a process in which 5.1.1.3 Resin may contain pigment, dyes, or colorants when
the principal circumferential load-bearing reinforcement is agreed upon between fabricator and purchaser.
applied by continuous filament winding. NOTE 4—The addition of pigment, dyes, or colorants may interfere with
3.3 contact molding—a molding process that includes “hand visual inspection of laminate quality.
lay-up,” “spray-up,” or a combination of these manufacturing 5.1.1.4 Ultraviolet absorbers may be added to the exterior
processes. surface for improved weather resistance, if agreed upon be-
tween fabricator and purchaser.
4. Classification
5.1.1.5 Antimony compounds or other fire-retardant agents
4.1 Tanks meeting this specification are classified according may be added to halogenated resins for improved fire
to type as follows, and it is the responsibility of the purchaser resistance, if agreed upon between fabricator and purchaser.
to specify the requirement for Type II tanks, the operating
pressure or vacuum levels, and the safety factor required for NOTE 5—Because the addition of fire-retardant agents may interfere
with visual inspection of laminate quality, they should not be used in the
external pressure. Absence of a designation of type required inner surface (7.1.1) or interior layer (7.1.2) unless their functional
shall imply that Type I is adequate. advantages would outweigh the loss of visual inspection.
4.1.1 Type I—Atmospheric pressure tanks vented directly to 5.2 Reinforcement:
the atmosphere, designed for pressure no greater or lower than 5.2.1 Chopped-Strand Mat—Chopped-strand mat shall be
atmospheric. constructed from chopped commercial-grade E-type glass
4.1.2 Type II—Atmospheric pressure tanks vented directly strands bonded together using a binder. The strands should be
into a fume conservation system, and designed to withstand the treated with a sizing that is chemically compatible with the
specified positive and negative pressure not to exceed 14 in. resin system used.
(355.6 mm) of water when all tie-down lugs are properly
secured, in accordance with the fabricator’s recommendations NOTE 6—The selection of the particular chopped-strand mat is depen-
for flat-bottom tanks. dent upon the performance characteristics required of the finished product
and upon the processing techniques to be used.
4.2 Tanks meeting this specification are classified according
5.2.2 Continuous Roving—Continuous roving shall be a
to grade as follows:
commercial-grade of E-type glass fiber with a sizing that is
4.2.1 Grade 1—Tanks manufactured with a single generic
chemically compatible with the resin system used.
type of thermoset resin throughout.
5.2.3 Nonwoven Biaxial or Unidirectional Fabric—These
4.2.2 Grade 2—Tanks manufactured with different generic
products shall be a commercial Grade of E-type glass fiber with
types of thermoset resin in the barrier and the structural
a sizing that is chemically compatible with the resin system
portion.
used.
NOTE 2—The external corrosive environment due to spillage or 5.2.4 Woven Roving—Woven roving shall be in accordance
corrosive vapors should be considered when specifying Grade 2 tanks (see with Specification D2150.
7.1.3.3).
5.2.5 Surface Mat—The reinforcement used for the inner
5. Materials and Manufacture surface (7.1.1) shall be either a commercial-grade chemical
resistant glass surface mat or an organic-fiber surface mat. In
5.1 Resin—The resin used shall be a commercial-grade,
environments that attack glass, the use of an organic-fiber
corrosion-resistant thermoset that has either been evaluated in
surface mat is required.
a laminate by test in accordance with 11.3 or that has been
determined by previous documented service to be acceptable
6. Design Requirements
for the service conditions. Where service conditions have not
been evaluated, a suitable resin also may be selected by 6.1 Filament-Wound Laminates—Design for Internal
agreement between fabricator and purchaser. Pressure—The maximum allowable stress of the total laminate
5.1.1 The resin shall contain no pigment, dyes, colorants, or (that is, filament winding plus the corrosion barrier, which is
filler, except as follows: made up of the inner surface (7.1.1) and interior layer (7.1.2))
5.1.1.1 A thixotropic agent that does not interfere with shall be limited by the allowable movement (strain) of the tank
visual inspection of laminate quality, or with the required wall when filled with fluid.
corrosion resistance of the laminate, may be added for viscos- 6.1.1 The allowable strain of the tank wall shall not exceed
ity control. 0.0010 in./in. (mm/mm) at 70°F (21°C).
6.1.2 Tanks shall have a longitudinal strength at least equal
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., to that of a helically wound tank having a maximum angle of
4th Floor, New York, NY 10036, http://www.ansi.org. wind of 80° (measured from the tank axis, that is, 90° is hoop

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D3299 − 18
winding). For reference, the longitudinal tensile strength of a 2.6~ E/F !~ D o /L !~ t/D o ! 2.5
Pa 5 (4)
typical 80° helical winding is approximately 2200 psi (15,168 ~ L/D o ! 2 0.45 ~ t/D o ! 0.5
kPa).
where:
6.1.3 Hoop Design:
Do = outside diameter, in. (mm),
6.1.3.1 Normal Service (Structural Corrosion Barrier)— E = lower of hoop tensile modulus or axial tensile modulus,
When the product to be stored in the tank causes little or no psi (kPa),
degradation to the selected resin, the minimum required wall F = design factor = 5,
thickness shall be in accordance with Eq 1. L = design length, in., of a vessel section, taken as the
6.1.3.2 Severe Service (Non-Structural Corrosion largest of the following: (a) the distance between
Barrier)—When the product to be stored in the tank may cause head-tangent lines plus one-third the depth of each
degradation of the resin over time and with the agreement of formed head if there are no stiffening rings (excluding
the purchaser, the minimum required wall thickness of the tank conical heads and sections); (b) the distance between
shall be determined in accordance with Eq 2. cone-to-cylinder junctions for vessels with a cone or
0.036*γ*H*D conical heads if there are no stiffening rings; (c) the
tT 5 (1) greatest center-to-center distance between any two
2*E T *Z
adjacent stiffening rings; (d) the distance from the
or center of the first stiffening ring to the formed head
tangent line plus one-third the depth of the formed head
S tT 5
0.2489*γ*H*D
2*E T *Z D (excluding conical heads and sections), all measured
parallel to the axis of the vessel; (e) the distance from
0.036*γ*H*D the first stiffening ring in the cylinder to the cone-to-
t T 5 t CB1 (2)
2*E FW*Z cylinder junction,
Pa = allowable external pressure, psi (kPa), and
or t = wall thickness, in. (mm) (nominal).

S t T 5 t CB1
0.2489*γ*H*D
2*E FW*Z D 6.2.2 Torispherical Heads—For torispherical heads, com-
pute the allowable external pressure Pa as follows:
where: P a 5 0.36~ E/F !~ t/R o ! 2 (5)
tT = total thickness, in. (mm), where:
tCB = thickness of the corrosion barrier, in. (mm), Ro = outside crown radius of head, in. (mm).
H = fluid head, in. (mm),
γ = specific gravity of fluid, 6.2.2.1 For torispherical heads subject to internal loading,
D = inside diameter of tank, in. (mm). the knucle radius shall be externally reinforced in accordance
ET = hoop tensile modulus of the total laminate (see with Fig. 1. The reinforcement thickness shall be equal to the
Appendix X3), psi (kPa), thickness of the head as calculated above. The thickness of a
EFW = hoop tensile modulus of the filament winding only psi joint overlay near the knucle radius tangent line of a dished
(kPa), and head contributes to the knucle reinforcement.
Z = allowable strain in accordance with 6.1.2.
6.1.3.3 The minimum total thickness of the tank shall be
0.1875 in. (4.76 mm).
NOTE 7—The use of an accepted analytical technique, such as laminated
plate theory (LPT), for design and analysis of composite vessels may
predict stresses, strains, and strength on a ply-by-ply basis, given some
basic lamina properties.
NOTE 8—Tanks for installation outdoors shall be designed for the effect
of wind loading and other environmental factors in accordance with sound
design practice, including tank buckling analysis.
NOTE 9—Tanks with significant physical loadings other than fluid head
(such as side-mounted equipment, violent agitation, unusually high flow
rates, and unsupported bottoms) shall be given special design consider-
ation.
6.2 Design for External Pressure:
6.2.1 Cylindrical Shells—For cylindrical shell, compute the
value 1.73 (Do/t)0.5. If the result is less than L/Do of the
cylinder, compute Pa as follows:
P a 5 2.6~ E/F !~ D o /L !~ t/D o ! 2.5 (3)

If the result is greater than L/Do of the cylinder, compute Pa FIG. 1 Jointed Head Detail
as follows: Sketch A

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6.2.3 Stiffening Rings—The required moment of inertia, Is, mm) for over 6 to 12 ft (1.8 to 3.7 m) diameter, and 3⁄8 in. (9.5
of a circumferential stiffening ring for cylindrical shells under mm) for over 12 ft (3.7 m) diameter.
external pressure or internal vacuum shall not be less than that 6.3.2.1 Deflection of the flat bottom when the tank is empty,
determined by the following formula: commonly known as “oil canning,” is permissible as long as
I s 5 PLs D o 3 F/24E h (6) the requirements of 6.3.2.4 are met.
6.3.2.2 Bottom heads may be molded integrally with the
where:
straight shell or may be molded separately with a straight
Do = shell outside diameter, in. (mm), flange length for subsequent joining to shell.
Eh = hoop tensile modulus, psi (kPa),
F = design factor = 5, 6.3.2.3 The radius of the bottom knuckle of a flat-bottom
Is = moment of inertia, in.4 (mm4), of stiffener and effective tank shall be not less than 1 in. (25 mm) on tanks 4 ft (1.22 m)
length of shell, or smaller in diameter and 1.5 in. (38 mm) on tanks larger than
Ls = one-half of the distance from the centerline of the 4 ft (1.22 m) diameter. The minimum thickness of the radiused
stiffening ring to the next line of support on one side, section shall be equal to the combined thickness of the shell
plus one-half of the centerline distance to the next line wall and the bottom. The reinforcement of the knuckle-radius
of support on the other side of the stiffening ring, both area shall taper so that it is tangent to the flat bottom, and shall
measured parallel to the axis of the cylinder, in. A line not extend beyond the tangent line onto the tank bottom, unless
of support is the following: (a) a stiffening ring that methods of manufacture are used that maintain flat-bottom
meets the requirements of this paragraph; (b) a circum- configuration, and shall extend up the vertical tank wall a
ferential line on a head at one-third the depth of the minimum of 8 in. (200 mm) on tanks up to 4 ft (1.22 m) in
head from the head tangent line; (c) a cone-to-cylinder diameter, and 12 in. (304 mm) on tanks over 4 ft (1.22 m) in
junction, and diameter. The reinforcement shall then taper into the side wall
P = actual external pressure, psi (kPa). over an additional length of 4 in. (102 mm) (see Fig. 3).
Methods of manufacture that incorporate stiffening bands as a
Typical half-round stiffener sizes and dimensions for differ-
means of knuckle stabilization, are permissible alternatives by
ent values of Is are shown in Fig. 2. Other stiffener profiles
agreement between purchaser and fabricator, provided the
meeting the required moment of inertia may be used.
fabricator can document the validity of the design.
6.3 Contact Molded Laminates—Portions of the tank, such 6.3.2.4 The tank bottom shall not have variations from a
as joints, heads, nozzles, and supports, may be fabricated by nominally flat plane that would prevent uniform contact of the
contact molding. Contact-molded laminates shall satisfy the entire bottom surface with a properly prepared flat support
minimum property requirements listed in Specification C582, surface when the tank is filled with liquid. The bottom laminate
as shown in Table 1. surface shall be a hand-work finish, and shall have no exces-
6.3.1 Top Head—The top head, regardless of shape, shall be sive laminate projections that would prevent uniform contact
able to support a single 250-lbf (113.4 kg) load on a 4 by 4-in. with a properly prepared flat support surface when the tank is
(100 by 100-mm) area without damage and with a maximum filled with liquid.
deflection of 1⁄2 % of the tank diameter at the area the load is
applied. NOTE 11—This requirement is not intended to exclude the use of drain
6.3.1.1 The minimum thickness shall be 0.1876 in. (4.76 nozzles which are commonly used at the bottom of the side shell. They do,
however, require foundation cut-outs of the appropriate dimensions for the
mm). nozzle type and size.
NOTE 10—Support of auxiliary equipment, snow load, or operation
personnel may require additional reinforcement or the use of stiffener ribs,
6.3.2.5 The thickness of an elevated torispherical dished
sandwich construction, or other stiffening systems. Type II tanks may also bottom, suitable for supporting the weight of the fluid head,
require additional reinforcement. shall be determined by the following equation, but shall not be
6.3.2 Bottom Head—The minimum thickness for a fully less than 3⁄16 in. (4.8 mm):
supported flat-bottom head for Type I tanks shall be as follows:
3⁄16 in. (4.8 mm) for 2 to 6 ft (0.6 to 1.8 m) diameter, 1⁄4 in. (6.4 t5
0.885 PR 0.885 ~ 0.036γHR!
S
5
S
or S
0.885 ~ 0.2489γHR!
S D (7)

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FIG. 2 Penetrating Nozzle Installation

TABLE 1 Minimum Contact-Molded Laminate Physical PropertiesA


NOTE 1— Based on use of woven roving in thickness 1⁄4 in. (6mm) and above.
Property Thickness, in. (mm)
⁄ to 3⁄16 (3.2 to 4.8)
18 ⁄ (6.4)
14 ⁄
5 16 (7.9) ⁄ & up (9.5 and up)
38

Ultimate tensile strength, min, psi (MPa) 9 000 (62.05) 12 000 (82.74) 13 000 (89.63) 15 000 (103.4)
Tensile modulus, psi (MPa) 1 000 000 (6895) 1 300 000 (8963) 1 400 000 (9653) 1 500 000 (10342)
Flexural strength, min, psi (MPa) 16 000 (110.3) 19 000 (131.0) 20 000 (137.9) 22 000 (151.7)
Flexural modulus of elasticity (tangent), min, psi 700 000 (4826) 800 000 (5516) 900 000 (6205) 1 000 000 (6894)
(MPa)
A
Laminates that do not meet the minimum values of Table 1 are considered acceptable, provided they are made to afford the same overall strength that would be obtained
with a laminate meeting the specified thickness.

where: PD
t5 (8)
t = thickness, in. (mm), 2S
S = allowable tensile strength (not to exceed 1⁄10 of ultimate
For Cone Bottom:
strength), psi (kPa) (see 11.6.1),
γ = specific gravity of fluid, PD
t5 (9)
P = pressure, psi (kPa), 2S· cos ~ α !
R = inside radius of dished head, in. (mm), and
H = distance from the top of the fluid to the deepest portion where:
of the bottom, in. (mm). α = 1⁄2 the included (apex) angle of the cone at the centerline
of the head. ( Not greater than 30°)
For Elliptical Bottom Head:

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FIG. 3 Flat-Bottom Tank Corner Detail

NOTE 12—An alternative method for design of an elevated torispherical 6.3.3 Open-Top Tanks—The top edge of open-top tanks
dished bottom is shown in Appendix X2. shall have a horizontal reinforcing flange or other means of
6.3.2.6 The torispherical dished-bottom head shall have a reinforcement sufficiently rigid to maintain the shape of the
radius of curvature that is equal to or less than the inside tank after installation, such as stiffener ribs. The flange shall be
diameter of the tank straight shell, and a minimum knuckle in accordance with Table 2.
radius of at least 6 % of the diameter of the head. 6.3.4 Joints:

TABLE 2 Reinforcing Flange for Open-Top TanksA,B


Tank Diameter, ft (m) Flange Dimensions
Flange
L,C ft (m) 2 4 6 8 9 10 11 12 Width ThicknessD
Type
(0.610) (1.219) (1.629) (2.438) (2.743) (3.048) (3.353) (3.658) in. (mm) in. (mm)
2 (0.610) A A A C D E F G A 2 (51) 14⁄ (5)
4 (1.212) A A A C D E F G B 2 (51) 3 ⁄8 (10)
6 (1.829) A A A C D E F G C 2 (51) 1 ⁄2 (13)
8 (2.438) A A A C D E F G D 21⁄2 (64) 3 ⁄8 (10)
10 (3.048) A A B C D E F G E 21⁄2 (64) 1 ⁄2 (13)
12 (3.658) A A B D D E F G F 3 (76) 3 ⁄8 (10)
14 (4.267) A A B D E F F G G 3 (76) 1 ⁄2 (13)
16 (4.877) A A C E E G G H H 3 (76) 5 ⁄8 (16)
18 (5.486) A A C E F G G H J 3 (76) 3 ⁄4 (19)
20 (6.096) A A D E F G H J K 3 (76) 1 (25)
24 (7.315) A B D F G H J K
30 (9.144) A B E G H H K K
36 (10.973) A B E H J K K
40 (12.192) A B E H J K
A
This table is based on handling considerations only. Significant superimposed loads, such as from wind or seismic conditions, should be considered independently.
B
Reinforcement configurations other than a flange may be used if equal or greater stiffness is provided.
C
L = maximum distance from flange to the tank bottom or to the uppermost shell stiffener when used.
D
Flange thickness shall be at least equal to local vessel thickness.

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6.3.4.1 The cured resin surfaces to be overlaid shall be overlay width shall be 4 in. (100 mm). This internal overlay
roughened using 36 or coarser grit abrasive media and shall shall not be considered a structural element in determining
extend beyond the lay-up area so that no reinforcement is joint thickness.
applied to an unroughened surface. Surfaces shall be clean and 6.3.4.5 The thickness of a joint near the bottom tangent line
dry before lay-up. The entire roughened area shall be coated shall not be considered to contribute to the knuckle reinforce-
with paraffinated resin after the joint lay-up is made. ment of 6.3.2.3, but shall be additive thereto.
6.3.4.2 Joints between tank-wall sections shall be over- 6.3.5 Fittings:
wound to a thickness as calculated in 6.1.3.2, or they may be
overlaid by a contact-molded laminate. When contact-molded 6.3.5.1 The more common method of fabricating nozzles is
laminate joints are used to join hoop segments of the straight by contact molding both the nozzle neck and flange to the
shell, or to join the bottom or top head to the shell, the dimensions shown in Specification D5421 and Table 4. The
thickness of the structural joint overlay shall be determined by corrosion-resistant barrier of the nozzle shall be at least
the following equation, but shall not be less than 3⁄16 in. (4.8 equivalent to the inner surface and interior layer (7.1.1 and
mm): 7.1.2) and shall be fabricated from the same resin as the tank
head or shell to which it is attached.
t5
PD
2S h
5
0.036γHD
2S h
or S
0.2489γHD
2S h D (10) 6.3.5.2 Acceptable alternative methods to be agreed upon
between fabricator and purchaser are the use of contact-molded
where: pipe, filament-wound pipe, in accordance with Specification
t = wall thickness, in. (mm), D2996, or centrifugally cast pipe, in accordance with Specifi-
Sh = allowable hoop tensile strength (not to exceed 1⁄10 of the cation D2997, joined to a suitable contact-molded (Specifica-
ultimate hoop strength), psi (kPa), tion D5421), or filament-wound flange (Specification D4024).
P = pressure, psi (kPa), The corrosion-resistant barrier of the contact-molded portions
H = fluid head, in. (mm), of such nozzles shall be equivalent to the inner surface and
γ = specific gravity of fluid, and interior layer (7.1.1 and 7.1.2) and shall be fabricated from the
D = inside diameter of tank, in. (mm). same resin as the tank head or shell to which they are attached.
6.3.4.3 The minimum width of the structural joint overlay 6.3.5.3 Nozzles 4 in. (100 mm) and smaller shall be
for bottom-supported tanks is shown in Table 3. supported by a suitable gusseting technique, using plate gussets
6.3.4.4 The corrosion-resistant barrier component of the or conical gussets, as shown in Fig. 4 and Fig. 5. Plate gussets,
joint shall be formed in the same manner as the inner surface where needed, shall be evenly spaced around the nozzle and
and the interior layer (7.1.1 and 7.1.2) and the minimum are to be added after complete assembly by the nozzle on the

TABLE 3 Minimum Widths of Joint Overlay for Circumferential Joints

H × DA = 60 100 140 180 220 260 300 340 380 420 460 500
minimum
width of
outsideB
in. 4 4 5 6 7 8 9 10 11 12 13 14
(mm) (102) (102) (127) (152) (178) (203) (229) (254) (279) (305) (330) (356)
A
where: H = distance from the top of the liquid level to the joint, ft (m) and
D = inside diameter of the tank, ft (m).
B
Axial joint overlay widths shall be twice the width shown in table.

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TABLE 4 Dimensions for Contact-Molded Flanged Nozzles (25 psi Rating)

Nozzle Inside Minimum Wall Minimum Flange Minimum Hub Minimum Hub Length
Diameter (D), in. (mm) Thickness (tn), Thickness (tf), in. Thickness (th), (h), in. (mm)
in. (mm) (mm) in. (mm)
1 (25) ⁄ (5)
3 16 ⁄ (13)
12 14⁄ (6) 2 (51)
11⁄2 (38) ⁄ (5)
3 16 ⁄ (13)
12 14⁄ (6) 2 (51)
2 (51) 3⁄16 (5) 1⁄2 (13) 1⁄4 (6) 2 (51)
3 (76) 3⁄16 (5) 1⁄2 (13) 1⁄4 (6) 2 (51)
4 (102) 3⁄16 (5) 1⁄2 (13) 1⁄4 (6) 2 (51)
6 (152) 3⁄16 (5) 1⁄2 (13) 1⁄4 (6) 2 (51)
8 (203) 3⁄16 (5) 9⁄16 (14) 5⁄16 (8) 21⁄2 (57)
10 (254) 3⁄16 (5) 11⁄16 (17) 3⁄8 (10) 23⁄4 (70)
12 (305) 3⁄16 (5) 3⁄4 (19) 3⁄8 (10) 3 (76)
14 (356) 1⁄4 (6) 13⁄16 (21) 7⁄16 (11) 31⁄4 (83)
16 (406) 1⁄4 (6) 7⁄8 (22) 7⁄16 (11) 31⁄2 (89)
18 (457) 1⁄4 (6) 15⁄16 (24) 1⁄2 (13) 33⁄4 (95)
20 (508) 1⁄4 (6) 1 (25) 1⁄2 (13) 4 (102)
24 (610) 1⁄4 (6) 11⁄8 (29) 9⁄16 (14) 41⁄2 (114)

FIG. 4 Plate-Type Gussets

shell. Larger nozzles, subject to superimposed mechanical


forces, require special consideration.

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NOTE 1—This design does not require lay-up of nozzle neck to exterior of tank wall. Nozzle may be penetrating type or flush type as illustrated.
FIG. 5 Conical Type Gussets

6.3.5.4 Manways installed in top heads may be of the NOTE 13—Tanks over 6 ft (1.8 m) straight-shell height may need both
flanged or nonflanged design, as agreed upon between the top- and side-shell opening manways for safety and maintenance consid-
erations.
fabricator and purchaser.
6.3.5.5 Side-shell manways shall be installed in accordance 6.4 Vents:
with 7.3.2, 7.3.3, and Fig. 6. 6.4.1 Vents that discharge freely into the atmosphere must
6.3.5.6 Typical manway dimensions are shown in Table 5. be provided in all Type I closed-top tanks. Minimum vent size

NOTE 1—This installation method is used only when the nozzle is being installed with an integral conical gusset which would prevent application of
an exterior laminate.
FIG. 6 Nozzle Installation and Cutout Reinforcement Location Alternative

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TABLE 5 Typical Dimensions of Manways
NOTE 1—Bolt size equals bolt hole diameter minus 1⁄8 in. (3 mm).
NOTE 2—Gaskets shall be 1⁄8 in. thick full-face elastomeric material having a hardness of Shore A80 ± 5.
Minimum Minimum Diameter of Minimum Thickness of Minimum Manway Diameter of Bolt Number of Bolt Hole Diameter, in.
Size, in. Flange and Cover, in. Flange and Cover, in. Wall Thickness, in. Circle, in. (mm)ABC Bolts (mm)
(mm) (mm) (mm) (mm)
Pressurized Manway—up to 15 psig
20 (508) 271⁄2 (699) 1 (25.4) 3⁄8 (9.5) 25 (635) 20 ⁄ (19)
34

22 (559) 30 (762) 1 (25.4) 3⁄8 (9.5) 27 (686) 20 ⁄ (19)


34

24 (610) 32 (813) 1 ⁄4 (31.8)


1 3⁄8 (9.5) 291⁄2 (749) 20 ⁄ (19)
34

Manway—Atmospheric Pressure up to 0.5 psig


20 (508) 271⁄2 (699) 3⁄8 (9.5) 1⁄4 (6.4) 25 (635) 20 ⁄ (12.7)
12

22 (559) 30 (762) 3⁄8 (9.5) 1⁄4 (6.4) 27 (686) 20 ⁄ (12.7)


12

24 (610) 32 (813) 3⁄8 (9.5) 1⁄4 (6.4) 291⁄2 (748) 20 1⁄2 (12.7)

A
±0.06 in. (1.5 mm) (ASME/ANSI B 16.5).
B
±0.03 in. (0.76 mm) center to center of adjacent bolt holes (ASME/ANSI B 16.5).
C
±0.06 in. (1.5 mm) eccentricity between bolt circle and center of nozzle.

shall be sufficient to handle the flow displacement of all resistant glass fiber surface mat or with an organic fiber surface
combined inlet or outlet nozzles without creating any pressure mat, in accordance with 5.2.5.
above atmospheric, or any vacuum condition.
NOTE 15—This resin-rich inner surface will usually contain less than
NOTE 14—Special vent sizing consideration should be given to the 20 % by weight of reinforcing material.
numerous operating situations that could otherwise cause a positive or a 7.1.2 Interior Layer—The inner surface layer exposed to the
negative pressure in a closed tank. Since overfilling a closed tank with the
vent on the top can cause the tank to be over-pressured, a suitably sized corrosive environment shall be followed with a layer composed
overflow, properly located, or other appropriate protection, may be of resin, reinforced only with noncontinuous glass-fiber strands
required to prevent over-pressuring the tank. applied in a minimum of two plies of chopped-strand mat
6.4.2 Type II tanks shall be designed to withstand the equivalent to a total of 3 oz/ft2 (0.92 kg/m2 ). As an alternative,
specified positive or negative pressures not to exceed 14 in. a minimum of two passes of chopped roving of minimum
(355.6 mm) of water. Special design consideration must be length 0.5 in. (13 mm) to a maximum length of 2.0 in. (50.8
given to buckling of tank wall and heads, the hold-down lug mm), shall be applied uniformly to an equivalent weight of 3
system, and top and bottom knuckle requirements. Fluid level oz/ft2 (0.92 kg/m2). Each ply of mat or pass of chopped roving
in the tank is an important consideration in the analysis. shall be well-rolled prior to the application of additional
6.4.2.1 Flat-bottom Type II tanks must have all hold-down reinforcement. The combined thickness of the inner surface
lugs properly secured to the foundation, in accordance with the and interior layer shall not be less than 0.10 in. (2.5 mm).
tank fabricator’s recommendation for the design of the lugs 7.1.2.1 Glass content of the inner liner and the interior layer
used and for the tank installation and operation. combined shall be 27 6 5 % by weight when tested in
accordance with 11.4.
6.5 Hold-Down Lugs—Hold-down lugs shall be a require-
7.1.2.2 The degree of cure of the laminate shall be such as
ment on all tanks for outdoor service, on all Type II tanks, and
to exhibit a Barcol hardness on the inner surface of at least
on tanks subject to seismic loads or vibrations. The design
90 % of the resin manufacturer’s minimum specified hardness
number and attachment of such lugs is the responsibility of the
for the cured resin, when tested in accordance with 11.5 and
fabricator, based on the wind, seismic, and other loads speci-
Note 18, Note 19, and Note 20.
fied by the purchaser.
7.1.3 Structural Layer:
6.5.1 Hold-down lugs shall be placed on the tank in such a
7.1.3.1 Filament-Wound Structural Layer—Subsequent re-
way that they do not protrude below the bottom surface of the
inforcement shall be continuous-strand roving in accordance
tank.
with 5.2.2, that is needed to satisfy the requirements of 6.1.3.2.
6.6 Lifting Lugs—Lifting lugs or other provisions for lifting The thickness of the filament-wound portion of the tank shell
tanks (see Appendix X1) shall be provided for tanks over 500 may be varied with tank height (tapered-wall construction),
lb (227 kg) in weight. provided these requirements are met at any height level. If
additional longitudinal strength is required, the use of other
7. Laminate Construction Requirements reinforcements, such as woven fabric, nonwoven unidirectional
7.1 Structural Tank—The laminate comprising the structural or bidirectional fabric, chopped-strand mat, or chopped
tank (bottom, cylindrical shell, top head) shall consist of a strands, may be interspersed in the winding to provide addi-
corrosion-resistant barrier (also known as “liner”) comprised of tional strength. Glass content of this filament-wound structural
an inner surface and interior layer, and a structural layer. layer shall be 50 to 80 % by weight. Only those constructions
7.1.1 Inner Surface—The inner surface exposed to the evaluated for design properties in 11.6 shall be used.
chemical environment shall be a resin-rich layer 0.010 to 0.020 7.1.3.2 Contact-Molded Structural Layer in Top and Bottom
in. (0.25 to 0.5 mm) thick, reinforced with a suitable chemical- Heads—Subsequent reinforcement shall be comprised of 1.5

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D3299 − 18
oz/ft2 (0.46 kg/m2) chopped-strand mat or equivalent weight 7.2.5 The outer structural overlay of a joint shall be centered
of chopped roving, or shall be comprised of chopped-strand on the joint, fabricated in accordance with 6.3.4.2, and shall be
mat or chopped roving and such additional number of alter- finished in accordance with 7.1.3.5.
nating plies of 24 oz/yd2 (0.81 kg/m2) woven roving 18 7.3 Fittings and Accessories:
oz/yd2 (0.61 kg/m2) nonwoven biaxial fabric to a thickness as
7.3.1 The surfaces of fittings, tank accessories, and the
required to meet the physical properties that are used for the
laminates required for their installation that are exposed to the
design. The use of woven roving is optional. The designations corrosive media, shall be constructed in accordance with 7.1.1
of these specific weights of glass reinforcement are for and 7.1.2, except for those fitting surfaces which are made by
reference only and may be comprised of other weight combi- manufacturing processes other than contact molding (see
nations of reinforcement materials, when agreed to between the 6.3.5.2).
fabricator and purchaser. Each successive ply or pass of
7.3.1.1 The cut edges of all laminates exposed to the
reinforcement shall be well-rolled prior to the application of
chemical environment shall be sealed with a laminate conform-
additional reinforcement. Where woven roving is used,
ing to 7.1.1 and 7.1.2. Where shape, thickness, or other
chopped-strand glass reinforcement shall be used as alternating
restrictions preclude covering the edges with the preceding
and final layers. All woven roving, nonwoven fabric, and
laminate, such cut edges and any machined flange faces shall
surfacing mat shall be overlapped. Laps in subsequent layers
be at least coated with resin. In either case, the resin used shall
shall be staggered at least 2.25 in. (60 mm) from laps in the
be that used in the equipment laminate and finished in
preceding layer.
accordance with 7.1.3.5.
7.1.3.3 When the outer surface of this structural layer is to 7.3.2 Nozzle and Manway Installation—Flanged nozzles
be subject to spillage or a corrosive environment, a resin-rich may be installed with the pipe stub flush with the inside of the
layer, in accordance with 7.1.1, shall be applied over the final tank shell (flush type, Fig. 4) or projecting inside the tank
layer of reinforcement. (penetrating type, Fig. 5).
7.1.3.4 Tanks used for outdoor service or subject to ultra- 7.3.2.1 Nozzle Projection—The installed nozzle shall main-
violet exposure shall incorporate provisions to minimize ultra- tain a minimum clearance of 3 in. (76 mm) between the back
violet degradation. Suitable methods include use of ultraviolet face of the flange and the exterior of the cutout opening
absorbers, incorporation of pigment of sufficient opacity in the reinforcement. In addition, this clearance shall not be less than
outer surface resin-rich layer, or use of resins inherently the shear distance required for proper installation of the nozzle
resistant to ultraviolet degradation. Since pigmentation makes (see 7.3.3).
inspection difficult, it shall be added after inspection or 7.3.2.2 Cutout Reinforcement Laminate—When a vessel
otherwise by agreement between the purchaser and fabricator. shell or head is cut in an area bearing hydrostatic pressure, P,
7.1.3.5 Where air-inhibited resin is exposed to air, full the cutout shall be reinforced on a circular area concentric with
surface cure of the inner surface shall be obtained by coating the cutout, as shown in Fig. 4 and Fig. 5. Acceptable patterns
such surface with a coat of resin containing 0.2 to 0.6 % of reinforcement placement are shown in Fig. 2.
paraffin wax, having a melting point between 122 and 126°F 7.3.2.3 Cutout Reinforcement Diameter—The outer diam-
(50 and 52°C). Other techniques such as sprayed, wrapped, or eter of the cutout reinforcing laminate, dr, shall not be less than
overlaid films are also acceptable methods to attain surface two times the nominal nozzle diameter. For nozzles less than 6
cure. in. (152 mm) in diameter, the minimum cutout reinforcement
7.2 Joints: diameter, dr, shall be the nominal nozzle size plus 6 in. (152
mm).
7.2.1 The width of the first layer of joint overlay shall be 3
in. (76 mm) minimum. Successive layers shall uniformly 7.3.2.4 Cutout Reinforcement Thickness—The thickness, tr,
increase in width in that specified in Table 3 to form a smooth of the cutout reinforcement laminate for nozzles installed in
contour laminate that is centered on the joint. cylindrical shells or dished heads shall be determined as
follows:
7.2.2 A highly filled resin paste shall be placed in the
crevices between joined pieces, leaving a smooth surface for t r 5 PDK/2S r (11)
lay-up. where:
7.2.3 The cured resin surfaces of parts to be joined shall be K = 1.0 for nozzles 6 in. (152 mm) diameter and larger,
roughened using 36 or coarser abrasive grit media to expose K = d/(dr − d) for nozzles less than 6 in. (152 mm) diameter,
glass fibers. This roughened area shall extend beyond the P = hydrostatic pressure at the point of nozzle installation,
lay-up areas so that no reinforcement is applied to an unpre- psi (kPa),
pared surface. The entire roughened area shall be coated with D = inside diameter of tank, in. (mm),
paraffinated resin after joint overlay is made. Sr = allowable tensile stress (not to exceed 1⁄10 of the
7.2.4 The interior overlay of a joint shall consist of a ultimate strength of the cutout reinforcing laminate);
minimum of two plies of 1.5 oz/ft2 (0.46 kg/m2) chopped- see Table 1,
strand mat reinforcement, followed by a resin-rich layer d = nominal nozzle diameter, in. (mm), and
reinforced with surfacing mat. This overlay shall be the d r = cutout reinforcement diameter, in. (mm).
equivalent of 7.1.1 and 7.1.2 combined, and shall be centered This thickness, tr, may be applied to the outer or inner
on the joint. It shall be finished in accordance with 7.1.3.5. surfaces, or be divided between them as shown in Fig. 6.

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NOTE 16—When tr is calculated to be 1⁄8 in. (3.2 mm) or less, it can be preceded and followed by a layer of 11⁄2 –oz (0.458 kg/m2) mat
disregarded, as the strength requirements will be met by t0 (see Figs. 2 and and then covered with a laminate equivalent to 7.1.1 and 7.1.2.
7).
When the inside laminate consists only of a corrosion barrier,
7.3.2.5 When reinforcing materials are cut to facilitate the length of the laminate, hr shall be a minimum of 3 in. and
placement around an installed nozzle, joints in successive hi shall be the lesser of 3 in. (76mm) or the nominal radius of
reinforcing layers should be staggered to avoid overlapping the nozzle.
and (on cylindrical shell installations) shall not be placed so 7.3.3.3 Installation Laminate Lengths—The length of the
they parallel the axis of the tank. The intent of these require- outside laminate, ho, and the inside laminate, hi, shall each be
ments is to avoid orienting joints in reinforcing layers perpen- equal to the shear length, hs, given in Table 6 based on the
dicular to the maximum load-bearing direction (circumferen- thickness of the individual laminates.
tial).
7.3.3 Nozzle Installation Laminates—Nozzle installation 7.3.3.4 In nozzle installations where the installation overlay
laminate dimensions are shown in Fig. 2 and Fig. 7. Installation is installed before the cutout reinforcement has fully cured, that
laminate placements are shown in Fig. 6. The all-interior portion of the overlay which extends onto the tank shell may be
installation laminate placement is used only when the nozzle considered to become a part of the cutout reinforcement
being installed has an integral conical gusset preventing laminate if the installation laminate length is extended to the
application of an exterior laminate. required cutout reinforcement diameter, dr.
7.3.3.1 Installation Laminate Thickness—The inside and 7.3.3.5 Monolithic Installation—The total bond thickness,
outside installation thicknesses (ti and to) combined shall be at tm, shall be the greater of either the cutout reinforcement
least as thick as the nozzle neck. thickness, tr, or the outside bond thickness, to.
7.3.3.2 Inside Installation Laminate Construction—The in- 7.3.4 Gussets—If gussets (either plate or conical) are used to
side installation laminate shall be constructed using only stiffen the installed nozzle, gusset installation laminates are in
noncontinuous glass reinforcements, except that when woven addition to the requirements of 7.3.3. Typical plate type and
roving is included to strengthen the laminate, it shall be conical type gussets are shown in Fig. 6 and Fig. 7. Other

FIG. 7 Flush Nozzle Installation

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TABLE 6 Shear Bond Length (see Figs. 2 and 7)
NOTE 1—When internal overlay serves only as a corrosion barrier, the total shear length must be placed on the exterior overlay.
Inch-Pound Units
Overlay thickness, in. ⁄
14 ⁄
5 16 ⁄
38 ⁄
7 16 1 ⁄2 9⁄16 ⁄
58 ⁄
11 16 ⁄
34 ⁄
78 1
hA (shear length), in. 3 3 3 31⁄2 4 41⁄2 5 5 1 ⁄2 6 7 8
SI Units
Overall thickness, mm 6.4 8 9.5 11 13 14 16 17.5 19 22 25.4
h (shear length), mm 76 76 76 90 100 114 127 140 152 178 203
A
h = total shear length (ho+ hi) (Fig. 4).

gusseted nozzle installations may be used as agreed upon 8.5 The standard orientation of flanges shall provide bolt
between fabricator and purchaser. holes straddling the normal centerlines of the tank. Bolt holes
7.3.5 Location of Cutouts on the Shell—For cutouts made of flanges located on the tank top or bottom, shall straddle the
within 6 in. (152 mm) of the knuckle radius area of a head or principal centerline of the vessel or lines parallel to it as shown
within 6 in. (152 mm) of a shell-to-shell or shell-to-head joint, in Fig. 8.
additional hole-cutout reinforcement is required, unless the 8.6 An alternative method of orientation of flanges on the
area of installation is at a point within the vessel that is not tank top or bottom, with the bolt holes straddling the radial
exposed to hydrostatic pressure. centerlines, shall be by agreement between the purchaser and
7.3.6 All nozzles and manways shall be installed in accor- fabricator.
dance with Fig. 2 and Fig. 7. The interior overlay shall present
the same corrosion resistance to the fluid as specified in 7.1.1 8.7 The location of nozzles shall be held to the tolerance
and 7.1.2. shown in Fig. 8.

9. Workmanship, Finish, and Appearance


8. Dimensions and Tolerances
9.1 The minimum acceptable level for workmanship and
8.1 Standard tank diameters, based on internal measure-
finish of the finished laminate shall conform to the require-
ments with the tank in the vertical position, are listed in Table
ments specified in Section 9 of Specification C582.
7. Tolerance on the inside diameter, including out-of-
roundness, shall be 61 %. NOTE 17—A representative laminate sample may be used for determi-
nation of an acceptable surface finish and acceptable level of visual
8.2 Where employed, shell taper shall be additive to the imperfections.
figure used for the tank diameter, unless otherwise specified by
the manufacturer and accepted by the purchaser. The shell taper 10. Requirements
shall not exceed 1⁄2 ° per side. 10.1 Degree of Cure—Degree of cure of the laminate shall
8.3 Tolerance on overall tank height shall be 1⁄2 %, but shall be found by determining the Barcol hardness as indicated in
not exceed 61⁄2 in. (12.7 mm). 11.5.
8.4 Nozzle flange faces shall be perpendicular to the axis of NOTE 18—A useful technique to check the cure of a non-molded surface
the pipe within tolerances shown in Fig. 8, and shall be flat of a polyester resin is as follows: Rub a few drops of acetone on the
within 61⁄32 in. (0.8 mm) through 18 in. (457 mm) nozzle size laminate surface until it evaporates. If the surface becomes softened or
tacky, it is and indication of under cure.
and 61⁄16 in. (1.6 mm) for large nozzle sizes. Tolerances on NOTE 19—The use of organic reinforcing materials may reduce the
installation are shown in Fig. 8. Barcol hardness readings without necessarily indicating undercure.
NOTE 20—Barcol hardness values may vary when tests are conducted at
temperatures that differ from those shown in 11.2.

TABLE 7 Standard Tank Inside Diameter 11. Test Methods


in. mm 11.1 Conditioning—Condition the specimens prior to test at
24 (610) 70 to 77°F (23 6 2°C) for not less than 40 h in accordance with
30 (762)
36 (914)
Procedure A of Methods D618, for those tests when condition-
42 (1067) ing is required, and in all cases of disagreement.
48 (1219)
54 (1372) 11.2 Test Conditions—Conduct the test in a laboratory
60 (1524) temperature of 70 to 77°F (23 6 2°C), unless otherwise
66 (1676) specified.
72 (1829)
84 (2134) 11.3 Chemical Resistance of Resin—Determine the chemi-
96 (2438)
108 (2743)
cal resistance of the resin in accordance with Practice C581.
120 (3048) 11.4 Glass Content—Determine the glass content of the
132 (3353)
144 (3658) inner liner and interior layer combined. Obtain a test sample by
carefully splitting these combined areas from the structural

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Nozzle Inside Diameter Permissible Angular Deviation, −0


Up to 10 in. (254mm) 1°
10 in. (254mm) and larger 1⁄ 2 °

NOTE 1—Larger tolerances may be agreed upon between purchaser and fabricator for tanks over 12 ft in diameter.
FIG. 8 Nozzle Location and Orientation Tolerances

layer. The glass content of the separated sample shall be D1599 with restrained end closures that prevent the application
determined in accordance with Test Method D2584. of axial tensile stress, or:
11.5 Degree of Cure—Degree of cure of the laminate shall 11.6.2.2 Strain-gage (hoop-elongation) tests on tanks filled
be found by determining the Barcol hardness using Barcol with water.
Model No. GYZJ934.1. Instrument calibration and method NOTE 21—Practical test methods on samples cut from filament-wound
shall be as described in Test Method D2583. specimens are not available to cover all cases of testing filament-wound
laminates. Other test methods for determination of hoop properties may be
11.6 Physical Properties: used when the fabricator can verify the validity of the selected method.
11.6.1 Contact Molded Laminates—Where required, physi-
cal properties of contact-molded laminates shall be determined 12. Product Marking
in accordance with the test methods listed in Specification
C582. 12.1 The tank shall be marked to identify the producer, date
11.6.2 Filament-Wound Laminates—Verify design stresses of manufacture, capacity, all resins used, inner surface
and moduli of elasticity of filament-wound tanks by manufac- reinforcements, specific gravity, design temperature, and the
turer’s test data based upon: words “Pressure-Atmospheric,” or the operating pressure and
11.6.2.1 Strain (that is, modulus) measurements of small- vacuum, shall be imprinted on the tank.
diameter filament-wound cylinders made to the same laminate 12.2 Additional marking requirements may be needed for
construction, helix angle, glass content, liner construction, and compliance with local codes. It is the responsibility of the
resin as the full-size tank, in accordance with Test Method purchaser/user to specify additional labeling requirements for

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D3299 − 18
the vessel, such as liquid content, operating and safety 14.3 A suitable means shall be provided at the open end of
instructions, and any other warnings necessitated by local open-top tanks to keep the loaded tank rigid.
codes.
14.4 Tanks shall be loaded to provide at least 2 in. (51 mm)
13. Packaging and Package Marking clearance between the tank (including fittings) and the bulk-
13.1 All packing, packaging, and marking provisions of heads or bed of the vehicle.
Practice D3892 shall apply to this specification. 14.5 When two or more tanks are shipped on the same
14. Shipping vehicle, sufficient clearance or padding shall be provided
between tanks to prevent contact in transit.
14.1 Since there are variations in the design of support
cradles, lifting- and hold-down lugs, and methods of shipping, 14.6 Upon arrival at the destination, the purchaser shall be
the manufacturer’s special instructions shall be followed in all responsible for inspection for damage in transit. If damage has
cases. occurred, a claim should be filed with the carrier by the
purchaser, and the supplier should be notified. If the damage is
14.2 Tanks shall be mounted on cradles if shipping
not first repaired by the fabricator prior to the tank being put
horizontally, or on a suitable skid or pallet if shipping in the
into service, the purchaser accepts all future responsibility for
vertical position. The cradles or skid shall be padded and
secured to the bed of the vehicle in such a manner that will the effects of tank failure resulting from such damage.
prevent damage to the tank with normal handling. The tank
shall be secured to the cradles or skid so that there can be no 15. Keywords
movement of the tank in relation to the skid or cradle under 15.1 above ground; atmospheric; filament wound; polyester;
normal handling. tank; vinylester

APPENDIXES

(Nonmandatory Information)

X1. HANDLING AND INSTALLATION

X1.1 Handling end of the tank. Tanks can be moved by positioning fork-lift
X1.1.1 The following normal precautions should be taken in trucks on either side of the tank with forks padded.
handling the tank at the destination: X1.1.1.7 Under no conditions should chains or cables be
X1.1.1.1 Proper rigging practices should be observed at all allowed to contact a tank. Full protection must be provided
times. Hoisting equipment operators should attach a guide line when using chains or cables. Do not attach lifting devices to
to prevent tank from swinging out of control. any fitting other than lifting lugs.
X1.1.1.2 The tank should not be dropped or allowed to X1.1.1.8 When storing the tank on the ground prior to
strike any other object. Damage caused by such action may installation, it should be placed on the shipping cradles and tied
result in cracking the inner corrosion-resistant liner, as well as down so that it cannot roll, due to wind or sloping ground.
the structural portion of the tank.
X1.1.1.3 The tank should not be rolled or slid on rough X1.2 Installation
ground. Never set a tank upon a fitting or other protrusion that X1.2.1 Vertical flat bottom tanks should be installed on a
may be attached to the shell. base provided continuous support and having sufficient
X1.1.1.4 In working around the tank, care should be exer- strength to support the weight of the tank full of liquid with
cised to prevent tools, scaffolding, or other objects from negligible deflection. Full support of the bottom should be
striking the tank or being dropped on, or inside the tank. obtained by one of the following:
Soft-soled shoes should be worn by workmen entering the X1.2.1.1 If the surface of the pad and the bottom of the tank
tank. Where ladders are used (inside and outside), all points of are flat and have no projections from the plane surface, the tank
contact with the tank should be cushioned to protect the surface may be set on such a surface.
from scratching or point loading. X1.2.1.2 If the conditions of X1.2.1.1 cannot be met,
X1.1.1.5 The use of a crane is recommended, both in lifting methods of support recommended by the manufacturer should
and positioning the tank. The clearance between the head be used.
shackle of the crane and the tank should be at least equal to the
span between the lugs used for lifting. If this is not possible, a X1.2.2 If the tank has a bottom drain, a hole should be
spreader bar must be used to approximate the same angle in provided in the pad with sufficient clearance so that the drain
lifting. and its flange will not contact the base at any point.
X1.1.1.6 Where tanks are not equipped with lifting lugs, it X1.2.3 Erection of Vertical Tank:
is recommended that such tanks be lifted with canvas or rope X1.2.3.1 Tanks should be handled with a crane, using the
slings (over 1 in. (25 mm) in diameter) positioned near each lifting lugs provided. Do not attempt to lift tank by attaching to

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D3299 − 18
other fittings. Prior to hoisting the top end, a suitable protection X1.2.3.3 Valves, controllers, or other heavy items connected
pad of material should be placed under the bottom pivot point to tank nozzle should be independently supported.
of tank so that as the tank rises, the strain is taken on the pad. X1.2.3.4 When agitators, mixers, or cooling/heating coils
The hoist wire should be connected to the top lifting lugs, and are to be installed, special design considerations must be used.
the tank should be raised carefully, using guide ropes to
prevent sudden swinging.
X1.2.3.2 All hold-down lugs supplied should be utilized to
secure the tank to its pad. Hold-down lugs should be grouted or
shimmied to prevent excessive loads being transferred to the
tank shell.

X2. DISHED BOTTOM

X2.1 An alternative method for calculating the thickness of


an elevated dished torispherical bottom head is as follows
(refer to 6.3.4 and see Fig. X2.1):

tc 5
PRc 0.036γ HRc
2S
5
2S S or
0.2489γHRc ,
2S D (X2.1)

ti 5
PRc W 0.036γHRc W
2S
5
2S S or
0.2489γ HRc W
2S D (X2.2)

where:
tc = head thickness in area of the crown radius, in. (mm),
ti = head thickness in area of the knuckle radius, in. (mm),
S = allowable stress, psi (kPa),
γ = specific gravity of fluid,
P = pressure, psi (kPa),
Rc = crown radius of dished head, in. (m),
H = fluid head, in. (mm),
W = stress intensification factor =

S D~
1
4
31 =R c /r i , !
and
ri = knuckle radius of the dished head, in. (mm).

FIG. X2.1 Thickness of Dished-Bottom Head

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X3. EXPRESSION OF HOOP TENSILE MODULUS OF A LAMINATE

X3.1 The hoop tensile modulus of a laminate, composed E FW = hoop modulus of filament winding,
partially of filament winding and partially of a contact molded ECB = modulus of corrosion barrier,
corrosion barrier, is expressed by: tL = corrosion barrier thickness,
tFW = filament winding thickness,
E FW*t FW E CB*t CB
ET 5 1 (X3.1) tT = total thickness, = tCB + tFW
tT tT

where: This expression will give a good approximation of total


laminate modulus for values of EFW of 3.0–6.0 × 106 psi
ET = hoop modulus of total laminate, (20.7–41.4 GPa).

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3517 − 19

Standard Specification for


“Fiberglass” (Glass-Fiber-Reinforced Thermosetting-Resin)
Pressure Pipe1
This standard is issued under the fixed designation D3517; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This specification covers machine-made fiberglass pipe, 2.1 ASTM Standards:2
8 in. (200 mm) through 156 in. (4000 mm), intended for use in C33/C33M Specification for Concrete Aggregates
water conveyance systems which operate at internal gage D638 Test Method for Tensile Properties of Plastics
pressures of 450 psi (3103 kPa) or less. Both glass-fiber- D695 Test Method for Compressive Properties of Rigid
reinforced thermosetting-resin pipe (RTRP) and glass-fiber- Plastics
reinforced polymer mortar pipe (RPMP) are fiberglass pipes. D790 Test Methods for Flexural Properties of Unreinforced
The standard is suited primarily for pipes to be installed in and Reinforced Plastics and Electrical Insulating Materi-
buried applications, although it may be used to the extent als
applicable for other installations such as, but not limited to, D883 Terminology Relating to Plastics
jacking, tunnel lining and slip-lining rehabilitation of existing D1600 Terminology for Abbreviated Terms Relating to Plas-
pipelines. tics
NOTE 1—For the purposes of this standard, polymer does not include
natural polymers. D2290 Test Method for Apparent Hoop Tensile Strength of
Plastic or Reinforced Plastic Pipe
1.2 The values stated in inch-pound units are to be regarded D2412 Test Method for Determination of External Loading
as the standard. The values given in parentheses are provided Characteristics of Plastic Pipe by Parallel-Plate Loading
for information purposes only.
D2584 Test Method for Ignition Loss of Cured Reinforced
NOTE 2—There is no known ISO equivalent to this standard.
Resins
1.3 The following safety hazards caveat pertains only to the D2992 Practice for Obtaining Hydrostatic or Pressure De-
test methods portion, Section 8, of this specification: This sign Basis for “Fiberglass” (Glass-Fiber-Reinforced
standard does not purport to address all of the safety concerns, Thermosetting-Resin) Pipe and Fittings
if any, associated with its use. It is the responsibility of the user
D3567 Practice for Determining Dimensions of “Fiberglass”
of this standard to establish appropriate safety, health, and
(Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
environmental practices and determine the applicability of
Fittings
regulatory limitations prior to use.
D3892 Practice for Packaging/Packing of Plastics
1.4 This international standard was developed in accor-
D4161 Specification for “Fiberglass” (Glass-Fiber-
dance with internationally recognized principles on standard-
Reinforced Thermosetting-Resin) Pipe Joints Using Flex-
ization established in the Decision on Principles for the
ible Elastomeric Seals
Development of International Standards, Guides and Recom-
F412 Terminology Relating to Plastic Piping Systems
mendations issued by the World Trade Organization Technical
F477 Specification for Elastomeric Seals (Gaskets) for Join-
Barriers to Trade (TBT) Committee.
ing Plastic Pipe
1
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced
2
Plastic Piping Systems and Chemical Equipment. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Aug. 1, 2019. Published August 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1976. Last previous edition approved 2014 as D3517 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D3517-19. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D3517 − 19
2.2 ISO Standard: stiffness by a capital letter. Table 1 presents a summary of the
ISO 1172 Textile Glass Reinforced Plastics—Determination designation requirements. Thus, a complete material code shall
of Loss on Ignition3 consist of ASTM D3517. . . three numerals, C . . . and two or
2.3 NSF Standard: three numerals, and a capital letter.
Standard No. 61 Drinking Water System Components4 NOTE 4—Examples of the designation are as follows: (1) ASTM
D3517-1-1-3-C50-A for glass-fiber reinforced aggregate and polyester
3. Terminology resin mortar pipe with a reinforced thermoset liner and an unreinforced
3.1 Definitions: polyester resin and sand surface layer, for operation at 50 psi (345 kPa),
and having a minimum pipe stiffness of 9 psi (62 kPa), (2) ASTM
3.1.1 General—Definitions are in accordance with Termi-
D3517-4-2-6-C200-C for glass-fiber reinforced epoxy resin pipe with a
nology D883 and Terminology F412 and abbreviations are in non-reinforced thermoset liner, no surface layer, for operation at 200 psi
accordance with Terminology D1600, unless otherwise indi- (1380 kPa), and having a minimum pipe stiffness of 36 psi (248 kPa).
cated. NOTE 5—Although the “Form and Style for ASTM Standards” manual
requires that the type classification be roman numerals, it is recognized
3.2 Definitions of Terms Specific to This Standard: that companies have stencil cutting equipment for this style of type, and
3.2.1 fiberglass pipe—a tubular product containing glass- it is therefore acceptable to mark the product type in arabic numbers.
fiber reinforcements embedded in or surrounded by cured
thermosetting resin. The composite structure may contain 5. Materials and Manufacture
aggregate, granular, or platelet fillers, thixotropic agents, 5.1 General—The thermosetting resins, glass fiber
pigments, or dyes. Thermoplastic or thermosetting liners or reinforcements, fillers, and other materials, when combined as
coatings may be included. a composite structure, shall produce piping products that meet
3.2.2 flexible joint —a joint that is capable of axial displace- the performance requirements of this specification.
ment or angular rotation, or both. 5.2 Wall Composition—The basic structural wall composi-
3.2.3 liner—a resin layer, with or without filler, or tion shall consist of thermosetting resin, glass fiber
reinforcement, or both, forming the interior surface of the pipe. reinforcement, and, if used, an aggregate filler.
3.2.4 qualification test—one or more tests used to prove the 5.2.1 Resin—A thermosetting polyester or epoxy resin, with
design of a product. Not a routine quality control test. or without filler.
5.2.2 Reinforcement—A commercial grade of glass fibers
3.2.5 reinforced polymer mortar pipe (RPMP)—a fiberglass compatible with the resin used.
pipe with aggregate. 5.2.3 Aggregate—A siliceous sand conforming to the re-
3.2.6 reinforced thermosetting resin pipe (RTRP)—a fiber- quirements of Specification C33/C33M, except that the re-
glass pipe without aggregate. quirements for gradation shall not apply.
3.2.7 rigid joint —a joint that is not capable of axial NOTE 6—Fiberglass pipe intended for use in the transport of potable
displacement or angular rotation. water should be evaluated and certified as safe for this purpose by a testing
3.2.8 surface layer—a resin layer, with or without filler, or agency acceptable to the local health authority. The evaluation should be
in accordance with requirements for chemical extraction, taste, and odor
reinforcements, or both, applied to the exterior surface of the that are no less restrictive than those included in National Sanitation
pipe structural wall. Foundation (NSF) Standard No. 61. The seal or mark of the laboratory
making the evaluation should be included on the fiberglass pipe.
4. Classification
5.3 Liner and Surface Layers—Liner or surface layer, or
4.1 General—This specification covers fiberglass pressure both, when incorporated into or onto the pipe, shall meet the
pipe defined by raw materials in the structural wall (type) and structural requirements of this specification.
liner, surface layer material (grade), operating pressure (class),
5.4 Joints—The pipe shall have a joining system that shall
and pipe stiffness. Table 1 lists the types, liners, grades, classes,
provide for fluid tightness for the intended service condition. A
and stiffnesses that are covered.
particular type of joint may be restrained or unrestrained and
NOTE 3—All possible combinations of types, liners, grades, classes, and flexible or rigid depending on the specific configuration and
stiffnesses may not be commercially available. Additional types, liners, design conditions.
grades, and stiffnesses may be added as they become commercially
available. The purchaser should determine for himself or consult with the
5.4.1 Unrestrained—Pipe joints capable of withstanding
manufacturer for the proper class, type, liner, grade and stiffness of pipe internal pressure but not longitudinal tensile loads.
to be used under the installation and operating conditions that will exist for 5.4.1.1 Coupling or Bell-and-Spigot Gasket Joints, with a
the project in which the pipe is to be used. groove either on the spigot or in the bell to retain an
4.2 Designation Requirements—The pipe materials designa- elastomeric gasket that shall be the sole element of the joint to
tion code shall consist of the standard designation, ASTM provide watertightness. For typical joint details see Fig. 1.
D3517, followed by type, liner, and grade in Arabic numerals, 5.4.1.2 Mechanical Coupling Joint, with elastomeric seals.
class by the letter C and two or three Arabic numerals, and pipe 5.4.1.3 Butt Joint, with laminated overlay.
5.4.1.4 Flanged Joint, both integral and loose ring.
3
5.4.2 Restrained—Pipe joints capable of withstanding inter-
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
nal pressure and longitudinal tensile loads..
4th Floor, New York, NY 10036, http://www.ansi.org.
4
Available from NSF International, P.O. Box 130140, 789 N. Dixboro Rd., Ann 5.4.2.1 Joints similar to those in 5.4.1.1 with supplemental
Arbor, MI 48113-0140, http://www.nsf.org. restraining elements.

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TABLE 1 General Designation Requirements for Fiberglass Pressure Pipe
Desig-
nation Property Cell Limits (Note 1)
Order

1 Type 1 2 3 4
glass-fiber-reinforced ther- glass-fiber-reinforced ther- glass-fiber-reinforced ther- glass-fiber-reinforced ther-
mosetting polyester (Note 2) resin mosetting polyester (Note 2) resin mosetting epoxy resin mor- mosetting epoxy resin
mortar (RPMP polyester (Note 2)) (RTRP polyester (Note 2)) tar (RPMP epoxy) (RTRP epoxy)
2 Liner 1 2 3 4
reinforced thermoset liner non-reinforced thermoset liner thermoplastic liner no liner

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3 Grade 1 2 3 4 5 6

3
polyester (Note 2) polyester (Note 2) polyester (Note 2) epoxy resin sur- epoxy resin sur- no surface
resin surface layer—reinforced resin surface resin and sand surface face layer— face layer—non- layer
layer—non- layer nonreinforced reinforced reinforced
reinforced
D3517 − 19

4 Class (Note 3) C50 C100 C150 C200 C250 C300 C350 C400 C450

5 Pipe Stiffness A B C D
psi (kPa) 9 (62) 18 (124) 36 (248) 72 (496)

NOTE 1—The cell-type format provides the means of identification and specification of piping materials. This cell-type format, however, is subject to misapplication since unobtainable property
combinations can be selected if the user is not familiar with non-commercially available products. The manufacturer should be consulted.
NOTE 2—For the purposes of this standard, polyester includes vinyl ester resins.
NOTE 3— Based on operating pressure in psig (numerals).

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D3517 − 19

FIG. 1 Typical Joints

FIG. 2 Beam Strength—Test Setup

5.4.2.2 Butt Joint, with laminated overlay. 6.1.2 The inside surface of each pipe shall be free of bulges,
5.4.2.3 Bell-and-Spigot, with laminated overlay. dents, ridges, and other defects that result in a variation of
5.4.2.4 Bell-and-Spigot, adhesive-bonded joint: Three types inside diameter of more than 1⁄8 in. (3.2 mm) from that obtained
of adhesive-bonded joints are permitted by this standard as on adjacent unaffected portions of the surface. No glass fiber
follows: reinforcement shall penetrate the interior surface of the pipe
(1) Tapered bell-and-spigot, an adhesive joint that is manu- wall.
factured with a tapered socket for use in conjunction with a 6.1.3 Joint sealing surfaces shall be free of dents, gouges,
tapered spigot and a suitable adhesive. and other surface irregularities that will affect the integrity of
(2) Straight bell-and-spigot, an adhesive joint that is manu- the joints.
factured with an untapered socket for use in conjunction with 6.2 Dimensions:
an untapered spigot and a suitable adhesive. 6.2.1 Pipe Diameters—Pipe shall be supplied in the nominal
(3) Tapered bell and straight spigot, an adhesive joint that diameters shown in Table 2 or Table 3. The pipe diameter
is manufactured with a tapered socket for use with an unta- tolerances shall be as shown in Table 2 or Table 3, when
pered spigot and a suitable adhesive. measured in accordance with 8.1.1.
5.4.2.5 Flanged Joint, both integral and loose ring 6.2.2 Lengths—Pipe shall be supplied in nominal lengths of
5.4.2.6 Mechanical Coupling, an elastomeric sealed cou- 10, 20, 30, 40, and 60 ft. (3.05, 6.10, 9.15, 12.19, and 18.29 m).
pling with a supplemental restraining elements. The actual laying length shall be the nominal length 62 in.
5.4.2.7 Threaded Joints. (651 mm), when measured in accordance with 8.1.2. At least
NOTE 7—Other types of joints may be added as they become commer- 90 % of the total footage of any one size and class, excluding
cially available. special order lengths, shall be furnished in the nominal lengths
NOTE 8—Restrained joints typically increase service loads on the pipe specified by the purchaser. Random lengths, if furnished, shall
to greater than those experienced with unrestrained joints. The purchaser
is cautioned to take into consideration all conditions that may be not vary from the nominal lengths by more than 5 ft (1.53 m)
encountered in the anticipated service and to consult the manufacturer or 25 %, whichever is less.
regarding the suitability of a particular type and class of pipe for service 6.2.3 Wall Thickness—The average wall thickness of the
with restrained joint systems. pipe shall not be less than the nominal wall thickness published
5.5 Gaskets—Elastomeric gaskets when used with this pipe in the manufacturer’s literature current at the time of purchase,
shall conform to the requirements of Specification F477. and the minimum wall thickness at any point shall not be less
than 87.5 % of the nominal wall thickness when measured in
6. Requirements accordance with 8.1.3.
6.1 Workmanship: 6.2.4 Squareness of Pipe Ends—All points around each end
6.1.1 Each pipe shall be free from all defects including of a pipe unit shall fall within 61⁄4 in. (66.4 mm) or 60.5 %
indentations, delaminations, bubbles, pinholes, cracks, pits, of the nominal diameter of the pipe, whichever is greater, to a
blisters, foreign inclusions, and resin-starved areas that due to plane perpendicular to the longitudinal axis of the pipe, when
their nature, degree, or extent, detrimentally affect the strength measured in accordance with 8.1.4.
and serviceability of the pipe. The pipe shall be as uniform as 6.3 Soundness—Unless otherwise agreed upon between pur-
commercially practicable in color, opacity, density, and other chaser and supplier, test each length of pipe up to 96 in. (2400
physical properties. mm) diameter hydrostatically without leakage or cracking, at

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D3517 − 19
TABLE 2 Nominal Inside Diameters (ID) and Tolerances Inside Diameter Control Pipe
Inch-Pound Units SI Units

Nominal Nominal Metric ID RangeB , mm ToleranceB on


Tolerance, in. Declared ID,
DiameterA , in. DiameterB , mm Minimum Maximum mm

8 ±0.25 200 196 204 ±1.5


10 ±0.25 250 246 255 ±1.5
12 ±0.25 300 296 306 ±1.8
14 ±0.25 400 396 408 ±2.4
15 ±0.25 500 496 510 ±3.0
16 ±0.25 600 595 612 ±3.6
18 ±0.25 700 695 714 ±4.2
20 ±0.25 800 795 816 ±4.2
21 ±0.25 900 895 918 ±4.2
24 ±0.25 1000 995 1020 ±5.0
27 ±0.27 1200 1195 1220 ±5.0
30 ±0.30 1400 1395 1420 ±5.0
33 ±0.33 1600 1595 1620 ±5.0
36 ±0.36 1800 1795 1820 ±5.0
39 ±0.39 2000 1995 2020 ±5.0
42 ±0.42 (2200) 2195 2220 ±6.0
45 ±0.45 2400 2395 2420 ±6.0
48 ±0.48 (2600) 2595 2620 ±6.0
51 ±0.51 2800 2795 2820 ±6.0
54 ±0.54 (3000) 2995 3020 ±6.0
60 ±0.60 3200 3195 3220 ±7.0
66 ±0.66 (3400) 3395 3420 ±7.0
72 ±0.72 3600 3595 3620 ±7.0
78 ±0.78 (3800) 3795 3820 ±7.0
84 ±0.84 4000 3995 4020 ±7.0
90 ±0.90 ... ... ... ...
96 ±0.96 ... ... ... ...
102 ±1.00 ... ... ... ...
108 ±1.00 ... ... ... ...
114 ±1.00 ... ... ... ...
120 ±1.00 ... ... ... ...
132 ±1.00 ... ... ... ...
144 ±1.00 ... ... ... ...
156 ±1.00 ... ... ... ...
A
Inside diameters other than those shown shall be permitted by agreement between purchaser and supplier.
B
Values are taken from International Standards Organization documents. Parentheses indicate non-preferred diameters.

the internal hydrostatic proof pressures specified for the specimen evidenced by surface cracks. At deflection level B
applicable class in Table 4, when tested in accordance with 8.2. per Table 7, there shall be no indication of structural damage as
For sizes over 96 in. (2400 mm), the frequency of hydrostatic evidenced by interlaminar separation, separation of the liner or
leak tests shall be as agreed upon by purchaser and supplier. surface layer (if incorporated) from the structural wall, tensile
6.4 Hydrostatic Design Basis: failure of the glass fiber reinforcement, and fracture or buck-
6.4.1 Long-Term Hydrostatic Pressure—The pressure ling of the pipe wall.
classes shall be based on long-term hydrostatic pressure data NOTE 10—This is a visual observation (made with the unaided eye) for
obtained in accordance with 8.3 and categorized in accordance quality control purposes only and should not be considered a simulated
with Table 5. Pressure classes are based on extrapolated service test. Table 7 values are based on an in-use long-term deflection
limit of 5 % and provide an appropriate uniform safety margin for all pipe
strengths at 50 years. For pipe subjected to longitudinal loads stiffnesses. Since the pipe stiffness values (F/∆y) shown in Table 6 vary,
or circumferential bending, the effect of these conditions on the the percent deflection of the pipe under a given set of installation
hydrostatic design pressure, classification of the pipe must be conditions will not be constant for all pipes. To avoid possible
considered. misapplication, take care to analyze all conditions which might affect
6.4.2 Control Requirements—Test pipe specimens periodi- performance of the installed pipe.
cally in accordance with Practice D2992. 6.5.1 For other pipe stiffness levels, appropriate values for
Level A and Level B deflections (Table 7) may be computed as
NOTE 9—Hydrostatic design basis (HDB-extrapolated value at 50
years) determined in accordance with Procedure A of Practice D2992, may follows:
be substituted for the Procedure B evaluation required by 8.3. It is
generally accepted that the Procedure A HDB value times 3 is equivalent
to the Procedure B HDB value.
Level A at new PS 5 S 72
new PS D 0.33

~9! (1)

Level B at new PS 5 new Level A÷0.6


6.5 Stiffness—Each length of pipe shall have sufficient
strength to exhibit the minimum pipe stiffness (F/∆y) specified 6.5.2 Since products may have use limits of other than 5 %
in Table 6, when tested in accordance with 8.4. At deflection long-term deflection, Level A and Level B deflections (Table 7)
level A per Table 7, there shall be no visible damage in the test may be proportionally adjusted to maintain equivalent in-use

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D3517 − 19
TABLE 3 Nominal Outside Diameters (OD) and Tolerances
NOTE 1—The external diameter of the pipe at the spigots shall be within the tolerances given in the table, and the manufacturer shall declare his
allowable maximum and minimum spigot diameters. Some pipes are manufactured such that the entire pipe meets the OD tolerances while other pipes
meet the tolerances at the spigots, in which case, if such pipes are cut (shortened) the ends may need to be calibrated to meet the tolerances.

Metric Ductile Iron Pipe Tolerance Upper, Tolerance Lower, International O.D., Tolerance Upper, Tolerance Lower,
Pipe Size, mm Equivalent, mm mm mm mm mm mm
200 220.0 +1.0 0.0 ... ... ...
250 271.8 +1.0 -0.2 ... ... ...
300 323.8 +1.0 -0.3 310 +1.0 -1.0
350 375.7 +1.0 -0.3 361 +1.0 -1.2
400 426.6 +1.0 -0.3 412 +1.0 -1.4
450 477.6 +1.0 -0.4 463 +1.0 -1.6
500 529.5 +1.0 -0.4 514 +1.0 -1.8
600 632.5 +1.0 -0.5 616 +1.0 -2.0
700 718 +1.0 -2.2
800 820 +1.0 -2.4
900 924 +1.0 -2.6
1000 1026 +2.0 -2.6
1200 1229 +2.0 -2.6
1400 1434 +2.0 -2.8
1600 1638 +2.0 -2.8
1800 1842 +2.0 -3.0
2000 2046 +2.0 -3.0
2200 2250 +2.0 -3.2
2400 2453 +2.0 -3.4
2600 2658 +2.0 -3.6
2800 2861 +2.0 -3.8
3000 3066 +2.0 -4.0
3200 3270 +2.0 -4.2
3400 3474 +2.0 -4.4
3600 3678 +2.0 -4.6
3800 3882 +2.0 -4.8
4000 4086 +2.0 -5.0

safety margins. For example, a 4 % long-term limiting deflec- 6.5.3 For high stiffness pipes, 5 % deflection will likely be
tion would result in a 20 % reduction of Level A and Level B above the use limit and the adjusted level A test deflection. For
deflections, while a 6 % limiting deflection would result in a very high stiffness pipes, 5 % deflection may also be greater
20 % increase in Level A and Level B deflection values. than the adjusted level B test deflection. In such cases, the
However, minimum values for Level A and Level B deflections pipes may be damaged or fail prior to determining the pipe
shall be equivalent to strains of 0.6 and 1.0 % respectively (as stiffness at 5 % deflection. Therefore, it is permitted to set the
computed by Eq X1.4 in Appendix X1 of Specification pipe stiffness test deflection equal to the adjusted level A
D3262).

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D3517 − 19
TABLE 4 Hydrostatic-Pressure Test 6.6.1 Alternative Requirements—When agreed upon be-
Hydrostatic Proof Pressure tween the purchaser and the supplier, the minimum hoop-
Pressure Pipe Diameters Pipe Diameters tensile strength shall be as determined in accordance with
Class up to and >54 in. up to and
Including 54 in. Including 96 in. 8.5.1.
(psi) psi (kPa) psi (kPa)
C50 100 (689) 75 (517)
6.7 Joint Tightness—All joints shall meet the laboratory
C100 200 (1379) 150 (1034) performance requirements, of Specification D4161. Unre-
C150 300 (2068) 225 (1551) strained joints shall be tested with a fixed end closure condition
C200 400 (2757) 300 (2068)
C250 500 (3447) 375 (2585)
and restrained joints shall be tested with a free end closure
C300 600 (4136) 450 (3102) condition. Rigid joints shall be exempt from angular deflection
C350 700 (4826) 525 (3619) requirements of D4161. Rigid joints typically include butt
C400 800 (5515) 600 (4136)
C450 900 (6205) 675 (4654)
joints with laminated overlay, bell-and-spigot joints with lami-
nated overlay, flanged, bell-and-spigot adhesive bonded and
threaded.
TABLE 5 Long-Term Hydrostatic Pressure Categories 6.8 Longitudinal Strength:
Minimum Calculated Values of 6.8.1 Beam Strength—For pipe sizes up to 27 in. the pipe
Class Long-Term Hydrostatic
Pressure gage, psi (kPa)
shall withstand, without failure, the beam loads specified in
C50 90 (621)
Table 9, when tested in accordance with 8.6.1. For pipe sizes
C100 180 (1241) larger than 27 in., and alternatively for smaller sizes, adequate
C150 270 (1862) beam strength is demonstrated by tension and compression
C200 360 (2482)
C250 450 (3103)
tests conducted in accordance with 8.6.2 and 8.6.3,
C300 540 (3722) respectively, for pipe wall specimens oriented in the longitu-
C350 630 (4343) dinal direction, using the minimum tensile and compressive
C400 720 (4963)
C450 810 (5584)
strength specified in Table 9.
6.8.2 Longitudinal Tensile Strength—All pipe manufactured
under this specification shall have a minimum axial tensile
TABLE 6 Minimum Stiffness at 5 % Deflection elongation at failure of 0.25% and meet or exceed the longi-
Pipe Stiffness, psi (kPa) tudinal tensile strength shown for each size and class in Table
Nominal
Diameter, Designation 10, when tested in accordance with 8.6.2.
in. A B C D NOTE 12—The values listed in Table 10 are the minimum criteria for
8 ... ... 36 (248) 72 (496) products made to this standard. The values may not be indicative of the
10 ... 18 (124) 36 (248) 72 (496) axial strength of some products, or of the axial strength required by some
12 and greater 9 (62) 18 (124) 36 (248) 72 (496) installation conditions and joint configurations.
6.8.3 Conformance to the requirements of 6.8.1 shall satisfy
TABLE 7 Ring Deflection Without Damage or Structural Failure
the requirements of 6.8.2 for those pipe sizes and classes where
the minimum longitudinal tensile strength values of Table 9 are
Nominal Pipe
Stiffness, psi equal to the values of Table 10. Conformance to the require-
9 18 36 72 ments of 6.8.2 shall satisfy the longitudinal tensile strength
Level A 18 % 15 % 12 % 9% requirements of 6.8.1.
Level B 30 % 25 % 20 % 15 %
7. Sampling
7.1 Lot—Unless otherwise agreed upon between the pur-
chaser and the supplier, one lot shall consist of 100 lengths of
each type, grade, and size of pipe produced.
deflection, but not greater than 5 %. See Note 11 for additional
information and further clarification. 7.2 Production Tests—Select one pipe at random from each
lot and take one specimen from the pipe barrel to determine
NOTE 11—Depending upon the product modulus and allowable ring conformance of the material to the workmanship, dimensional,
bending strain, this will likely begin affecting pipes with stiffness between and stiffness, and strength requirements of 6.1, 6.2, 6.5, and
200 and 400 psi. For example, a pipe with pipe stiffness of PS360 may 6.6, respectively. Unless otherwise agreed upon between pur-
have a use limit of 4.3 %, an adjusted level A deflection of 4.5 % and an
chaser and supplier, all pipes (up to 96-in. (2400-mm) diam-
adjusted level B deflection of 7.5 %. Therefore, the new pipe stiffness test
deflection would be 4.5 %. Another possible product with a pipe stiffness eter) shall meet the soundness requirements of 6.3.
of PS900 may have a use limit of 2.8 %, an adjusted level A deflection of 7.3 Qualification Tests—Sampling for qualification tests
2.7 % and an adjusted level B deflection of 4.5%. Therefore, the new pipe (see section 3.2.4) is not required unless otherwise agreed upon
stiffness test deflection would be 2.7 %.
between the purchaser and the supplier. Qualification tests, for
6.6 Hoop-Tensile Strength—All pipe manufactured under which a certification and test report shall be furnished when
this specification shall meet or exceed the hoop-tensile strength requested by the purchaser include the following:
shown for each size and class in Table 8, when tested in 7.3.1 Long-Term Hydrostatic Pressure Test.
accordance with 8.5. 7.3.2 Joint-Tightness Test (See 6.7).

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TABLE 8 Minimum Hoop Tensile Strength of Pipe Wall
NOTE 1—The values in this table are equal to 2PD, where P is the pressure class in psi and D is the nominal diameter in inches.
Inch-Pound Units
Hoop Tensile Strength, lbf/in. Width
Nominal
Pressure Class
Diameter
C50 C100 C150 C200 C250 C300 C350 C400 C450
(in.)
(psi) (psi) (psi) (psi) (psi) (psi) (psi) (psi) (psi)
8 800 1600 2400 3200 4000 4800 5600 6400 7200
10 1000 2000 3000 4000 5000 6000 7000 8000 9000
12 1200 2400 3600 4800 6000 7200 8400 9600 10 800
14 1400 2800 4200 5600 7000 8400 9800 11 200 12 600
15 1500 3000 4500 6000 7500 9000 10 500 12 000 13 500
16 1600 3200 4800 6400 8000 9600 11 200 12 800 14 400
18 1800 3600 5400 7200 9000 10 800 12 600 14 400 16 200
20 2000 4000 6000 8000 10 000 12 000 14 000 16 000 18 000
21 2100 4200 6300 8400 10 500 12 600 14 700 16 800 18 900
24 2400 4800 7200 9600 12 000 14 400 16 800 19 200 21 600
27 2700 5400 8100 10 800 13 500 16 200 18 900 21 600 24 300
30 3000 6000 9000 12 000 15 000 18 000 21 000 24 000 27 000
33 3300 6600 9900 13 200 16 500 19 800 23 100 26 400 29 700
36 3600 7200 10 800 14 400 18 000 21 600 25 200 28 800 32 400
39 3900 7800 11 700 15 600 19 500 23 400 27 300 31 200 35 100
42 4200 8400 12 600 16 800 21 000 25 200 29 400 33 600 37 800
45 4500 9000 13 500 18 000 22 500 27 000 31 500 36 000 40 500
48 4800 9600 14 400 19 200 24 000 28 800 33 600 38 400 43 200
51 5100 10 200 15 300 20 400 25 500 30 600 35 700 40 800 45 900
54 5400 10 800 16 200 21 600 27 000 32 400 37 800 43 200 48 600
60 6000 12 000 18 000 24 000 30 000 36 000 42 000 48 000 54 000
66 6600 13 200 19 800 26 400 33 000 39 600 46 200 52 800 59 400
72 7200 14 400 21 600 28 800 36 000 43 200 50 400 57 600 64 800
78 7800 15 600 23 400 31 200 39 000 46 800 54 600 62 400 70 200
84 8400 16 800 25 200 33 600 42 000 50 400 58 800 67 200 75 600
90 9000 18 000 27 000 36 000 45 000 54 000 63 000 72 000 81 000
96 9600 19 200 28 800 38 400 48 000 57 600 67 200 76 800 86 400
102 10 200 20 400 30 600 40 800 51 000 61 200 71 400 81 600 91 800
108 10 800 21 600 32 400 43 200 54 000 64 800 75 600 86 400 97 200
114 11 400 22 800 34 200 45 600 57 000 68 400 79 800 91 200 10 2600
120 12 000 24 000 36 000 48 000 60 000 72 000 84 000 96 000 108 000
132 13 200 26 400 39 600 52 800 66 000 79 200 92 400 105 600 118 800
144 14 400 28 800 43 200 57 600 72 000 86 400 100 800 115 200 129 600
156 15 600 31 200 46 800 62 400 78 000 93 600 109 200 124 800 140 400
SI Units
Hoop Tensile Strength N/mm Width
Pressure
C50 C100 C150 C200 C250 C300 C350 C400 C450
Class
Nominal
345 689 1034 1379 1724 2069 2414 2759 3103
Diameter
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa)
(mm)
200 138 276 414 552 690 828 966 1104 1241
250 173 345 517 690 862 1035 1207 1380 1552
300 207 413 620 827 1034 1241 1448 1655 1862
350 242 482 724 965 1207 1448 1690 1931 2172
375 259 517 776 1034 1293 1552 1811 2069 2327
400 276 551 827 1103 1379 1655 1931 2207 2482
450 311 620 931 1241 1552 1862 2173 2483 2793
500 345 689 1034 1379 1724 2069 2414 2759 3103
550 380 758 1137 1517 1896 2276 2655 3035 3413
600 414 827 1241 1655 2069 2483 2897 3311 3724
700 483 965 1448 1931 2414 2897 3380 3863 4344
750 518 1034 1551 2069 2586 3104 3621 4139 4655
850 587 1171 1758 2344 2931 3517 4104 4690 5275
900 621 1240 1861 2482 3103 3724 4345 4966 5585
1000 690 1378 2068 2758 3448 4138 4828 5518 6206
1100 759 1516 2275 3034 3793 4552 5311 6070 6827
1150 794 1585 2378 3172 3965 4759 5552 6346 7137
1200 828 1654 2482 3310 4138 4966 5794 6622 7447
1300 897 1791 2688 3585 4482 5379 6276 7173 8068
1400 966 1929 2895 3861 4827 5793 6759 7725 8688
1500 1035 2067 3102 4137 5172 6207 7242 8277 9309
1700 1173 2343 3516 4689 5862 7035 8208 9381 10 550
1800 1242 2480 3722 4964 6206 7448 8690 9932 11 171
2000 1380 2756 4136 5516 6896 8276 9656 11 036 12 412
2200 1518 3032 4550 6068 7586 9104 10 622 12 140 13 653
2300 1587 3169 4756 6343 7930 9517 11 104 12 691 14 274
2400 1656 3307 4963 6619 8275 9931 11 587 13 243 14 894
2600 1794 3583 5377 7171 8965 10 759 12 553 14 347 16 136

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2800 1932 3858 5790 7722 9654 11 586 13 518 15 450 17 377
2900 2001 3996 5997 7998 9999 12 000 14 001 16 002 17 997
3000 2070 4134 6204 8274 10 344 12 414 14 484 16 554 18 618
3400 2346 4685 7031 9377 11 723 14 069 16 415 18 761 21 100
3600 2484 4961 7445 9929 12 413 14 897 17 381 19 865 22 342
4000 2760 5512 8272 11 032 13 792 16 552 19 312 22 072 24 824

TABLE 9 Beam-Strength Test Loads 8. Test Methods


Minimum
Minimum
Longitudinal 8.1 Dimensions:
Longitudinal
Nominal Beam Load
Tensile Strength,
Compressive 8.1.1 Diameters:
Diameter, (P) Strength,
in.
per Unit of
per Unit of 8.1.1.1 Inside Diameter—Take inside diameter measure-
Circumference
Circumference ments at a point approximately 6 in. (152 mm) from the end of
lbf (kN) lbf/in. (kN/m) lbf/in. (kN/m) the pipe section using a steel tape or an inside micrometer with
8 800 (3.6) 580 (102) 580 (102) graduations of 1⁄16 in. (1 mm) or less. Make two 90° opposing
10 1200 (5.3) 580 (102) 580 (102) measurements at each point of measurement and average the
12 1600 (7.1) 580 (102) 580 (102)
14 2200 (9.8) 580 (102) 580 (102) readings.
15 2600 (11.6) 580 (102) 580 (102) 8.1.1.2 Outside Diameter—Determine in accordance with
16 3000 (13.3) 580 (102) 580 (102)
18 4000 (17.8) 580 (102) 580 (102)
Test Method D3567.
20 4400 (19.6) 580 (102) 580 (102) 8.1.2 Length—Measure with a steel tape or gage having
21 5000 (22.2) 580 (102) 580 (102) graduations of 1⁄16 in. (1 mm) or less. Lay the tape or gage on
24 6400 (28.5) 580 (102) 580 (102)
27 8000 (35.6) 580 (102) 580 (102) or inside the pipe and measure the overall laying length of the
30 ... ... 580 (102) 580 (102) pipe.
33 ... ... 640 (111) 640 (111)
36 ... ... 700 (122) 700 (122)
8.1.3 Wall Thickness—Determine in accordance with Test
39 ... ... 780 (137) 780 (137) Method D3567.
42 ... ... 800 (140) 800 (140) 8.1.4 Squareness of Pipe Ends—Rotate the pipe on a man-
45 ... ... 860 (150) 860 (150)
48 ... ... 920 (161) 920 (161) drel or trunnions and measure the runout of the ends with a dial
51 ... ... 980 (171) 980 (171) indicator. The total indicated reading is equal to twice the
54 ... ... 1040 (182) 1040 (182) distance from a plane perpendicular to the longitudinal axis of
60 ... ... 1140 (200) 1140 (200)
66 ... ... 1260 (220) 1260 (220) the pipe. Alternatively, when squareness of pipe ends is rigidly
72 ... ... 1360 (238) 1360 (238) fixed by tooling, the tooling may be verified and reinspected at
78 ... ... 1480 (260) 1480 (260) frequent enough intervals to ensure that the squareness of the
84 ... ... 1600 (280) 1600 (280)
90 ... ... 1720 (301) 1720 (301) pipe ends is maintained within tolerance.
96 ... ... 1840 (322) 1840 (322)
102 ... ... 1940 (340) 1940 (340) 8.2 Soundness—Determine soundness by a hydrostatic
108 ... ... 2060 (360) 2060 (360) proof test procedure. Place the pipe in a hydrostatic pressure
114 ... ... 2180 (382) 2180 (382) testing machine that seals the ends and exerts no end loads. Fill
120 ... ... 2280 (400) 2280 (400)
132 ... ... 2520 (440) 2520 (440) the pipe with water, expelling all air, and apply internal water
144 ... ... 2740 (480) 2740 (480) pressure at a uniform rate not to exceed 50 psi (345 kPa)/s until
156 ... ... 2964 (519) 2964 (519) the Table 4 test pressure specified in accordance with 6.3 is
reached. Maintain this pressure for a minimum of 30 s. The
pipe shall show no visual signs of weeping, leakage, or fracture
of the structural wall.
7.3.3 Longitudinal-Strength Test, including: 8.3 Long-Term Hydrostatic Pressure—Determine the long-
term hydrostatic pressure at 50 years in accordance with
7.3.3.1 Beam strength and
Procedure B of Practice D2992, with the following exceptions
7.3.3.2 Longitudinal tensile strength. permitted:
7.4 Control Tests—The following test is considered a con- 8.3.1 Test at ambient temperatures between 50 and 110°F
trol requirement and shall be performed as agreed upon (10 and 43.5°C) and report the temperature range experienced
between the purchaser and the supplier: during the tests.
7.4.1 Soundness Test—102-in. (2600-mm) diameter pipe NOTE 13—Tests indicate no significant effects on long-term hydrostatic
and larger. pressure within the ambient temperature range specified.
7.4.2 Perform the sampling and testing for the control 8.3.2 Determine the hydrostatic design basis for the glass
requirements for hydrostatic design basis at least once every fiber reinforcement in accordance with the method in Annex
two years. A1.
7.5 For individual orders conduct only those additional tests 8.3.3 Calculate the long-term hydrostatic pressure and cat-
and numbers of tests specifically agreed upon between the egorize by class in accordance with Table 5. A1.6 explains how
purchaser and the supplier. to calculate the long-term hydrostatic pressure.

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D3517 − 19
TABLE 10 Longitudinal Tensile Strength of Pipe Wall
Inch-Pound Units
Longitudinal Tensile Strength lbf/in. of Circumference
Nominal
Pressure Class
Diameter
C50 C100 C150 C200 C250 C300 C350 C400 C450
(in.)
(psi) (psi) (psi) (psi) (psi) (psi) (psi) (psi) (psi)
8 580 580 580 580 580 624 700 800 900
10 580 580 580 580 650 780 875 1000 1125
12 580 580 580 624 780 936 1050 1200 1350
14 580 580 609 728 910 1092 1225 1400 1575
15 580 580 653 780 975 1170 1313 1500 1688
16 580 580 696 832 1040 1248 1400 1600 1800
18 580 580 783 936 1170 1404 1575 1800 2025
20 580 580 870 1040 1300 1560 1750 2000 2250
21 580 609 914 1092 1365 1638 1838 2100 2363
24 580 696 1044 1248 1560 1800 2100 2400 2700
27 580 783 1175 1404 1688 2025 2363 2700 3038
30 580 870 1305 1560 1875 2250 2625 3000 3375
33 627 957 1436 1716 2063 2475 2888 3300 3713
36 684 1044 1566 1800 2250 2700 3150 3600 4050
39 741 1131 1697 1872 2340 2808 3276 3744 4212
42 798 1218 1827 2016 2520 3024 3528 4032 4536
45 855 1305 1958 2160 2700 3240 3780 4320 4860
48 912 1392 2088 2304 2880 3456 4032 4608 5184
51 969 1479 2219 2448 3060 3672 4284 4896 5508
54 1026 1566 2349 2592 3240 3726 4347 4968 5589
60 1140 1740 2520 2880 3600 4140 4830 5520 6210
66 1254 1914 2673 3036 3795 4554 5313 5808 6534
72 1368 2088 2916 3312 4140 4968 5796 6336 7128
78 1482 2106 3159 3432 4290 5148 6006 6864 7722
84 1596 2268 3402 3696 4620 5292 6174 7056 7938
90 1710 2430 3645 3960 4950 5670 6615 7380 8303
96 1824 2592 3888 4224 5280 6048 7056 7680 8640
102 1938 2754 4131 4488 5610 6426 7497 8160 9180
108 2052 2916 4374 4752 5940 6804 7938 8640 9720
114 2166 3078 4617 5016 6270 7182 8379 9120 10 260
120 2280 3240 4860 5280 6600 7560 8820 9600 10 800
132 2508 3564 5346 5808 7260 8316 9702 10 560 11 880
144 2736 3888 5832 6336 7920 9072 10 584 11 520 12 960
156 2964 4212 6318 6864 8580 9828 11 466 12 480 14 040
SI Units
Longitudinal Tensile Strength N/mm of Circumference
Pressure
C50 C100 C150 C200 C250 C300 C350 C400 C450
Class
Nominal
345 689 1034 1379 1724 2069 2414 2759 3103
Diameter
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa)
(mm)
200 102 102 102 102 102 109 123 140 158
250 102 102 102 102 114 137 153 175 197
300 102 102 102 109 137 164 184 210 236
350 102 102 107 127 159 191 215 245 276
375 102 102 114 137 171 205 230 263 296
400 102 102 122 146 182 219 245 280 315
450 102 102 137 164 205 246 276 315 355
500 102 102 152 182 228 273 306 350 394
550 102 107 160 191 239 287 322 368 414
600 102 122 183 219 273 315 368 420 473
700 102 137 206 246 296 355 414 473 532
750 102 152 229 273 328 394 460 525 591
850 110 168 251 301 361 433 506 578 650
900 120 183 274 315 394 473 552 630 709
1000 130 198 297 328 410 492 574 656 738
1100 140 213 320 353 441 530 618 706 794
1150 150 229 343 378 473 567 662 757 851
1200 160 244 366 403 504 605 706 807 908
1300 170 259 388 429 536 643 750 857 965
1400 180 274 411 454 567 652 761 870 979
1500 200 305 441 504 630 725 846 967 1087
1700 220 335 468 532 665 797 930 1017 1144
1800 240 366 511 580 725 870 1015 1110 1248
2000 260 369 553 601 751 902 1052 1202 1352
2200 279 397 596 647 809 927 1081 1236 1390
2300 299 426 638 693 867 993 1158 1292 1454
2400 319 454 681 740 925 1059 1236 1345 1513
2600 339 482 723 786 982 1125 1313 1429 1608
2800 359 511 766 832 1040 1192 1390 1513 1702
2900 379 539 809 878 1098 1258 1467 1597 1797

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3000 399 567 851 925 1156 1324 1545 1681 1891
3400 439 624 936 1017 1271 1456 1699 1849 2080
3600 479 681 1021 1110 1387 1589 1853 2017 2270
4000 519 738 1106 1202 1503 1721 2008 2185 2459

8.4 Stiffness—Determine the pipe stiffness (F/∆y) at 5 % Si = initial design hoop tensile stress, psi,
deflection or the adjusted level determined in accordance with Sr = hoop tensile stress at rated operating pressure, psi,
6.5.3 for the specimen, using the apparatus and procedure of P = rated operating pressure class, psi, and
Test Method D2412, with the following exceptions permitted: r = inside radius of pipe, in.
8.4.1 Measure the wall thickness to the nearest 0.01 in. NOTE 15—A value of F less than 4 Pr results in a lower factor of safety
(0.25 mm). on short term loading than required by the values in Table 8.
8.4.2 Load the specimen to 5 % deflection or the adjusted The value for Si should be established by considering the
level determined in accordance with 6.5.3 and record the load. variations in glass reinforcement strength and manufacturing
Then load the specimen to deflection level A per Table 7 or to methods, but in any case should not be less than the 95 % lower
the adjusted level A deflection determined in accordance with confidence value on stress at 0.1 h, as determined by the
6.5.1 and 6.5.2 and examine the specimen for visible damage manufacturer’s testing carried out in accordance with 6.4. The
evidenced by surface cracks. Then load the specimen to value for Sr should be established from the manufacturer’s
deflection level B per Table 7 or to the adjusted level B hydrostatic design basis.
deflection determined in accordance with 6.5.1 and 6.5.2 and
8.6 Longitudinal Strength:
examine for evidence of structural damage, as evidenced by
8.6.1 Beam Strength—Place a 20-ft (6.1-m) nominal length
interlaminar separation, separation of the liner or surface layer
of pipe on saddles at each end. Hold the ends of the pipe round
(if incorporated) from the structural wall, tensile failure of the
during the test. Apply beam load for the diameter of pipe
glass fiber reinforcement, and fracture or buckling of the pipe
shown in Table 9 simultaneously to the pipe through two
wall. Calculate the pipe stiffness at 5 % deflection.
saddles located at the third points of the pipe (see Fig. 2). The
8.4.3 For production testing, test only one specimen to
loads shall be maintained for not less than 10 min with no
determine the pipe stiffness.
evidence of failure. The testing apparatus shall be designed to
8.4.4 The maximum specimen length shall be 12 in. (305
minimize stress concentrations at the loading points.
mm), or the length necessary to include stiffening ribs, if they
are used, whichever is greater. 8.6.2 Longitudinal Tensile Strength—Determine in accor-
dance with Test Method D638, except the provision for
NOTE 14—As an alternative to determining the pipe stiffness using the maximum thickness shall not apply.
apparatus and procedure of Test Method D2412 the supplier may submit
to the purchaser for approval a test method and test evaluation on Test
8.6.3 Longitudinal Compressive Strength—Determine in ac-
Method D790, accounting for the substitution of curved test specimens cordance with Test Method D695.
and measurement of stiffness at 5 % deflection.
8.5 Hoop-Tensile Strength—Determine the hoop-tensile 9. Packaging and Package Marking
strength by Test Method D2290, except that the sections on 9.1 Mark each length of pipe that meets or is part of a lot
Apparatus and Test Specimens may be modified to suit the size that meets the requirements of this specification at least once in
of specimens to be tested, and the maximum load rate may not letters not less than 1⁄2 in. (12 mm) in height and of bold-type
exceed 0.10 in/min. Alternatively, Test Method D638 may be style in a color and type that remains legible under normal
employed. Specimen width may be increased for pipe wall handling and installation procedures. The marking shall in-
thicknesses greater than 0.55 in. (14 mm). Means may be clude the nominal pipe size, manufacturer’s name or
provided to minimize the bending moment imposed during the trademark, this ASTM specification number: D3517, type,
test. Cut three specimens from the test sample. Record the load liner, grade, class, and stiffness in accordance with the desig-
to fail each specimen and determine the specimen width as nation code in 4.2.
close to the break as possible. Use the measured width and
failure load to calculate the hoop-tensile strength. 9.2 Prepare pipe for commercial shipment in such a way as
8.5.1 Alternative Minimum Hoop-Tensile Strength to ensure acceptance by common or other carriers.
Requirement—As an alternative, the minimum hoop-tensile 9.3 All packing, packaging, and marking provisions of
strength values may be determined as follows: Practice D3892 shall apply to this specification.
F 5 ~ S i /S r !~ Pr! (2)
10. Keywords
where:
10.1 fiberglass pipe; hydrostatic design basis; pressure pipe;
F = required minimum hoop tensile strength, lbf/in., RPMP; RTRP

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D3517 − 19
ANNEX

(Mandatory Information)

A1. ALTERNATIVE HYDROSTATIC DESIGN METHOD

A1.1 The following symbols are used: P 1 5 2 ~ t h sinθ !~ HDB! /D


The pipe is categorized in accordance with Table A1.1.
NOTE A1.2—The calculated result P1 may be multiplied by the factor
S = tensile stress in the glass fiber reinforcement in the 6.895 to convert from psig to kPa.
hoop orientation corrected for the helix angle,
psi, A1.6 Pressure Class Rating—The classes shown in Table
P = internal pressure, psig, A1.1 are based on the intended working pressure in psig for
P1 = long-term hydrostatic pressure, psig, commonly encountered conditions of water service. The pur-
D = nominal inside pipe diameter, in., chaser should determine the class of pipe most suitable to the
th = actual cross-sectional area of glass-fiber reinforce- installation and operating conditions that will exist on the
ment applied around the circumference of the pipe, project on which the pipe is to be used by multiplying the
in.2/in., values of P1 from Table A1.1 by a service (design) factor
θ = plane angle between hoop-oriented reinforcement selected for the application on the basis of two general groups
and longitudinal axis of the pipe (helix angle), of conditions. The first group considers the manufacturing and
and testing variables, specifically normal variations in the material,
HDB = hydrostatic-design basis, psi. manufacture, dimensions, good handling techniques, and in the
evaluation procedures in this method. The second group
A1.2 The hydrostatic design is based on the estimated
considers the application or use, specifically installation,
tensile stress of the reinforcement in the wall of the pipe in the
environment, temperature, hazard involved, life expectancy
circumferential (hoop) orientation that will cause failure after
desired, and the degree of reliability selected.
50 years of continuously applied pressure as described in
NOTE A1.3—It is not the intent of this standard to give service (design)
Procedure B of Practice D2992. Strength requirements are
factors. The service (design) factor should be selected by the design
calculated using the strength of hoop-oriented glass reinforce- engineer after evaluating fully the service conditions and the engineering
ment only, corrected for the helix angle of the fibers. properties of the specific plastic pipe material under consideration.
Recommended service (design) factors will not be developed or issued by
A1.3 Hoop-Stress Calculation is derived from the ISO ASTM.
equation for hoop stress, as follows:
S 5 PD/2 ~ t h sinθ !
This stress is used as the ordinate (long-term strength) in
calculating the regression line and lower confidence limit in TABLE A1.1 Long-Term Hydrostatic Pressure Categories
accordance with Annexes A1 and A3 of Practice D2992. Minimum Calculated Values of
Class Long-Term Hydrostatic
NOTE A1.1—The calculated result for S may be multiplied by the factor
Pressure gage, psi (kPa)
6.895 to convert from psi to kPa.
C50 90 (621)
A1.4 Hydrostatic-Design Basis—The value of S is deter- C100 180 (1241)
C150 270 (1862)
mined by extrapolation of the regression line to or 50 years in C200 360 (2482)
accordance with Practice D2992. C250 450 (3103)
C300 540 (3722)
A1.5 Hydrostatic-Design Basis Categories—Convert the C350 630 (4343)
C400 720 (4963)
value of the HDB to internal hydrostatic pressure in psig as C450 810 (5584)
follows:

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D3517 − 19
APPENDIXES

(Nonmandatory Information)

X1. INSTALLATION

X1.1 These specifications are material performance and and backfill, pipe characteristics, and care in the field construc-
purchase specifications only and do not include requirements tion work. The purchaser of the fiberglass pressure pipe
for engineering design, pressure surges, bedding, backfill or the specified herein is cautioned that he must properly correlate the
relationship between earth cover load, and the strength of the field requirements with the pipe requirements and provide
pipe. However, experience has shown that successful perfor- adequate inspection at the job site.
mance of this product depends upon the proper type of bedding

X2. RECOMMENDED METHODS FOR DETERMINING GLASS CONTENT

X2.1 Determine glass content as follows: X2.1.2 As a process control, by weight of the glass fiber
X2.1.1 By ignition loss analysis in accordance with Test reinforcement applied by machine into the pipe structure.
Method D2584 or ISO 1172.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D3517 – 14) that may impact the use of this standard. (August 1, 2019)

(1) Added 6.5.3 and Note 11. (2) Revised 7.2.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3567 − 17

Standard Practice for


Determining Dimensions of “Fiberglass” (Glass-Fiber-
Reinforced Thermosetting Resin) Pipe and Fittings1
This standard is issued under the fixed designation D3567; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* Intensity Instrument (Withdrawn 2008)3


1.1 This practice covers the determination of outside 2.2 ANSI Standard:
diameter, inside diameter, total wall thickness, reinforced wall B 2.1 Pipe Threads (Except Dryseal)4
thickness, liner thickness (where applicable), and length di- 2.3 API Standard:
mensions of “fiberglass” (glass-fiber-reinforced thermosetting API 5B Threading, Gaging, and Thread Inspection of
resin) pipe. Included are procedures for measuring tapered Casing, Tubing, and Line Pipe Threads5
dimensions and taper angles for pipe intended to be joined by
tapered socket fittings, and procedures for gaging internal and 3. Terminology
external threads. 3.1 Definitions of Terms Specific to This Standard:
1.2 This practice also includes procedures for determining 3.1.1 deviation from straightness—the maximum deviation
dimensions for fiberglass pipe fittings. from a straight line exhibited by a pipe specimen divided by the
length of the specimen.
1.3 The values stated in inch-pound units are to be regarded
as the standard. The SI units given in parentheses are for 3.1.2 fiberglass pipe—a tubular product containing glass-
information only. fiber reinforcements embedded in or surrounded by cured
thermosetting resin; the composite structure may contain
NOTE 1—There is no known ISO equivalent to this standard. aggregate, granular, or platelet fillers, thixotropic agents,
1.4 This standard does not purport to address all of the pigments, or dyes; thermoplastic or thermosetting liners or
safety concerns, if any, associated with its use. It is the coatings may be included.
responsibility of the user of this standard to establish appro- 3.1.3 laying length of fittings—the actual increase in the
priate safety, health, and environmental practices and deter- length of a line afforded by the fitting when installed.
mine the applicability of regulatory limitations prior to use. 3.1.4 liner and exterior surface layer thicknesses—the inner
1.5 This international standard was developed in accor- and outer portions of the wall used to enhance chemical and
dance with internationally recognized principles on standard- water resistance; they may have a different composition than
ization established in the Decision on Principles for the the reinforced wall and the thicknesses of these internal and
Development of International Standards, Guides and Recom- external surfaces may be measured when their boundary limits
mendations issued by the World Trade Organization Technical are visually indentifiable and if they are each at least 0.005 in.
Barriers to Trade (TBT) Committee. (0.10 mm) in thickness.
2. Referenced Documents 3.1.5 reinforced thermosetting resin pipe (RTRP)—a fiber-
glass pipe without aggregate.
2.1 ASTM Standards:2 3.1.6 reinforced wall thickness—the total wall thickness
D4166 Test Method for Measurement of Thickness of Non- minus the liner or exterior surface layer thickness, or both.
magnetic Materials by Means of a Digital Magnetic
4. Significance and Use
1
4.1 This practice provides for determining the physical
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and
is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic Piping dimensions of fiberglass pipe and fittings. This practice is
Systems and Chemical Equipment.
Current edition approved Sept. 1, 2017. Published September 2017. Originally
3
approved in 1977. Last previous edition approved in 2011 as D3567 – 97(2011). The last approved version of this historical standard is referenced on
DOI: 10.1520/D3567-17. www.astm.org.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 4th Floor, New York, NY 10036, http://www.ansi.org.
5
Standards volume information, refer to the standard’s Document Summary page on Available from American Petroleum Institute (API), 1220 L. St., NW,
the ASTM website. Washington, DC 20005-4070, http://api-ec.api.org.

*A Summary of Changes section appears at the end of this standard


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D3567 − 17
suitable for determination of dimensional compliance with surface. Remove burrs and sand the cut surface smooth, using
product specifications. 200-grit (or finer) sandpaper. Thoroughly wash the sanded
surface with clean water to remove resin and glass dust, then
5. Conditioning
blot dry.
5.1 Test conditions for measurements shall be in accordance 7.3.2 Reinforced Wall and Liner Thickness—Measure the
with appropriate product specification(s). cut surface of the pipe or fitting by setting a major scale
6. Total Wall Thickness—Pipe and Fittings division of the reticle at the apparent interface between the
liner and reinforced wall. Make 6 measurements 60° apart as
6.1 Apparatus—Calipers, optical comparators described in follows:
Section 7, ultrasonic thickness meters, or other gages such as 7.3.2.1 Read toward the outer surface of the pipe or fitting
the digital magnetic intensity instrument described by Test wall and observe the reinforced wall thickness.
Method D4166, with graduations of 0.01 in. (0.025 mm) or less 7.3.2.2 Read toward the inner surface of the pipe or fitting
that produces a thickness measuring accuracy of within 5 %, wall and observe the liner thickness.
may be used for measuring thicknesses of 0.20 in. (5.1 mm) or 7.3.3 Surface Layer Thickness—If the product specification
greater. For thicknesses less than the above, use a micrometer requires surface layer measurement, set a major scale division
or other gage with graduations of 0.001 in. (0.025 mm) and an at the apparent interface between the coating and the reinforced
accuracy of within 5 %. Use a cylindrical tubing micrometer or wall. Make 6 measurements 60° apart by reading toward the
spherical anvil micrometer with a radius end where the outer surface of the pipe or fitting and observing the surface
diameter of the pipe is small and a measuring error of 5 % or layer thickness.
less would be exceeded without its use.
7.3.4 Nonreinforced Layers, within the reinforced wall or
6.2 Procedure—Make a series of at least four readings at combination reinforcement layers. If the product involves
random selected locations, approximately equally spaced unreinforced layers or multiple reinforcement layers of differ-
around the circumference. The location of the measurements ent types, the amount and type of measurements shall be
should be taken some distance in from the pipe ends if the end agreed upon between the buyer and the seller.
thickness would be expected to be greater than other regions of 7.3.4.1 The thickness of these layers shall be determined by
the pipe. setting a major scale division of the reticle at the apparent
NOTE 2—Take care to ensure that the measurements are not made at interface and reading toward the next apparent interface. Make
either a tapered or belled pipe end. 6 measurements 60° apart.
NOTE 3—Take care to avoid misalignment of the anvil with the
longitudinal axis of the specimen when using cylindrical anvil microm- 7.4 Calculations—Calculate the average reinforced wall
eters that may bridge specimen surface curvature or indentations and give thickness and liner thickness by averaging the values obtained.
falsely high readings.
7.5 Report—The report shall include the following:
6.3 Calculation—Calculate the average total wall thickness 7.5.1 Observed minimum and maximum reinforced wall
of the four or more thicknesses taken. thickness,
6.4 Report—The report shall include the following: 7.5.2 Calculated average reinforced wall thickness,
6.4.1 Observed minimum and maximum wall thickness, and 7.5.3 Observed minimum and maximum liner thickness,
6.4.2 Calculated average total wall thickness. 7.5.4 Calculated average liner thickness, and
7.5.5 Observations of exterior surface layer, nonreinforced
7. Reinforced Wall Thickness and Liner Thicknesses—
layers, or other reinforced layer measurements within the
Pipe and Fittings
reinforced wall when measured.
7.1 Sampling—When performed on finished pipe or fittings,
this procedure will usually destroy or damage the part. When 8. Average Outside Diameter Measurements
this procedure is to be used for quality control or sampling, it NOTE 4—The need for measurements and the location of the measure-
is intended for use on samples taken from the excess of the ments should be evaluated since the outside surface of the pipe may not
fabrication, such as the ends of pipe or fittings, or both. If the be smooth. Uneven surfaces or burrs will influence the accuracy of the
outside diameter measurements.
procedure requires destructively testing the pipe or fittings, the
requirements shall be agreed upon between the buyer and the 8.1 Apparatus—A circumferential vernier wrap tape shall be
seller. used to determine the average outside diameter. The tape
should be accurate to within 6 0.02 in. (6 0.4 mm) on the
7.2 Apparatus—An optical scale comparator with a 7 to
circumference measured.
10X magnification and having a reticle graduated as follows:
7.2.1 For products with liner measurements less than 0.050 8.2 Procedure—Individually measure and record the outside
in. (1.27 mm): 0.001-in. (0.025-mm) divisions or not more than diameter end-sealing surfaces or special OD control surfaces.
10 % of liner thickness, whichever is smaller. Make the OD measurements near each end and at three
7.2.2 For products with liner measurements 0.050 in. (1.27 intermediate locations. Take the OD measurement by placing
mm) or larger: 0.005-in. (0.13-mm) divisions or smaller. the circumferential wrap tape around the pipe, making sure it is
7.3 Procedure: at right angles to the pipe axis. Average all five readings.
7.3.1 Surface Preparation—At the desired cross section of 8.2.1 Calculate the diameter as follows:
the pipe or fitting, make a sawcut at right angles to the inside D 5 C OD/π (1)

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D3567 − 17
where: 11.1.1 Procedure—Scribe two circumferential marks on the
COD = average of the readings. taper as far apart as possible, but at least 1⁄4 in. (6 mm) from the
NOTE 5—For larger diameter piping, the weight of the piping may cause small end of the taper. Measure the exact distance between
significant distortion. Take care in measurement and evaluation of the these marks within 0.01 in. (0.25 mm). Using calipers, measure
significance of this measurement. If significant product distortion due to the actual outside diameter at each of the scribe marks. Make
weight occurs, the pipe may be measured when in the vertical position.
Alternatively, the diameter may be measured as a reference from the
four measurements 45° apart.
mandril from which the pipe was made as follows: 11.2 Calculations—Using the actual diameters at the points
d 5 ~ C M /π12 3 wall thickness! (2) measured and the distances between the points, calculate the
taper angle, a, as follows:
where:
CM = outside circumference of the mandril, in. (mm) and the wall Sin a 5 @ ~ D 2 2 D 1 ! /2 # /L (4)
thickness is as described in 6.3. The measurement intervals are as where:
described in 8.2.
D2 = large diameter observed,
8.3 Report—When outside diameter measurements are D1 = smaller diameter observed, and
appropriate, the report shall include the minimum, maximum, L = distance between the two diameters measured along the
and average outside diameter. tapers.
9. Out-of-Round Measurements 11.3 Report—The report shall include the following:
9.1 Apparatus—A caliper, micrometer, or similar instrument 11.3.1 Apparatus used,
capable of measuring the OD within 6 0.25 % of nominal shall 11.3.2 Average D1,
be used. 11.3.3 Average D2,
9.2 Procedure—Using a micrometer or vernier calipers, take 11.3.4 The value of L, and
a series of outside diameter measurements at intervals spaced 11.3.5 Taper angle as calculated in 11.2, in terms of degrees
as in 8.2. Determine the maximum and minimum diameter by to the nearest 0.1°.
three measurements 120° apart at each interval.
12. Length of Pipe
NOTE 6—For large diameter piping, the weight of the piping may cause
significant distortion. Take care in measurement and evaluation of the 12.1 Apparatus—A steel tape, with 1⁄16-in. (1-mm) or finer
significance of this measurement. If significant product distortion due to graduations.
weight occurs, the pipe may be measured when in the vertical position.
Alternatively, with the pipe in a horizontal position, measure the pipe 12.2 Procedure—Lay the pipe specimen on a flat surface
diameter both vertically and horizontally and then remeasured after and in a straight line. Observe the length within the nearest
rotating the pipe 45°. Calculate the difference between the horizontal and 1⁄16 in. (1 mm).
vertical measurements in each case. The difference will be the average
out-of-roundness. The measurement intervals are as described in 9.2. 12.3 Report—The report shall include the length of each
9.3 Calculations—Calculate out-of-roundness as follows: specimen measured.
9.3.1 Subtract the minimum outside diameter from the
average outside diameter and subtract the average outside 13. Laying Lengths of Fittings
diameter from the maximum. 13.1 Apparatus—Two good quality commercial steel scales
9.4 Report—The report shall include the following: calibrated in 1⁄16-in. (1-mm) increments.
9.4.1 The average plus tolerance (maximum outside diam- 13.2 Procedure:
eter − average outside diameter), and
9.4.2 The average negative tolerance (average outside di- NOTE 7—Because of the wide variety of fittings and joining types,
specific procedures to cover every possible case cannot be written. As a
ameter − minimum outside diameter). result, the following general techniques may have to be modified to
include a specific configuration or adapter.
10. Inside Diameter
10.1 Calculate the average inside diameter as follows: 13.2.1 Elbows and Branch Fittings:
13.2.1.1 Insert a steel scale into one opening of the fitting so
d 5 D 2 2t a (3) that the inner edge of the scale is along the centerline of the
where: pipe when it is joined to the fittings. Repeat this procedure in
d = average inside diameter, in., the other leg of the fitting until the end of the second scale
D = average outside diameter, in., as determined in Section touches the inner edge of the first scale. Record the reading on
8, and the second scale at the mouth of the fitting as overall length, A.
ta = average total wall thickness, in., as determined in Now subtract from this overall length the socket or makeup
Section 6. length, X, as measured, or as specified by the manufacturer.
The difference, L, is the laying length of the fitting. See Fig. 1.
11. Pipe Taper Angle Measurement 13.2.2 Straight-Line Fittings:
11.1 Apparatus—Vernier Calipers, accurate to withing 13.2.2.1 Measure the overall length of the fitting. Subtract
0.001 in. (0.025 mm). These may also be used by comparing from this the makeup lengths on both sides, as specified by the
actual differences in diameter at specific distances on the taper. manufacturer. The difference is the laying length of the fitting.

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D3567 − 17
14.3 Estimate the difference between the gaging face of the
ring gage and the face of the fitting (external threads) or the
difference between the notch of the plug gage and the end of
the thread (internal threads) to the nearest 1⁄8 turn, after
correction has been made for any variation in the gage from
basic dimensions.

15. Straightness
15.1 Apparatus—A plane horizontal surface, a drawn line or
FIG. 1 Measurement for Calculation of Laying Length
string, and a metal rule with 1⁄16-in. (1.6-mm) or finer calibra-
tion.
13.3 Report—The report shall include laying lengths of each 15.2 Procedure—Place the pipe section on the plane surface
specimen measured. and allow it to come to rest. At a distance of half the outside
diameter above the plane surface, stretch the drawn line or
14. Gaging Threads
string from one pipe end to the other and draw it taut while in
14.1 Measure threads using American National Standard contact with both ends. Holding the ruler horizontally, deter-
tapered pipe thread gages conforming to ANSI B2.1 or API mine the maximum distance between the pipe and the line.
EUE 8 round (API 5B) dimensions. In gaging external taper Pipe with a nonuniform curvature will not necessarily show the
threads, screw up the ring gage tight by hand on the external maximum reading at the center.
thread. In gaging internal taper threads, screw up the plug gage
tight by hand into the fitting. 15.3 Report—The report shall include the specimen length
and the maximum deviation from straightness.
14.2 Gaging Chamfered, Countersunk, or Recessed
Threads—When the internal thread is chamfered, countersunk,
16. Keywords
or recessed the notch should be flush with the bottom of the
chamfer, which shall be considered the intersection of the 16.1 diameter; dimensions; fiberglass; fittings; gaging
chamfer cone and the pitch cone of the thread. Usually this threads; liner thickness; out-of-round; pipe; straightness; taper
depth is equal to one-half thread from the face of the fitting. angle; wall thickness

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D3567–97(2011)) that may impact the use of this standard. (September 1, 2017)

(1) Removed reference to measuring equipment no longer


commercially available (Section 11).

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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Downloaded/printed by
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3678 − 19 An American National Standard

Standard Specification for


Rigid Poly(Vinyl Chloride) (PVC) Interior-Profile Extrusions1
This standard is issued under the fixed designation D3678; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This specification establishes requirements for the ma- 2.1 ASTM Standards:2
terial properties, including dimensional stability and extrusion D618 Practice for Conditioning Plastics for Testing
quality, of rigid, poly(vinyl chloride) (PVC) interior-profile D696 Test Method for Coefficient of Linear Thermal Expan-
extrusions. Methods for identifying interior-profile extrusions sion of Plastics Between −30°C and 30°C with a Vitreous
that comply with the requirements of this specification are Silica Dilatometer
provided. D883 Terminology Relating to Plastics
1.2 Use of rigid PVC recycled plastic is permitted in D1042 Test Method for Linear Dimensional Changes of
accordance with the requirements of Sections 6 and 7. Plastics Caused by Exposure to Heat and Moisture
D1600 Terminology for Abbreviated Terms Relating to Plas-
1.3 Rigid PVC compounds for interior building product tics
applications are covered in Specification D1784. D1784 Specification for Rigid Poly(Vinyl Chloride) (PVC)
1.4 Rigid PVC exterior profile extrusions for assembled Compounds and Chlorinated Poly(Vinyl Chloride)
windows and doors are covered in Specification D4726. (CPVC) Compounds
1.5 The text of this standard references notes and footnotes D3892 Practice for Packaging/Packing of Plastics
which provide explanatory material. These notes and footnotes D4726 Specification for Rigid Poly(Vinyl Chloride) (PVC)
(excluding those in Tables and Figures) shall not be considered Exterior-Profile Extrusions Used for Assembled Windows
as requirements of this standard. and Doors
E631 Terminology of Building Constructions
1.6 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are given for 3. Terminology
information only. 3.1 General—Defintions are in accordance with Terminol-
NOTE 1—Information with regard to application should be obtained ogy D883 or Terminology E631 and abbreviations with Ter-
from the manufacturers of the profiles. minology D1600, unless otherwise indicated.
NOTE 2—There is no known ISO equivalent to this standard.
4. Significance and Use
1.7 The following precautionary caveat pertains only to the
test method portion, Section 8, of this specification: This 4.1 The purpose of this specification is to establish on a
standard does not purport to address all of the safety concerns, national basis, a recognized standard of quality for rigid
if any, associated with its use. It is the responsibility of the user poly(vinyl chloride) (PVC) interior-profile extrusions for inte-
of this standard to establish appropriate safety, health, and rior use other than cellular products, piping, tubing, and
environmental practices and determine the applicability of window and door profiles used in finished building products.
regulatory limitations prior to use. The information contained in this standard is intended to be
1.8 This international standard was developed in accor- helpful to producers, distributors, and users. It is also intended
dance with internationally recognized principles on standard- to serve as the basis for requirements on finished interior
ization established in the Decision on Principles for the building products which are either made from or employ rigid
Development of International Standards, Guides and Recom- PVC profile extrusions in their construction.
mendations issued by the World Trade Organization Technical 5. Classification
Barriers to Trade (TBT) Committee.
5.1 This standard covers three classes of rigid PVC interior-
1
profile extrusions as follows:
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.24 on Plastic Building
2
Products. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2019. Published January 2020. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1978. Last previous edition approved in 2014 as D3678 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D3678-19. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D3678 − 19
Class 1—Normal impact 2.2 %; those of 1.02-mm (0.040-in.) thickness or less shall
Class 2—Intermediate impact have a 3.0 % maximum shrinkage.
Class 3—High impact
8. Test Methods
6. Materials and Manufacture 8.1 General—Use the inspection and test procedures con-
6.1 This specification covers profile extrusions made from tained in this section to determine the conformance of products
plastics conforming to the requirements of Specification to the requirements of this specification. A producer or dis-
D1784, Table 1. Class 1 extrusions shall meet the requirements tributor representing products as conforming to this specifica-
for Class 12454 compound. Class 2 extrusions shall meet the tion shall utilize statistically based sampling plans that are
requirements for Class 14323 compound. Class 3 extrusions appropriate for each particular manufacturing process.
shall meet the requirements for Class 15223 compound. 8.2 Visual Inspection—Visually examine the interior-profile
6.2 Use of rigid PVC recycled plastic is permitted in this extrusions to determine their compliance with the requirements
product if all the requirements in the sections on Materials and of 6.5.
Manufacture (Section 6), and on Physical Requirements (Sec- 8.3 Conditioning of Specimens—Condition the test speci-
tion 7) are met by the extrusions containing PVC recycled mens in accordance with Procedure A of Practice D618, except
plastic. that the minimum conditioning time shall be 24 h.
6.3 All Class compounds shall have a minimum coefficient 8.4 Test Conditions—Conduct the tests at 23 6 1°C (73.4 6
of linear expansion of 10 × 10-5 cm ⁄cm ⁄°C (5.5 × 10- 1.8°F) and 50 6 10 % relative humidity, unless otherwise
5 in. ⁄in. ⁄°F).
specified in the applicable test method.
NOTE 3—Non-PVC materials may be used as a capstock. 8.5 Dimensional Stability—Determine the dimensional sta-
6.4 Rework Material—Clean, homogeneous PVC rework bility in accordance with Test Method D1042, except that the
material or rework material containing PVC capstock gener- test cycle shall consist of heating the specimens for 30 min in
ated from the manufacturer’s own production of the same class a uniformly heated oven at a temperature of 82.0 6 0.6°C (180
compound is permitted for use by the same manufacturer 6 1°F).
provided that the extruded profiles meet all the requirements of 8.6 Coeffıcient of Linear Expansion—Conduct this test in
this specification. Clean principally PVC rework material accordance with Test Method D696.
containing non-PVC capstock is permitted for use only in the
substrate of a capstocked product by the same manufacturer, 9. Product Marking
providing that the extruded profiles meet all of the require-
9.1 To aid identification of products conforming to all
ments of this specification.
requirements of this specification, producers and distributors
6.5 The PVC compound in extruded section shall maintain shall include a statement of compliance in conjunction with
visually uniform color and be free of any visual surface or their name and address on product labels, invoices, sales
structural changes, such as peeling, chipping, cracking, flaking, literature, and the like. The following statement is suggested:
or pitting. “Conforms to ASTM D3678 (name and address of producer
or distributors).”
7. Physical Requirements
7.1 Dimensions—The size, thickness, and dimensional tol- 10. Packaging
erances of the interior-profile extrusions shall be as agreed 10.1 All packing, packaging, and marking provisions of
upon between the supplier and purchaser. Practice D3892 shall apply to this specification.
7.2 Dimensional Stability—The dimensional stability of the
interior-profile extrusions shall be determined in the extrusion 11. Keywords
direction in accordance with 8.5. Extrusions over 1.02 mm 11.1 building products; extrusion; interior profile extru-
(0.040 in.) in thickness shall have a maximum shrinkage of sions; recycled plastic; rigid poly(vinyl chloride)

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D3678 − 19
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D3678 – 14) that may impact the use of this standard. (November 1, 2019)

(1) Section 2, remove reference to ASTM standards D2152, (8) Reword 8.4.
D4968 and D7209. (9) Delete 8.6.
(2) Reword 4.1. (10) Renumber 8.7 to 8.6.
(3) Reword 6.1, correct cell classification for Class 3 com- (11) Reword 9.1.
pounds. (12) Delete 9.2.
(4) Reword 6.2. (13) Delete 9.3.
(5) Reword 6.5, add ‘visual’ uniform color. (14) Reword 10.1 per ASTM D5740, 13.1.
(6) Delete 7.3, remove Acetone extrusion quality testing. (15) Summary of Change at end.
(7) Reword 8.1 to agree with wording in D4726.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

Copyright by ASTM Int'l (all rights reserved); Sat Jun 20 12:41:34 EDT 2020
3
Downloaded/printed by
Indian Inst of Tech Kharagpur (Indian Inst of Tech Kharagpur) pursuant to License Agreement. No further reproductions authorized.
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3679 − 17 An American National Standard

Standard Specification for


Rigid Poly(Vinyl Chloride) (PVC) Siding1
This standard is issued under the fixed designation D3679; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This specification establishes requirements and test 2.1 ASTM Standards:2
methods for the materials, dimensions, warp, shrinkage, impact D618 Practice for Conditioning Plastics for Testing
strength, expansion, appearance, and wind load resistance of D635 Test Method for Rate of Burning and/or Extent and
extruded single-wall siding manufactured from rigid (unplas- Time of Burning of Plastics in a Horizontal Position
ticized) PVC compound. Methods of indicating compliance D696 Test Method for Coefficient of Linear Thermal Expan-
with this specification are also provided. sion of Plastics Between −30°C and 30°C with a Vitreous
1.2 The use PVC recycled plastic in this product shall be in Silica Dilatometer
accordance with the requirements in Section 4. D883 Terminology Relating to Plastics
D1042 Test Method for Linear Dimensional Changes of
1.3 Rigid (unplasticized) PVC soffit is covered in Specifi- Plastics Caused by Exposure to Heat and Moisture
cation D4477. D1435 Practice for Outdoor Weathering of Plastics
1.4 Siding produced to this specification shall be installed in D1600 Terminology for Abbreviated Terms Relating to Plas-
accordance with Practice D4756. Reference shall also be made tics
to the manufacturer’s installation instructions for the specific D2244 Practice for Calculation of Color Tolerances and
product to be installed. Color Differences from Instrumentally Measured Color
Coordinates
NOTE 1—Information with regard to siding maintenance shall be
obtained from the manufacturer. D2457 Test Method for Specular Gloss of Plastic Films and
Solid Plastics
1.5 The values stated in inch-pound units are to be regarded
D3892 Practice for Packaging/Packing of Plastics
as standard. The values given in parentheses are mathematical
D4226 Test Methods for Impact Resistance of Rigid Poly-
conversions to SI units that are provided for information only
(Vinyl Chloride) (PVC) Building Products
and are not considered standard.
D4477 Specification for Rigid (Unplasticized) Poly(Vinyl
1.6 The following precautionary caveat pertains to the test Chloride) (PVC) Soffit
method portion only, Section 6, of this specification: This D4756 Practice for Installation of Rigid Poly(Vinyl Chlo-
standard does not purport to address all of the safety concerns, ride) (PVC) Siding and Soffit
if any, associated with its use. It is the responsibility of the user D5033 Guide for Development of ASTM Standards Relating
of this standard to establish appropriate safety and health to Recycling and Use of Recycled Plastics (Withdrawn
practices and determine the applicability of regulatory limita- 2007)3
tions prior to use. D5206 Test Method for Windload Resistance of Rigid Plas-
NOTE 2—There is no known ISO equivalent to this standard. tic Siding
1.7 This international standard was developed in accor- D5947 Test Methods for Physical Dimensions of Solid
dance with internationally recognized principles on standard- Plastics Specimens
ization established in the Decision on Principles for the E631 Terminology of Building Constructions
Development of International Standards, Guides and Recom- E1753 Practice for Use of Qualitative Chemical Spot Test
mendations issued by the World Trade Organization Technical Kits for Detection of Lead in Dry Paint Films
Barriers to Trade (TBT) Committee. G147 Practice for Conditioning and Handling of Nonmetal-
lic Materials for Natural and Artificial Weathering Tests

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.24 on Plastic Building contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Products. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2017. Published July 2017. Originally approved the ASTM website.
3
in 1979. Last previous edition approved in 2013 as D3679 – 13. DOI: 10.1520/ The last approved version of this historical standard is referenced on
D3679-17. www.astm.org.

*A Summary of Changes section appears at the end of this standard


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D3679 − 17
2.2 ASCE Standard: such that it is capable of resisting 100 % of positive and
ASCE 7-10 Minimum Design Loads for Buildings and negative wind pressures occurring under design conditions at
Other Structures4 the building location; and 2) with the standard fastening
2.3 International Code Council:5 method specified in building codes, general installation
International Building Code instructions, and the siding manufacturer’s instructions.
International Residential Code 3.2.6.2 alternative wind load design pressure rating—the
2.4 Vinyl Siding Institute, Inc.:6 wind load design pressure rating for a siding product when
VSI Vinyl Siding Installation Manual (2015) installed over a sheathing not designed and attached such that
2.5 Structural Building Components Association:7 it is capable of resisting 100 % of positive and negative wind
ANSI/SBCA FS 100-2012 Standard Requirements for Wind pressures occurring under design conditions at the building
Pressure Resistance of Foam Plastic Insulating Sheathing location, or when the siding is not fastened in the standard way;
Used in Exterior Wall Covering Assemblies as specified by the manufacturer.
3.2.6.3 Discussion—The standard test conditions,
3. Terminology
configuration, and fastening method used in this Specification
3.1 Definitions are in accordance with Terminologies D883, are specified in 6.14, while alternative sheathing and installa-
E631, and D1600, unless otherwise specified. tion conditions are specified by the manufacturer and must be
3.2 Definitions of Terms Specific to This Standard: reflected in the product’s installation instructions. Alternative
3.2.1 center-pinning—an installation technique in which the ratings apply only when the specified sheathing and fastening
siding panel is fastened tightly through the nail slot at the conditions are used. See Annex A1 for information on differ-
center length of the panel, in order to cause thermal expansion ences between the standard wind load design pressure rating
and contraction to occur equally in both directions from the and alternative wind load design pressure ratings, and how to
center. determine standard and alternative design pressure ratings.
3.2.2 heavily textured siding—in this standard, any vinyl 3.2.7 vinyl siding—a shaped material, made principally
siding using separate postextrusion processing to produce a from rigid poly(vinyl chloride) (PVC), that is used to clad
textured surface. exterior walls of buildings.
3.2.2.1 Discussion—Post-extrusion-forming does not in- 3.2.7.1 Discussion—Any exception to a homogeneous rigid
clude embossing of the surface or forming of the faces of the PVC compound is present in a coextruded or laminated
profile, but does include such processes as heat forming, capstock.
vacuum forming and compression molding applied to the 4. Materials and Manufacture
surface after the profile is extruded.
4.1 The siding shall be made of one or more layers of
3.2.3 nominal—the value that a manufacturer consistently poly(vinyl chloride) (PVC) compound. Any layers of materials
uses to represent a specific property or dimension of a vinyl other than poly (vinyl chloride) (PVC) compound shall be kept
siding product in public claims including, but not limited to, to less than 20 % by volume.
product literature, advertisements, quotations, and certificates
4.2 Where rigid PVC recycled plastic as defined in Guide
of conformance.
D5033 is used, the siding containing the PVC recycled plastic
3.2.4 process average thickness—the rolling, arithmetic shall meet all of the requirements of Section 3, Terminology;
mean of average specimen thicknesses measured according to Section 4, Materials and Manufacture; and Section 5, Physical
6.5 for a specific product during all productions runs for the Requirements.
most recent six month period.
4.3 The poly(vinyl chloride) siding material, when tested in
3.2.5 temperate northern climate—in weather testing, a accordance with Test Method D635, shall not exceed an
North American metropolitan area testing site located within average extent of burn of 4 in. (100 mm), with an average time
73 to 100°W longitude and 37 to 45°N latitude. of burn not to exceed 10 s. A minimum sample thickness of
3.2.6 wind load design pressure rating—the maximum wind 0.035 in. (0.9 mm) is required. (Warning—The flammability
pressure that a vinyl siding product is rated to withstand, based testing data, conclusions, and recommendations of Test
on testing under Test Method D5206; there are two types of Method D635 related solely to the measurement and descrip-
wind load design pressure rating used in this standard: tion of properties for classification of the poly(vinyl chloride)
3.2.6.1 standard wind load design pressure rating—the siding material in response to flame under controlled laboratory
wind load design pressure rating for a siding product when conditions and shall not be used for the description or appraisal
installed 1) over a sheathing material designed and attached of the fire hazard of vinyl siding under actual fire conditions.)
4.4 The PVC compound when extruded into siding shall
4
maintain uniform color and be free of any visual surface or
Available from American Society of Civil Engineers (ASCE), 1801 Alexander
Bell Dr., Reston, VA 20191, http://www.asce.org.
structural changes, such as peeling, chipping, cracking, flaking,
5
Available from International Code Council (ICC), 500 New Jersey Ave., NW, or pitting.
6th Floor, Washington, DC 20001, http://www.iccsafe.org.
6
National Housing Center, 1201 15th Street NW, Suite 220, Washington, DC
4.5 The PVC compound shall be compounded so as to
20005, http://www.vinylsiding.org provide the heat stability and weather exposure stability
7
6300 Enterprise Lane, Madison, WI 53719, http://www.sbcindustry.com required for the siding market application.

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4.6 PVC siding shall not contain elemental lead (Pb) or upon between the purchaser and the manufacturer. The color
compounds of that material other than traces incidental to raw specified shall be uniform on the surface of the siding panels,
materials or the manufacturing process. This limitation applies except in the case of multicolored woodgrain panels.
to both PVC substrate and to any cap or film material. 5.9.1 Uniformity of Color—When tested in accordance with
Compliance with this requirement shall be demonstrated by 6.13, the total color change, ∆E, between a production speci-
one of the methods in 6.16 men and the appropriate reference specimen or agreed-upon
color coordinates shall not vary by more than 1.5, and the
5. Physical Requirements chromatic coordinates thereof shall not change by more than
5.1 Length and Width—The nominal length and width of the 6∆aH = 1.0 and 6∆bH = 1.0.
siding shall be as agreed upon between the purchaser and the 5.10 Weathering:
seller. The actual length shall not be less than 1⁄4 in. (6.4 mm) 5.10.1 The siding shall maintain a uniform color and be free
of the nominal length and the actual width shall be within 61⁄16 of any visual surface or structural changes such as peeling,
in. (1.6 mm) of the nominal width when measured in accor- chipping, cracking, flaking, and pitting when tested in accor-
dance with 6.3 and 6.4. dance with 6.10.
5.2 Thickness—Except for heavily textured siding, these NOTE 3—Weathering-conformance-testing requirements are to reflect
requirements pertain only to measurements of the portions of performance of a “typical” extrusion siding profile representing a specific
the siding that are exposed after installation of the panel, color of PVC compound and a specific extrusion technology. In no case is
measured in accordance with the procedure in 6.5. For heavily there an implied requirement for testing all the various shaped and sized
siding profiles produced in this color. The lengthy outdoor weatherability
textured siding, these requirements apply to the portion of the
testing for new products may be performed concurrently with market
siding selected for measurement in accordance with 6.5. The development and sales of siding to existing markets. Completion of
average thickness of each specimen shall be no less than 0.035 weatherability testing prior to marketing of the product is not required.
in. No individual measurement shall be thinner than 0.003 in. 5.11 Wind Load Resistance—The siding shall withstand a
below the nominal thickness. The process average thickness as minimum static test pressure and a standard wind load design
defined in 3.2.4 shall be no thinner than 0.001 in. below the pressure rating shall be determined.
nominal thickness.
5.11.1 Minimum Test Pressure—The siding panel(s) shall be
5.3 Camber—A full length of siding (typically 10 or 12 ft able to withstand a minimum static test pressure of 22.5
(3.05 or 3.61 m)) shall not have a camber greater than 1⁄8 in. lbf/ft2 (1077 Pa) when tested in accordance with 6.14. The
(3.2 mm) when measured in accordance with 6.6. average maximum sustained static test pressure determined in
5.4 Heat Shrinkage—The average heat shrinkage shall not 6.14 shall be equal to or greater than this value.
exceed 3.0 % when determined by the method described in 6.7. NOTE 4—The static test pressure of 22.5 lbf/ft2 (1077 Pa) was estab-
5.5 Impact Resistance—Siding shall have a minimum im- lished to withstand structural loading conditions that occur in wind
exposures of approximately 110 mph (177 km/h) (VASD) for mean roof
pact strength of 60 in.·lbf (6.78 J) when tested in accordance heights of 30 ft (9.1 m) and less in exposure category B, and corresponds
with 6.8. to 30.0 lbf/ft2 (1436 Pa) negative design pressure, to match the default
5.6 Coeffıcient of Linear Expansion—The siding shall have wind design conditions of Table 703.3(1) in the 2015 International
Residential Code.
a coefficient of linear expansion not greater than 4.5 by 10-5 NOTE 5—Refer to Annex A1 for an explanation as to how the negative
in./in./°F (8.1 by 10−5 mm/mm/°C) when tested in accordance design pressure was established, and for applications where effective
with 6.9. negative design pressure as specified in ASCE 7-10 is different from 30.00
lbf/ft2 (1436 Pa) (for example, wind-zone areas greater than 110 mph (177
5.7 Gloss—The gloss of smooth and embossed siding shall km/h) (VASD) (225 km/h (VULT)) or mean roof height above 30 ft (9.1 m),
be uniform across the exposed surface. The average of all or exposures other than exposure category B).
readings for a panel determined in 6.11.2.5 shall not differ from
5.11.1.1 The design-pressure values can be negative (suc-
the manufacturer’s specified gloss value more than the permit-
tion loads) or positive. The negative values are the largest in
ted variation in Table 1, and each individual reading shall not
magnitude and are the values used in this specification.
vary more than 10 points from the average. Gloss of smooth
and embossed siding shall be tested in accordance with 6.11. NOTE 6—In that the siding is being tested as a weather-resistant exterior
TABLE 1 product applied to an existing exterior structural wall, forces (negative)
working to pull the siding off the wall, fasteners, or disengage locks will
Manufacturer’s Specified Permitted difference
Gloss Value from
be the most important criteria for testing. Positive wind forces test the
Mfg. Spec. Gloss integrity of the total wall sections, and do not provide a measure of the
Value performance of the siding.
Less than or equal to 35 ±8
Greater than 35 ±10
5.11.2 Standard Wind Load Design Pressure Rating—The
standard wind load design pressure rating shall be determined
5.8 Surface Distortion—The siding shall be free of bulges, from the results of testing in accordance with 6.14, using the
waves, and ripples when tested to a minimum temperature of procedures described in A1.3.
120°F (49°C) in accordance with the procedure in 6.12. This
distortion is called “oil-canning.” NOTE 7—The standard design pressure rating is valid for applications
where the siding is installed over sheathing and its fastening that are
5.9 Color—The color of the siding shall be within the capable of independently resisting both positive and negative wind
defined color space parameters for the specific color agreed pressures occurring under design conditions at the building location. For

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D3679 − 17
applications over other sheathing, a different design pressure rating is 6.3 Length—Lay the specimen on a flat surface and measure
applicable, and is determined in accordance with A1.3. Determination of with a steel tape. Measure the length of a siding panel to the
a rating other than the standard design pressure rating is not required by
this section.
nearest 1⁄16 in. (1.6 mm) at the center, the butt edge, and the
bottom of the top lock. The average of the three measurements
5.11.3 Alternative Design Pressure Ratings—Design pres- is the actual length.
sure ratings other than the standard wind load design pressure
rating, for use with different sheathing materials or using 6.4 Width—Interlock two specimens, each at least 26 in.
different installation or fastening, are permitted to be deter- (660 mm) long, in the normal mode for installation. Lay the
mined in accordance with testing under 6.14, using the two specimens on a flat surface. Measure to the nearest 1⁄16 in.
procedures in Annex A1. (1.6 mm), the distance between the lowest butt edge of the top
specimen and the lowest butt edge of the bottom specimen.
5.12 Nail Slot Allowance for Thermal Expansion—For sid- Commencing approximately one in. (25 mm) from one end of
ing panels utilizing nail slots to allow for thermal expansion the specimens, make 5 measurements at 6-in. (152-mm)
and contraction, the nail slot shall be sized to allow for the intervals, making sure that the measurement is made perpen-
expected range of expansion and contraction over a range of dicular to the butt edge. Average the measurements. The
100°F. Compliance with this requirement shall be demon- average constitutes the exposed width of siding.
strated either by the test method in 6.15 or by sizing of the nail
slots according to the specifications in the following sections. 6.5 Thickness—Thickness shall be measured in accordance
The instrument used shall be capable of measuring to the with Test Method A of Test Method D5947. The micrometer
nearest 0.01 in. The manufacturing tolerance shall not exceed shall be calibrated in accordance with Section 8 of Test Method
-0.030 inch. D5947. All measurements shall be taken to the nearest 0.001
5.12.1 For panels shorter than 6 ft (1829 mm) in length, the inch. Calculate and report the average of these measurements.
minimum nail slot width shall be 3⁄8 in. (11.4 mm). Also report the thinnest individual measurement.
6.5.1 Non-Heavily Textured Siding—The thickness of the
5.12.2 For panels 6 ft (1829 mm) in length or longer the
siding shall be measured at a minimum of five locations
minimum nail slot width shall be determined according to the
equally spaced across the entire portion of the siding that will
following formula. The minimum width shall be the width
be exposed after installation.
resulting from application of the formula, rounded to the next
lower quarter-inch. Regardless of the results of the calculation, 6.5.2 Heavily Textured Siding—The thickness of the siding
the minimum nail slot width for panels 6 feet or longer shall be shall be measured at a minimum of five locations on a flat
1 in. (25.4 mm). surface such as an end tab or other surface that is representative
of the extruded thickness. More than one panel shall be used as
WS 5 P c 3 ~ α 3 100 °F 3 L ! 1T c (1) necessary to provide a random selection of measurement
where: locations.
WS = Minimum width of nail slot, in. 6.6 Camber—Place a full length of siding (typically 10 or
Pc = Center-pinning coefficient: 1 if manufacturer’s in- 12 ft (3.05 or 3.61 m)) on a flat surface alongside a straightedge
structions require panel to be center-pinned; 1.5 if at least as long as the siding specimen. Measure the maximum
center-pinning is not required space between edge of the siding specimen and the straight-
α = Coefficient of linear thermal expansion, 4.5 × 10-5 edge for each edge to the nearest 1⁄16 in. (1.6 mm).
in./in./°F or actual known coefficient for material
6.7 Heat Shrinkage:
used, as determined by 6.9
L = Length of panel, inches 6.7.1 Apparatus:
Tc = Centering tolerance: 0.25 in. 6.7.1.1 Scriber, similar to that described in Test Method
D1042, with the exception that the needle points shall be
6. Test Methods separated by 10 6 0.01 in. (254 6 0.254 mm).
6.7.1.2 Test Media, a controlled-temperature water bath of 5
6.1 General—The inspection and test procedures contained gal (10 L) or more, equipped with an efficient stirrer that will
in this section are used to determine the conformance of maintain uniform temperature throughout. Heater and
products to the requirements of this specification. Each pro- temperature-control devices must maintain the water at 160 6
ducer who represents its products as conforming to this 1°F (71 6 0.5°C). Use a wire rack to raise and lower
specification shall be permitted to use statistically based specimens into the water bath. As an alternative to the use of a
sampling plans that are appropriate for each manufacturing water bath, the specimens may be heated for 30 min in a
process, but shall keep the essential records necessary to uniformly heated forced-air oven maintained at a temperature
document, with a high degree of assurance, his claim that all of of 160 6 1°F (71 6 0.5°C).
the requirements of this specification have been met. Addi- 6.7.1.3 Make measurements with any device capable of
tional sampling and testing of the product, as agreed upon measuring the distance between two scribe marks to the nearest
between the purchaser and the manufacturer, are not precluded 0.01 in. (0.254 mm).
by this section. 6.7.2 Procedure:
6.2 Conditioning and Test Conditions—Condition the test 6.7.2.1 Scribing shall be done on either the front or back
specimen in accordance with Procedure A of Practice D618 and surface of the siding as necessary to provide a clean, recog-
test under those conditions, unless otherwise specified herein. nizable line.

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D3679 − 17
6.7.2.2 Cut three specimens from the siding panel, each 1 in. 6.10.4 Select a minimum of four specimens per sample per
(25.4 mm) wide by 12 in. (305 mm) long. Cut one specimen test site to allow for three test specimens and one file specimen
from the center and one from each of the extreme edges of the for each sample evaluated.
flat surface. The long axis shall be parallel to the machine 6.10.5 Mark each specimen permanently to ensure retention
direction. of identity during and after exposure testing.
6.7.2.3 Condition specimens at 73.4 6 3.6°F (23 6 2°C) NOTE 9—Use of a vibratool leaves a permanent mark that satisfies this
and 50 6 10 % relative humidity for at least 24 hours. criterion.
6.7.2.4 Make a slight mark with the scribe on each specimen
6.10.6 All exposures shall be conducted at an angle of 45°
so that a reference point will be clearly visible.
South, plywood backed, in accordance with Practices D1435
6.7.2.5 Place specimens in the test medium.
and G147.
6.7.2.6 Remove specimens after 30 min and place on a flat 6.10.7 After a minimum of 24 months of exposure, remove
surface until cool. the samples and inspect each exposed test specimen for
6.7.2.7 Repeat conditioning in accordance with 6.7.2.3. appearance and surface condition. Record observations and
6.7.2.8 Make a second mark with the scribe on each inspection date in a permanent record.
specimen, using the same center.
6.7.2.9 Measure the distance, D, between the scribe marks 6.11 Gloss:
to the nearest 0.01 in. (0.254 mm). 6.11.1 Apparatus—Measure gloss using a 75° geometry
6.7.2.10 Calculate the percent shrinkage as (D/10) × 100. glossmeter that meets the requirements of the Apparatus
section of D2457.
6.7.2.11 Report the average shrinkage of the three speci-
6.11.2 Procedure:
mens tested.
6.11.2.1 Gloss measurements shall be made in accordance
6.8 Impact Resistance—Test impact resistance of siding in with the procedure in Section 9 of D2457, unless otherwise
accordance with Test Method D4226, Procedure A, impactor specified herein.
head configuration H.25. 4 in.-lb increments (0.5 in. height 6.11.2.2 Measure gloss on one piece of siding on at least
increments with 8 lb falling weight) shall be used. Minimum three widely separated sections across the width of the exposed
sample dimensions shall be 1.5 by 1.5 in. Samples shall be surface of the panel. At least one reading shall be taken on each
tested with the normally exposed surface facing up. Condition- face of the panel. Care needs to be taken to ensure that a new
ing time for quality-control tests shall be at least 1 hour. surface area is used for each reading since instrument contact
6.8.1 For purposes of evaluating failure of the specimen may leave scratches on the specimen surface. The area tested
under 3.2.1 of Test Method D4226, a ductile tear of less than must be flat. If a flat area on the exposed surface cannot be
0.2 in. (5 mm) in length shall not be considered a failure. Any found due to the style or depth of embossing of the panel being
brittle break of any dimensions is considered a failure. tested, then a non-exposed area of the panel shall be chosen in
6.9 Coeffıcient of Linear Expansion—Conduct this test in its place. Such locations shall be representative of the gloss of
accordance with Test Method D696. the area that will be exposed after installation.
6.9.1 Alternative Specimen Preparation—Specimens pre- 6.11.2.3 Measure gloss parallel to the direction of emboss-
pared from strips cut from extruded siding are permitted to be ing. When the embossing pattern is not apparent, measure the
used in testing under Test Method D696. Where such speci- gloss in the direction of extrusion.
mens are used, they shall be cut with the long dimension 6.11.2.4 Each reading shall be within the appropriate limit
parallel to the long axis of the siding panel. Guides shall be specified in 5.7.
used in accordance with Test Method D696 to prevent bending 6.11.2.5 The average of all readings shall be used to
or twisting of the specimen in the dilatometer. represent the gloss of the sample.
6.10 Weatherability: 6.12 Surface Distortion:
6.10.1 A minimum of three samples shall be exposed at each 6.12.1 Test Specimen/Apparatus:
of at least three test sites. Test sites shall be located in a 6.12.1.1 The test specimen shall consist of three courses of
northern temperate climate, represented by Cleveland, Ohio or siding, a minimum of 6 ft (1.83 m) in length, mounted on a flat
Louisville, Kentucky; a hot, humid climate represented by rigid frame in accordance with the manufacturer’s recom-
Miami, Florida; and a hot, dry climate represented by Phoenix, mended installation instructions.
Arizona. The samples shall be exposed for a minimum of 24 6.12.1.2 Heat-sensing elements shall be located at the mid-
months. point of the backside of the second course of siding.
6.10.2 Samples shall consist of a flat section of siding with 6.12.1.3 Radiant-Heat Rod, 600 W for each linear foot (0.31
minimum dimensions of 2 in. by 3 3⁄4 in. (25 mm by 95 mm). m), mounted parallel to the middle course and approximately
6.10.3 Samples shall be representative of the product to be 32 in. (810 mm) away from the surface of the siding.
evaluated. 6.12.1.4 Temperature-Control Device, used to regulate the
temperature of the radiant-heat rod, shall be able to maintain
NOTE 8—Samples prepared in the laboratory in the same manner as the conditions specified in 6.12.2.1.
commercial samples are permitted to be used as an alternative to a
commercial part. If the commercial product is extruded, the laboratory
6.12.2 Procedure:
specimen must be extruded; if the commercial product is injection 6.12.2.1 Heat the test panel (second course of siding) at a
molded, the laboratory specimen must be injection molded, and so forth. rate of 3.0 to 6.0°F/min (1.7 to 3.3°C/min) until a minimum

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D3679 − 17
temperature of 120°F (49°C) is achieved as measured by the maintained for at least 15 minutes. Means for circulating air to
heat-sensing element on the midpoint of the backside of the provide a uniform air temperature throughout the chamber
second course. During this heating period, observe the test shall be provided. A vertical wall shall be provided for
panel for surface distortion. mounting of samples. The wall shall be insulated such that,
6.12.2.2 Failure is defined as the appearance of bulges, with no panels mounted, the inner surface of the wall does not
waves, or ripples before a temperature of 120°F (49°C) is deviate more than 10°F (5.5°C) from the air temperature at the
reached. high and low temperature extremes after a holding period of 5
minutes. The test chamber shall be of sufficient size to
6.13 Color Uniformity—Calculate the difference between
accommodate the longest panel to be tested, including ex-
the LH, aH, and bH color coordinates for a production specimen
pected thermal expansion of the panel. Means shall be pro-
to those of either the appropriate reference specimen or the
vided to measure the actual temperature of the surface of each
agreed upon color coordinates for that specific color product in
panel at a minimum of three evenly-spaced locations along the
accordance with Test Method D2244. Calculate the total
length of the panel.
difference ∆E between the production specimen and the
reference specimen in accordance with Test Method D2244. 6.15.3 Length Measurement—A means for measuring the
length of each sample throughout the temperature range shall
6.14 Wind Load Resistance—Conduct the test on wind load be provided. The method utilized for length measurement shall
resistance of finished siding in accordance with Test Method not be influenced by the temperature of the chamber and shall
D5206. The average maximum sustained static test pressure have a minimum resolution of no greater than 0.0625 in. (1.59
determined from this testing is used in 5.11. For purposes of mm).
determining compliance with the minimum test pressure and 6.15.4 Procedure—Install the sample panels on the wall
standard design pressure requirements in 5.11, the test structure inside the test chamber, following the manufacturer’s instruc-
shall be constructed with vertical studs 16 inches on center, the tions for fastener type, spacing, location and tightness. At
siding in the test installation shall be installed over wood ambient temperature measure and record the length of each
sheathing with a nominal thickness of 7⁄16 to 1⁄2 inch, and panel and the temperature of the panel, averaged from a
fastened as follows: minimum of three locations along the length of the panel.
6.14.1 Fastener Type—Roofing nail, smooth shank, 0.120
6.15.4.1 Test Cycle—Test cycles shall be performed by
in. (1⁄8 in. nominal; 3.2 mm) shank diameter, 5⁄16 in. (7.9 mm)
raising the air temperature to 100°F 6 5°F (38°C 6 2.75°C) at
head diameter, length as necessary to penetrate into sheathing
an average rate of 2°F (1.11°C) per minute, holding the air
and stud a total of 1 1⁄4 in. (32 mm). For vertical siding, length
temperature at 100°F (38°C 6 2.75°C) for 15 minutes,
as necessary to penetrate the thickness of the sheathing plus 1⁄4
lowering the air temperature to 0°F 6 5°F (-18°C 6 2.75°C) at
in. (6.4 mm).
an average rate of 2°F (1.11°C) per minute, holding at 0°F
6.14.2 Fastener Spacing—Every 16 in. (406 mm) into (-18°C 6 2.75°C) for 15 minutes, and returning to ambient
center of stud for horizontal siding. For vertical siding, every temperature at an average rate of 2°F per minute.
12 inches into sheathing only.
6.15.4.2 Conditioning—Close the test chamber and perform
6.14.3 Fasteners shall not be driven tightly against the
at least two conditioning cycles using the procedure in
siding. Allow approximately 1⁄32 in. (0.8 mm) clearance be-
6.15.4.1. No interruption is required between conditioning
tween the fastener head and siding surface.
cycles.
NOTE 10—The installation details described in 6.14 conform to the 6.15.4.3 Test—Following completion of the conditioning
minimum requirements of the 2015 International Residential Code and the cycles, conduct three test cycles using the procedure in
VSI Vinyl Siding Installation Manual.
6.15.4.1. It is acceptable for the test cycles to follow immedi-
6.15 Nail Slot Allowance for Thermal Expansion—As an ately upon completion of the final conditioning cycle, and no
alternative to conformance with the nail slot width specifica- interruption is required between test cycles. After a minimum
tion in 5.12.1 or 5.12.2, provision for thermal expansion and holding period of 15 minutes at the high and low extremes of
contraction shall be demonstrated through the following test each test cycle, measure and record the length of each panel
procedure. and the temperature of the panel, averaged from a minimum of
6.15.1 Samples—At least three samples of each profile in three locations along the length of the panel.
which the siding is produced shall be provided. The length of 6.15.5 Normalization—From among the length measure-
each sample shall be at least 50 % of the longest length in ments recorded for all three cycles, identify the shortest and
which the profile is produced, and not shorter than 12 ft (3658 longest length of each panel, and the average panel temperature
mm). at the time that length was recorded. Determine the maximum
6.15.2 Test Chamber—The test chamber shall consist of an difference in length, ∆L, and the maximum difference in
environmentally controlled room or compartment capable of temperature, ∆T, by subtracting the smaller from the larger.
providing an air temperature range of at least 0°F to 100°F Normalize the change in length to the full length of the panel
(-18°C to 38°C) without exposure of the panel to radiant over a 100°F (38°C) temperature range using the following
energy from heating or cooling elements. Air temperature shall formula:
be controlled such that a rate of temperature change of 2°F
E t 5 ∆L x ~ 100/∆T ! x ~ L f /L t ! (2)
(1.11°C) per minute can be achieved over the full temperature
range, and the minimum and maximum temperatures can be where:

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D3679 − 17

Et = Total thermal expansion and contraction of a full and the like. The following statement is suggested when
length panel over a range of 100 °F (38 °C) sufficient space is available:
∆ L = Maximum change in length of the tested panel This PVC siding conforms to all the requirements estab-
∆T = Maximum change in temperature of the tested panel lished in ASTM Specification D3679, developed cooperatively
Lf = Longest length in which the panel is produced with the industry and published by ASTM.
Lt = Actual length of the panel as tested Full responsibility for the conformance of this product to the
6.15.6 Acceptable Performance—When tested in accor- specification is assumed by (name and address of producer or
dance with this procedure, the result of (Et × 2) + 0.25 in. for distributor).
each of the three samples for each profile shall not be greater 7.4 The following abbreviated statement is suggested when
than the width of the nail slot. If the manufacturer’s installation available space on labels is insufficient for the full statement:
instructions require the panel to be center-pinned, the result of Conforms to ASTM Specification D3679 (name and address
Et + 0.25 in. for each of the three samples for each profile shall of producer or distributor).
not be greater than the width of the nail slot. 7.5 The standard wind load design pressure rating deter-
6.16 Lead Content: mined in accordance with 5.11.2 shall be stated on the product
6.16.1 Testing for lead content shall be conducted on or on the product package by one of the means in 7.5.1 or 7.5.2.
extruded siding using a rhodizinate-type lead swab test kit 7.5.1 The package shall be marked or labeled with the
conforming to Practice E1753. Testing shall be performed in standard wind load design pressure rating. The marking shall
accordance with the test kit manufacturer’s instructions. The be in the format “Standard Wind Load Design Pressure Rating:
siding shall be deemed to comply with 4.6 if the test shows a ##.# psf (ASD)”.
negative or not-detected result; that is, the test does not indicate 7.5.2 The standard design pressure rating shall be included
the presence of lead. The test shall be conducted separately on on a line imprint or other marking on the front (outward-
the substrate and on any cap or film material. facing) surface of all siding panels. It is not required that the
6.16.2 As an alternative to the method in 6.16.1, and as a marking be visible after installation, provided that the marking
means of resolving any ambiguous results from that method, an can be revealed and read by detaching the lower edge lock of
analytical method capable of detecting lead at least as low as an adjacent course, without removal of any fasteners. The
0.02 percent by sample weight shall be employed. Under this standard design pressure marking shall be stated at least once
alternative, neither the substrate nor any cap or film shall per panel. The marking shall be in the format “Std Design
contain a concentration of lead in excess of 0.02 percent by Pressure Rating: ##.# psf (ASD)”.
weight. 7.5.3 At the option of the manufacturer, additional marking
or labeling of the package or product with alternative wind load
7. Packaging and Package Marking design pressure ratings determined in accordance with 5.11.3
7.1 The siding shall be packed in such a manner as to for use with alternative sheathings, wall configurations or
provide reasonable protection against damage in ordinary fastening methods is permitted. The marking shall use the
handling, transportation, and storage. format specified in 7.5, shall indicate the type of sheathing or
wall configuration for which it is applicable, and shall refer to
7.2 Provisions of Practice D3892 shall apply to this speci-
the manufacturer’s instructions for more information and any
fication.
installation requirements.
7.3 To aid identification of siding conforming to all require-
ments of this specification, producers and distributors shall 8. Keywords
include a statement of compliance in conjunction with their 8.1 plastic building products; plastic weatherability; re-
name and address on product labels, invoices, sales literature, cycled plastic; rigid PVC siding; specification

ANNEX

(Mandatory Information)

A1. WIND LOAD RESISTANCE TEST DESIGN FACTORS

A1.1 Wind Load Criteria: given location, produce a wind speed approximately 30 % greater than
that of the previous maps. This larger magnitude (higher return period)
A1.1.1 ASCE 7-10 is the basis for determining the design wind speed, referred to as the ultimate wind speed, (VULT), is used directly
pressures used in this specification. Design wind loads are (with a load factor of 1.0) to determine nominal wind loads on a Strength
determined on an ASD basis in this specification. Design (LRFD) or “ultimate” wind load basis. When Allowable Stress
Design (ASD) is used, ASCE 7-10 provides for these ultimate wind loads,
NOTE A1.1—In previous editions of ASCE 7, wind loads were deter- determined from the ultimate wind speed map velocities, to be multiplied
mined using wind speed maps based on a 50-year return period. In ASCE
by a load factor of 0.6. Alternatively, the adjustment can be made directly
7-10, maps based on a 700-year return period are used which, for any

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D3679 − 17
to the wind velocity, which is the approach taken in this method (see A1.1.5 ASCE 7-10 recommends various internal and exter-
A1.1.2). This procedure produces results consistent with past ASD wind nal pressure coefficients, which include gust response factors.
loads.
These coefficients vary with the effective area of the cladding
A1.1.2 It is necessary to determine whether the wind component, the location of the cladding component relative to
velocity to be used is based on the maps in ASCE 7-10 or on building corners, and the configuration of the building (open
older maps designed for direct application of ASD. Wind versus enclosed). The internal and external pressure coeffi-
velocity, V, based on ASD is used in this method. Wind speeds cients are taken from Table 26.11-1 and Figure 30.4-1 of ASCE
determined using the maps in ASCE 7-10, referred to as VULT, 7–10. The effective area is taken as 10 square ft (the area of one
are converted to ASD wind speeds, VASD, by multiplying by the piece of siding), an enclosed building is assumed, and factors
square root of 0.6. Wind speeds based on maps using an ASD for the building corners are used. The pressure coefficients are
basis do not require conversion (see A1.3) Thus: as follows:
Internal Pressure Coefficient 5 60.18
V 5 V ASD 5 V ULT 3 =0.6 (A1.1)
External Pressure Coefficient 5 11.00 and 2 1.40
The V determined in this section is used in the following
calculations: The design pressure is calculated by multiplying the velocity
pressures by the algebraic sum of the internal and external
A1.1.3 The velocity pressures, q, used in this specification pressure coefficients.
have been computed using the following equation:
A1.2 Design Pressure:
q 5 0.00256 K z K d V 2 I ~ lb/sq ft!
50.613 K z K d V 2 I ~ N/m 2 ! Positive Design Pressure 5 ~ 18.43!~ 1.0010.18! 5 21.74 psf

where: Negative Design Pressure 5 ~ 18.43!~ 21.40 2 0.18! 5 229.12 psf


NOTE A1.5—Because the wind velocity has already been adjusted from
V = wind velocity, mph (km/h). The basic wind speed an ultimate basis to an ASD basis at the beginning of these calculations,
corresponds to a 3-s gust speed at 33 ft (10.1 m) above the design pressure determined in this step is an ASD load. This correlates
ground in exposure category C, as described in ASCE to the design pressure requirements stated in tables in the 2015 Interna-
7-10. A velocity of V = VASD= 110 mph (177 km/h) was tional Residential Code and other codes which have also been adjusted to
used in this specification. (See Note A1.2 and Note an ASD basis. However, the required design pressures in some other codes
and design standards have not been adjusted to an ASD basis. Where
A1.3.) required design pressures are based on ultimate wind loads determined
I = “importance factor” as described in editions of ASCE 7 from ASCE 7-10 wind speeds, those loads must be multiplied by 0.60 to
prior to ASCE 7-10. A value of 1.0 is used. This factor match the design pressure determined from this equation.
is not used where the wind speed has been determined
A1.2.1 The negative values (suction loads) are the largest in
from a map in ASCE 7-10. (See Note A1.4.)
magnitude and are the design values used in this specification.
Kz = “velocity pressure coefficient” as described in ASCE
Research conducted by various organizations8,9 has shown that
7-10. A “Kz” of 0.70 is used in the wind pressure
a certain amount of pressure equalization occurs through
calculations, which is the value from ASCE 7-10 for a
residential siding products installed with sheathing under high
mean roof height of 30 ft (9.1 m) above ground level
dynamic pressures. In light of this pressure equalization, the
and Exposure Category B.
Kd = “wind directionality factor” as described in ASCE design pressure in the ASCE 7-10 wind load standards is
7-10. A “Kd” of 0.85 is used. reduced by a factor of 0.5.
A1.2.2 Therefore, the required test pressures are calculated
A1.1.4 The velocity pressure = -18.43 lbf/ft2 (882 Pa).
as follows:
NOTE A1.2—As explained in Note A1.1, the wind velocity used in this
P t 5 D P 3 PEF 3 1.5
method is converted from the VULT given by wind speed maps in ASCE
7-10 to VASD using the equation in A1.1.2. A VULT wind speed of where:
approximately 140 mph from the maps is equivalent to a VASD of 110 mph,
which is the velocity V used in this specification. Pt = test pressure, lbf/ft2 (Pa),
NOTE A1.3—In ASCE 7-10 the default wind speeds are given for DP = design pressure, lbf/ft2 (Pa),
exposure category C, and a table is provided to adjust this wind speed for PEF = pressure equalization factor, 0.5, and
other exposure categories. Since most vinyl siding is installed on buildings 1.5 = safety factor.
located in exposure category B, the velocity pressure coefficient, Kz is
included in the equation to make this adjustment. A1.2.2.1 If documentation in support of the use of compen-
NOTE A1.4—Editions of ASCE 7 prior to ASCE 7-10 included an sation for pressure equalization other than 0.5 is provided, use
importance factor to represent the relative significance of the building and the calculation in A1.2.2, substituting the appropriate pressure
the consequences of its loss. Because most vinyl siding is installed on equalization factor.
residential and light commercial buildings, the importance factor was set
at 1.0 by default. ASCE 7-10 has removed the importance factor from the
velocity pressure equation, and instead provides a different wind speed
map for each of the building importance categories (referred to as risk 8
Vinyl Siding Pressure Equalization Factor, Architectural Testing, Inc., Report
categories in ASCE 7-10). Thus, the importance factor will already have No. 01-40776.01, September, 2002.
been incorporated into the wind speed determined from the appropriate 9
Morrison, M.J., Cope, A.D., Wind Performance and Evaluation Methods of
map, and the importance factor is not used for determining velocity Multi-Layered Wall Assemblies, Structures Congress, 2735-2748, Portland, OR,
pressure using wind speeds from ASCE 7-10 maps. 2015.

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D3679 − 17
A1.2.3 Using the above equations, in a 110 mph (177 km/h) A1.2.6.2 If the adjusted PEF for a given combination of
(VASD) wind zone area specifying a design pressure of -29.12 siding and sheathing is known, and an appropriate safety factor
lbf/ft2 (1394 Pa) for a building 30 ft (9.1 m) in height or less, is used, a minimum test pressure can be determined using the
the required minimum siding uniform load test pressure is equation in A1.2.1. However, it is normally more appropriate
21.84 lb/ft2 (1047 Pa). to make an adjustment for alternative sheathings when deter-
A1.2.3.1 For compliance with 5.11, the referenced design mining the design pressure rating, as discussed in A1.3.
pressure has been rounded to -30.0 lbf/ft2 (1436 Pa) to match
the standard design conditions specified by the 2015 Interna- NOTE A1.7—Where the sheathing is not capable of independently
resisting both positive and negative wind pressures occurring under design
tional Residential Code. When tested under Test Method conditions at the building location, the layer of siding over the sheathing,
D5206, the siding must attain an average maximum sustained and its fastening through the sheathing, act to reinforce the sheathing such
static test pressure equal to or greater than the corresponding that the whole wall covering (siding-sheathing) assembly is capable of
minimum test pressure of 22.5 lb/ft2 (1077 Pa). resisting such wind pressures. Because vinyl siding is tested by itself (not
as part of a siding-sheathing assembly) in Test Method D5206, the
A1.2.4 For applications where the effective design pressure adjustment of test pressure (before the test) or of the design pressure (after
is greater than -30.0 lbf/ft2 (1436 Pa) (for example, wind zone the test) ensures that the wind load resistance of the assembly as a whole
areas greater than 110 mph (177 km/h) (VASD), mean roof is reflected in the rating of the siding.
height over 30 ft (9.1 m), or exposure conditions other than NOTE A1.8—In some high wind hazard regions, such as south Florida,
Exposure B), refer to ASCE 7-10 for the effective design the exterior wall covering assembly may also be required to meet
wind-borne debris impact resistance criteria which would affect the choice
pressure. To be shown to be suitable for the application, when of sheathing material to be used together with vinyl siding. Such
tested under Test Method D5206 the siding must attain an considerations are beyond the scope of this standard.
average maximum sustained static test pressure equal to or
greater than the minimum test pressure determined by the A1.3 Wind Design Pressure Rating (Maximum Allowable
formula in A1.2.2, using the design pressure, DP, determined Pressure):
for the application using the procedure in A1.1.2 through A1.2. A1.3.1 A design pressure rating is the maximum wind
A1.2.5 These loading conditions apply only to siding in- pressure that a particular vinyl siding product is rated to be able
stalled without an air space, directly over sheathing of a type to withstand. It is used in building design and building codes to
and fastening method that is capable of independently resisting determine the acceptability of a siding product for use under
both positive and negative wind design pressures at the the design wind conditions for a specific application. To be
building location. Examples of such sheathing include oriented acceptable, a siding’s design pressure rating must be equal to or
strand board (OSB) and plywood fastened to resist the design greater than the design pressure for the specific building at the
wind pressures. For applications where the siding is installed specific location. The design pressure rating is determined
over open studding, without sheathing, rapid pressure equal- from the average maximum sustained static test pressure for a
ization does not occur. In these applications, the load the siding siding product produced by testing under Test Method D5206,
will see is equal to the total design pressure, and the pressure the pressure equalization factor, and a safety factor.
equalization factor (PEF) is set to 1.0. The static test pressure
A1.3.2 Standard Design Pressure Rating—The standard
required for products used under these conditions is as follows:
design pressure rating is used for applications where the siding
P t 5 D P 3 PEF 3 1.5 is installed over a sheathing type and fastening method that is
where: capable of independently resisting both positive and negative
wind pressures occurring under design conditions at the
Pt = static test pressure, lbf/ft2 (Pa),
building location.
DP = design pressure, lbf/ft2 (Pa),
PEF = pressure equalization factor, 1.0, and A1.3.2.1 The standard design pressure rating assumes that
1.5 = safety factor. the siding is fastened to the building in the standard manner,
NOTE A1.6—Building codes and vinyl siding installation instructions with the minimum fastener type, size, spacing, and penetration
require vinyl siding to be installed over sheathing, so calculation of depth prescribed in Chapter 7 of the International Residential
minimum test pressure for siding installed without sheathing is essentially Code and the VSI Vinyl Siding Installation Manual. The
moot. However, the calculation has been retained for completeness and
comparison with other installation conditions.
installation of the siding for testing under Test Method D5206
must be consistent with these minimum fastening require-
A1.2.6 When siding is installed over sheathing that is not ments. However, this does not prevent additional testing, using
capable of independently resisting both positive and negative different fastening, to support design pressure ratings for other
wind pressures occurring under design conditions at the applications, such as special high wind installations.
building location, a greater percentage of the total wind
pressure is transferred to the siding and its fasteners. This has A1.3.2.2 The pressure equalization factor and safety factor
the effect of partially or completely countering the effect of the are the same as those used to determine the test pressure in
pressure equalization factor. In these cases a value between 0.5 A1.2.1, using the following equation:
and 1.0 is used for the pressure equalization factor (PEF). Pm
D Rstd 5 (A1.2)
A1.2.6.1 In addition, in cases where failure of the siding ~ PEF 3 SF!
would result in failure of the exterior wall covering assembly where:
(that is, siding and sheathing) a safety factor of greater than 1.5
DRstd = standard design pressure rating, lbf/ft2 (Pa),
is indicated.

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D3679 − 17

Pm = average maximum sustained static test pressure, which is then attached directly to framing, without intervening
lbf/ft2 (Pa), sheathing. The PEF and safety factor for each case are as
PEF = pressure equalization factor, 0.5, and follows:
SF = safety factor, 1.5. Case PEF Safety Factor
Case 1 0.7 2.0
A1.3.3 Alternative Design Pressure Ratings—Design pres- Case 2 1.0 2.0
sure ratings for applications other than the standard conditions
A1.3.3.4 Adjustment of the standard design pressure rating
described above can be developed. Common circumstances
is not necessary when foam plastic insulating sheathing is
where this is done include the use of alternative fastening
installed directly over sheathing that is capable of indepen-
methods in order to achieve a higher design pressure rating,
dently resisting both positive and negative wind pressures
and cases where the sheathing is not capable of independently
occurring under design conditions at the building location, or
resisting wind pressures under design conditions, which neces-
where the sheathing is fastened in a way that allows it to
sitates a reduction in the siding’s design pressure rating.
independently resist the design wind pressure. For such cases
A1.3.3.1 Alternative Fastening—Where an alternative fas-
the standard design pressure rating is applied.
tening method is specified by the manufacturer, the siding is
permitted to be tested under Test Method D5206 using the A1.4 Design Wind Speeds:
specified fastening. The resulting average maximum sustained
static test pressure is used in the above equation to determine A1.4.1 The wind velocity maps in ASCE 7-10 provide one
the alternative design pressure rating. In order for this alterna- source of design wind speeds for particular geographic regions.
tive rating to be realized, the siding must be installed using the The velocities on these maps are stated in terms of “ultimate,”
alternative method, and the rating must be clearly tied to 700-year return interval speeds. To be used in the procedure in
installation requirements in manufacturer’s literature and in- this Annex, those velocities need to be converted to the ASD
structions. equivalent in accordance with A1.1.2, and the resulting veloc-
A1.3.3.2 Alternative Sheathing—An adjusted design pres- ity V used in the equation in A1.1.3. The 2012 and 2015
sure rating for use of the siding over sheathings not capable of International Building Code and 2015 International Residential
independently resisting both positive and negative wind pres- Code also contain maps based on ultimate wind speeds.
sures occurring under design conditions at the building A1.4.2 Other maps are available that do not require conver-
location, as discussed in A1.2.6, can be calculated using the sion of wind velocities. Examples include the wind map in the
above equation if the appropriate PEF and safety factor are 2012 International Residential Code, on which the velocities
specified. have already been converted from those on the ASCE 7-10
A1.3.3.3 Alternative PEF and safety factor values have been maps. Maps from previous editions of ASCE 7 used ASD
documented (see 2009 and 2012 International Residential velocities and do not require conversion. However, only
Code, section R703.11.2) for one type of sheathing, foam editions since 1995 used the 3-second gust basis that is used in
plastic insulating sheathing complying with ANSI/SBCA FS this Annex. The 1998, 2002, and 2005 editions of ASCE 7
100. Two wall assembly cases are considered: 1) where the continued the use of 3-second gust wind basis, but with
interior surface of the wall is covered with gypsum wall board improved hazard modeling of hurricane wind speeds first made
or equivalent; and 2) where the interior surface of the wall is in the 1998 edition. These previous editions also do not have
not covered with gypsum wall board or equivalent. In both the benefit of further improved hurricane hazard modeling that
cases vinyl siding is installed directly over foam sheathing, was incorporated into the maps used in ASCE 7-10.

BIBLIOGRPHY

(1) ASHRAE Handbook of Fundamentals, American Society of States, American Society of Civil Engineers, Environmental Engi-
Heating, Refrigerating and Air Conditioning Engineers, Inc. Chap- neering Conference Preprint 431, Dallas, TX, Feb. 6, 1967.
ter 26, 1977. (5) Sachs, Peter, Wind Forces in Engineering, Pergamon Press,
(2) “ Wind Forces on Structures,” Transactions of the American Soci- Elmsford, NY 1972.
ety of Civil Engineers, Vol 126, Part II, 1961, pp. 1124–1198. (6) MacDonald, A. J., Wind Loading on Buildings, Applied Sciences
(3) AAMA, TIR-A2, American Architectural Manufacturers Assn., Publishers, Ltd., Essex, England, 1975.
Design Wind Loads for Aluminum Curtain Walls, American Archi- (7) Houghton, E., and Carruthers, N., Wind Forces on Buildings and
tectural Manufacturers Assn., 2700 River Rd., Palatine, IL. Structures, John Wiley & Sons, New York, NY, 1976.
(4) Thom, H. C. S., New Distribution of Extreme Winds in the United

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D3679 − 17
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D3679 - 13)
that may impact the use of this standard. (June 1, 2017)

(1) Section 2 was revised to add references to building codes Provisions specifying marking of the standard design pressure
and to the VSI Vinyl Siding Installation Manual. and alternative design pressures were added.
(2) Section 3 was revised to add definitions of design wind load (7) Subsection A1.2 was revised to add provisions for adjusting
pressure rating, standard wind load design pressure rating, and the minimum required test pressure for applications of siding
alternative wind load design pressure rating. over certain alternative sheathing types.
(3) Subsection 5.11 was revised to clarify current requirements (8) In A1.2.1, the pressure equalization factor was changed and
and put non-mandatory information in Notes, and to provide a reference added to research supporting this change.
for the determination of standard and alternative wind load (9) Added A1.2.1.1 to provide for the use of alternative
design pressure ratings. pressure equalization factors.
(4) In 5.11, the minimum static test pressure was changed to (10) In A1.2.3 and A1.2.3.1, the minimum test pressures were
reflect the change in pressure equalization factor in A1.2.1. changed to reflect the change in pressure equalization factor in
(5) Subsection 6.14 was revised to provide the standard test
A1.2.1.
conditions for determining compliance with the minimum test
(11) Subsection A1.3 was added to describe the procedures for
pressure and standard wind load design pressure rating.
determining design pressure ratings.
(6) Section 7 was deleted and its content merged into a new
Section 7 dealing with packaging and package marking.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3681 − 18

Standard Test Method for


Chemical Resistance of “Fiberglass”
(Glass–Fiber–Reinforced Thermosetting-Resin) Pipe in a
Deflected Condition1
This standard is issued under the fixed designation D3681; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D3567 Practice for Determining Dimensions of “Fiberglass”


1.1 This test method covers the procedure for determining (Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
the chemical-resistant properties of fiberglass pipe in a de- Fittings
flected condition for diameters 4 in. (102 mm) and larger. Both
glass–fiber–reinforced thermosetting resin pipe (RTRP) and 3. Terminology
glass–fiber–reinforced polymer mortar pipe (RPMP) are fiber- 3.1 Definitions:
glass pipes. 3.1.1 General—Definitions are in accordance with Termi-
NOTE 1—For the purposes for this standard, polymer does not include nology D883 and abbreviations are in accordance with Termi-
natural polymers. nology D1600 unless otherwise indicated.
1.2 Inch-pound units are to be regarded as the standard. The 3.2 Definitions of Terms Specific to This Standard:
values given in parentheses are for information only. 3.2.1 end point—the passage of the fluid through the pipe
1.3 This standard does not purport to address all of the wall unless otherwise stated. The failure mode may be
safety concerns, if any, associated with its use. It is the catastrophic, characterized by a sudden fracture through the
responsibility of the user of this standard to establish appro- pipe wall in the area of greatest strain, parallel to the axis of the
priate safety, health, and environmental practices and deter- pipe, with the fiber reinforcement cleanly broken at the edge of
mine the applicability of regulatory limitations prior to use. the fracture. Visual evidence of surface etching or pitting may
Specific precautionary statements are given in 9.5. or may not be present.
NOTE 2—There is no known ISO equivalent to this standard.
3.2.2 fiberglass pipe—tubular product containing glass fiber
reinforcements embedded in or surrounded by cured thermo-
1.4 This international standard was developed in accor- setting resin. The composite structure may contain aggregate,
dance with internationally recognized principles on standard- granular or platelet fillers, thixotropic agents, pigments, or
ization established in the Decision on Principles for the dyes. Thermoplastic or thermosetting liners or coatings may be
Development of International Standards, Guides and Recom- included.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 3.2.3 reinforced polymer mortar pipe (RPMP)—fiberglass
pipe with aggregate.
2. Referenced Documents 3.2.4 reinforced thermosetting resin pipe (RTRP)—
2.1 ASTM Standards:2 fiberglass pipe without aggregate.
D883 Terminology Relating to Plastics 3.2.5 strain-corrosion—the failure of the pipe wall caused
D1600 Terminology for Abbreviated Terms Relating to Plas- by the exposure of the inside surface, while in a strained
tics condition, to a corrosive environment for a period of time.

1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
4. Summary of Test Method
and is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic 4.1 This test method consists of exposing the interior of a
Piping Systems and Chemical Equipment.
Current edition approved Aug. 1, 2018. Published August 2018. Originally minimum of 18 specimens of pipe to a corrosive test solution
approved in 1978. Last previous edition approved in 2012 as D3681 – 12ɛ1. DOI: while the pipe is constantly maintained in a deflected condition
10.1520/D3681-18.
2
at differing induced initial ring flexural strain levels, and
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
measuring the time to failure for each strain level. Test
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on temperatures are obtained by testing in an air environment
the ASTM website. where the temperature is controlled.

*A Summary of Changes section appears at the end of this standard


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D3681 − 18
4.2 The long-term resistance of the pipe to the test solution run. The test specimens shall have a minimum length of one
is obtained by an extrapolation to 50 years of a log-log linear nominal pipe diameter or 12 in. (300 mm) 6 5 %, whichever
regression line for initial strain level versus time. is less.
NOTE 3—It is the consensus of Subcommittee D20.23 that the log–log
linear regression analysis of test data is a conservative approach and is 8. Test Conditions
representative of standard industry practice.
8.1 The standard temperature shall be 73.4 6 3.6°F (23 6
5. Significance and Use 2°C).
5.1 This test method evaluates the effect of a chemical
9. Procedure
environment on pipe when in a deflected condition. It has been
found that effects of chemical environments can be accelerated 9.1 General—Determine the initial strain level induced in
by strain induced by deflection. This information is useful and the pipe by calculation, or strain gage measurement, or both.
necessary for the design and application of buried fiberglass Procedure A describes the determination of initial strain by
pipe. calculation; Procedure B describes the determination of initial
strain as obtained by use of foil-type resistance strain gages.
NOTE 4—Pipe of the same diameter but of different wall thicknesses
will develop different strains with the same deflection. Also, pipes having 9.2 Determination of Test Level:
the same wall thickness but different constructions making up the wall 9.2.1 Test Procedure A:
may develop different strains with the same deflection.
9.2.1.1 In accordance with Practice D3567 measure the wall
6. Apparatus thickness to the nearest 0.001 in. (0.025 mm) in at least five
6.1 Use parallel plate apparatus suitable to maintain a equally spaced places along the bottom of the pipe specimen on
constant deflection on the pipe. In order to achieve uniform a line parallel with the pipe axis, and average the measure-
strain along the pipe, use 0.25-in. (6-mm) thick elastomeric ments.
pads between the parallel plate (channel) surfaces and the pipe 9.2.1.2 In accordance with Practice D3567 measure the
ring (see Note 5). Foil type, single element strain gages suitable vertical inside diameter to the nearest 0.01 in. (0.25 mm) at
for strain levels to 1.50 % strain and a length appropriate to the both ends prior to deflection and average the measurements.
diameter of the pipe are required when initial strain is to be NOTE 7—It is recommended that the vertical inside diameter be
determined by Procedure B (see Note 6). An example of the measured with the axis vertical.
apparatus required is shown in Fig. 1. 9.2.1.3 Place the pipe specimen in the test apparatus (Fig. 1)
NOTE 5—Elastomeric pads with a hardness of Shore A15 to 70 have with the measured wall thicknesses at the bottom and apply
been used successfully. force to the apparatus to deflect the specimen while keeping the
NOTE 6—Strain gages of 1⁄4 and 1⁄2-in. (6 and 13-mm) length have been top and bottom plates (channels) of the apparatus as near
found to be effective for pipe diameters 12 through 24 in. (305 through
610 mm). Consult the strain gage manufacturer for gage length recom-
parallel as possible. When the desired deflection is obtained,
mendations for other pipe diameters. lock the apparatus to maintain the specimen in the deflected
condition.
7. Test Specimens
NOTE 8—Alignment of the specimen within the channels is critical. The
7.1 The test specimens shall be ring sections taken from a channels shall not only be parallel with the load points 180° opposite, but
sample of pipe selected at random from a normal production the pipe shall be centered between the rods.

FIG. 1 Strain-Corrosion Test Apparatus

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9.2.1.4 Measure the vertical inside diameter of the deflected 9.3 When using Procedure A, verify the strain level by using
pipe specimen at both ends to the nearest 0.01 in. (0.25 mm). strain gages as described in Procedure B for at least one
Average the measurements and determine the deflection by specimen in every nine. Conversely, when using Procedure B,
subtracting the average vertical inside diameter after deflection verify the strain level by measurement and calculation as
from the measurement determined in 9.2.1.2. described in Procedure A for at least one specimen in every
9.2.1.5 Calculate the initial strain level using the following nine. If the calculated strain and the indicated strain do not vary
equation which includes compensation for increased horizontal more than 10 %, consider the strain levels accurate within
diameter with increasing deflection. normal experimental error.
ε T 5 428~ t !~ ∆ ! NOTE 12—Deflections in excess of 28 % of diameter may cause local

SD m1
∆ 2
2 D flattening of the pipe and lead to erratic strain distribution. For deflections
approaching 28 % improved accuracy is obtained by use of strain gages or
by establishing, for a typical pipe, a calibration of deflection versus
where: measured strain. This calibration technique is also useful at all deflection
levels as a check of the calculations by 9.2.1.5, which assumes neutral axis
at pipe wall midpoint.
εT = initial strain, %,
9.4 After the initial strain is obtained using Procedure A or
t = average wall thickness at bottom, in. (mm),
∆ = average deflection, in. (mm), B, install chemically inert dams using a flexible sealant so that
Dm = mean diameter, in. (mm) D̄ + t, and only the interior surface of the pipe will be exposed to the test
D̄ = average inside pipe diameter, free state, in. (mm). environment. The dams shall not add support to the pipe
specimen.
NOTE 9—The calculation assumes that the neutral axis is at the pipe 9.5 Place the apparatus containing the specimen in a chemi-
wall midpoint. For pipe wall constructions that produce an altered neutral cally resistant trough or pan and introduce the test solution. The
axis position, it may be necessary to evaluate results substituting 2 ȳ for
t. (ȳ is the distance from the inside pipe surface to the neutral axis.)
solution should be added within 30 minutes of locking the
Neutral axis position must be determined with strain gage couples. See apparatus and the time shall be recorded from the addition of
also Note 11. the solution. (Warning—Since the failure mode could be
catastrophic, precautions should be taken to contain any
9.2.2 Procedure B:
sudden leakage that may occur. The use of spacers (such as,
9.2.2.1 Carefully align and attach three strain gages on the wooden blocks) under the apparatus is suggested to reduce
inside bottom surface of the pipe specimen in the circumfer- attack of the apparatus after failure of the sample.)
ential direction to measure initial circumferential strains. Place
the gages perpendicular to the pipe axis as follows: one in the 9.6 Periodically check and maintain the test solution within
middle and the other two at the quarter points along the invert 65 % of the specified strength or concentration for the
of the specimen. The adhesive used to attach the gages shall not duration of the test. Maintain the level at a depth of not less
cover more than 37 % of the pipe specimen length along the than 1 in. (25.4 mm) during the period of the test.
invert. Zero-in the gages while the pipe is circular in shape. NOTE 13—As some solutions become more concentrated with the
evaporation of water, care must be exercised in replenishment to prevent
NOTE 10—It is recommended that the pipe specimen be placed with its a build-up in strength. It may be necessary, with some reagents, to
axis vertical to maintain roundness when the bridge is balanced to “zero” periodically clean the deflected specimen and replace the test solution with
the instrument. a fresh mixture. The use of plastic film, cut carefully to fit between the
9.2.2.2 After installing the strain gages, place the specimen dams and floated on the top of the test solution, has been found helpful in
reducing evaporation.
in the test apparatus (see Fig. 1) with the strain gages at the
bottom. Extreme care shall be taken to ensure that the gages are 9.7 Record the following data:
located at the point of maximum strain (6 o’clock position). 9.7.1 Average pipe wall thickness,
9.7.2 Average inside pipe diameter before deflection,
NOTE 11—Alignment of the specimen within the channels is critical. 9.7.3 Average inside pipe diameter after deflection,
The channels shall not only be parallel with the load points 180° opposite,
but the pipe shall be centered between the rods. 9.7.4 Percent deflection,
9.7.5 Initial strain and method of determination,
9.2.2.3 Apply force to the apparatus to deflect the specimen 9.7.6 Type, location, and time of any distress of the pipe
while keeping the top and bottom plates (channels) of the wall, and
apparatus as parallel as possible. When the desired strain level 9.7.7 Time to end point. Times are measured from the
is reached, lock the apparatus to maintain the specimen in the addition of solution.
deflected condition. Read the gages as soon as the apparatus is
locked. Initial strain shall be recorded within 2 min after 9.8 To determine the regression line and the lower confi-
locking the apparatus. At least two gages shall read within 5 % dence level for the report, a minimum of 18 samples is
of each other for a valid experiment. If any gage reads more required. Distribution of data points shall be as follows:
than 5 % from the average of the other two gages, disregard the Hours Failure Points
10 to 1000 at least 4
indication unless thickness verification implies the strain gage 1000 to 6000 at least 3
reading was accurate. Average the valid gage indications, and After 6000 at least 3
record as initial (indicated) strain. In addition, measure and After 10 000 at least 1
record the deflection. 9.9 Perform inspection of the test samples as follows:

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Hours Inspect at Least Hours to Failure (Average of Set) Failure Points


10 to 20 every 1 h 10 to 200 at least 3
20 to 40 every 2 h More than 1000 at least 3
40 to 60 every 4 h Total: at least 6
60 to 100 every 8 h
100 to 600 every 24 h For the purpose of reconfirmation, it is permitted to include
600 to 6000 every 48 h as failures those specimens which have not failed after 1200
After 6000 every week hours provided they exceed the regression line.
Record the time to end point for each specimen.
10.4 Consider any changes in material or manufacturing
NOTE 14—The use of electronic timers is considered highly desirable in process minor and permissible if the results of 10.3 meet the
monitoring failure time particularly on short term tests.
following criteria.
9.10 Analyze the test results by using for each specimen, the 10.4.1 The average time to failure for each strain level falls
logarithm of the strain in percent and the logarithm of the on or above the 95 % lower confidence limit of the original
time-to-failure in hours as described in Annex A1. Calculate regression line.
the strain at 50 years (YL). 10.4.2 The earliest individual failure time at each strain
9.11 Those specimens that have not failed after more than level falls on or above the 95 % lower prediction limit of the
10 000 h are permitted to be included as failures to establish original regression line.
the regression line. Use of these data points may result in a 10.4.3 The failure points are distributed about the originally
lower or higher extrapolated strain. In either case the require- determined regression line. No more than two-thirds of the
ments of 9.14 must be satisfied. individual failure points may fall below the original regression
NOTE 15—Non-failed specimens may be left under test and the line.
regression line recalculated as failures are obtained.
10.5 It is permitted to assume that data meeting the criteria
9.12 Determine the final line for extrapolation to 50 years of 10.4 are part of the original data set and a new regression
by the method of least squares given in Annex A1, using all line determined using all failure points. Specimens that have
end points along with those non-failure points selected by the not failed after 1200 hours are not suitable for establishing a
method described in 9.11. Calculate Sxy in accordance with new regression line; however, it is permitted to use these data
A1.4.2 and the coefficient of correlation, r, in accordance with points for the purpose of reconfirmation.
A1.4.3.
10.6 If the data fails to satisfy the criteria of 10.4.1, the
9.13 If Sxy is greater than 0 (see A1.4.2), consider the data changes are considered major and a new regression line must
unsuitable. be established. While the new test program is being conducted,
9.14 If the coefficient of correlation value (see A1.4.3), r, is an interim strain corrosion value for the material or process
less than the applicable minimum value given in Table A1.1 as change may be taken as the lower of:
a function of n, reject the data. 10.6.1 The 95 % lower confidence limit of the value ob-
9.15 Prepare a graph on a log-log diagram in accordance tained by extrapolating the failure points of 10.3 to 438 000 h
with 9.12 showing time to failure versus strain, with time (50 years) by the procedure in Annex A1.
plotted on the horizontal (x) axis and strain plotted on the 10.6.2 The 95 % lower confidence limit of the original
vertical (y) axis. regression line at 50 years.
10. Reconfirmation of Strain Corrosion Regression Line
11. Report
10.1 When a piping product has an existing strain corrosion
regression line, any change in material, manufacturing process, 11.1 The report shall include the following:
construction, or liner shall necessitate a screening evaluation 11.1.1 Complete identification of the pipe composition,
(reconfirmation) as described in 10.2, 10.3, 10.4, and 10.5. manufacturer’s code, size, and minimum wall thickness.
11.1.2 Test procedure used.
10.2 Calculate and plot the 95 % confidence limits and the
95 % prediction limits of the original regression line in 11.1.3 Data in 9.7.
accordance with A1.4 using only data obtained prior to the 11.1.4 Notations of any type of distress observed in the
change. specimens, whether it be discoloration, leakage, small fracture,
surface crazing, or complete cracking, together with the time
NOTE 16—Prediction limits define the bounds for single observations, and date of occurrence, and the location of distress. Indicate the
whereas confidence limits define the bounds for the regression line.
NOTE 17—For 95 % confidence limits, there is a 2.5 % probability that location of distress using the bottom center as the reference
the mean value for the regression line may fall above the UCL and a 2.5 % point.
probability that the mean value for the regression line may fall below the 11.1.5 Complete description of the test solution (reagent).
LCL. For 95 % prediction limits, there is a 2.5 % probability that
individual data points may fall above the UPL and a 2.5 % probability that
11.1.6 Type of strain gage employed and method of mount-
individual data points may fall below the LPL. ing.
10.3 From the original regression line, select strain levels 11.1.7 Temperature at which the test was run.
for at least two sets of specimens, each set consisting of three 11.1.8 Graph of 9.15.
or more specimens each to be tested at the same strain level as 11.1.9 Strains at 50 years.
follows: 11.1.10 Coefficient of correlation, r (see 9.12).

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12. Precision and Bias 13. Keywords
12.1 No precision and bias statement can be made for this 13.1 chemical resistance; constant deflection; extrapolation;
test method since controlled round-robin test programs have fiberglass pipe; regression line; strain-corrosion
not been run. This test method is generally used to evaluate
large-diameter fiberglass pipe.

ANNEX

(Mandatory Information)

A1. LEAST SQUARES CALCULATION FOR LONG TERM STRAIN CORROSION VALUE

A1.1 General yi = the log10 of Vi, where Vi is the strain at failure of


A1.1.1 The analysis is based on the following relationship: observation i; i = 1, . . . n,
xi = the log10 of ti, where ti is the time to failure (in hours) of
y 5 a1bx (A1.1) observation i; i = 1, . . . n,
where: ȳ = the arithmetic mean of all yi values:
y = one variable, 1
x = the other variable 5
n (y i (A1.2)
b = the slope of the line, and
a = the intercept on the y axis. x̄ = the arithmetic mean of all xi values:
A1.1.2 A linear functional relationship analysis (sometimes 1
called “covariance analysis”) is used, subject to tests for the
5
n (x i (A1.3)

sign (that is, “+” or “−”) of the slope and the coefficient of A1.4.2 Relevant Sums-of-Squares:
correlation for the quantity of data available. The relevant A1.4.2.1 Calculate the following sums-of-squares and
equations are given together with example data and results, on cross-products:
the basis of which any other statistical computing package may
1
be used subject to validation by agreement with the example S xy 5 ( ~ x 2 x̄ !~ y 2 ȳ !
i i (A1.4)
n
results to within the indicated limits.
A1.1.3 For the purposes of this annex, a design service life A1.4.2.2 If Sxy > 0, consider the data unsuitable for
of 50 years has been assumed. evaluating the material; otherwise, calculate also:
1
A1.2 Procedure for Analysis of Data S xx 5
n ( ~ x 2 x̄ !
i
2
(A1.5)

A1.2.1 Use a linear functional relationship analysis to 1


analyze n pairs of data values (as y and x) to obtain the S yy 5
n ( ~ y 2 ȳ !
i
2
(A1.6)
following information:
A1.4.3 Correlation of Data:
A1.2.1.1 The slope of line, b,
A1.4.3.1 Calculate the coefficient of correlation, r, from the
A1.2.1.2 The intercept on the y axis, a, following relationship:
A1.2.1.3 The correlation coefficient, r, and
A1.2.1.4 The predicted mean and the lower 95 % confi- 2
~ S xy! 2
r 5 (A1.7)
dence and prediction intervals on the mean value. ~ S xx 3 S yy!
r 5 =r 2
A1.3 Assignment of Variables
A1.4.3.2 If the value of r is less than the applicable
A1.3.1 Let x be log10t, where t is the time, in hours, and let
minimum value given in Table A1.1 as a function of n, reject
y be log10V, where V is the strain value.
the data; otherwise, proceed to A1.4.4.
A1.4 Functional Relationship Equations and Method of A1.4.4 Functional Relationships:
Calculation A1.4.4.1 To find a and b for the functional relationship line,
A1.4.1 Basic Statistics and Symbols: y = a + bx (Eq A1.1), first set:
A1.4.1.1 The following basic statistics and symbols are
used: λ5 S D S yy
S xx
(A1.8)

and then let:


n = the number of pairs of observed data values (Vi, ti),
b 5 2 =λ (A1.9)

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TABLE A1.1 Minimum Values for the Coefficient of Correlation, r, the variance, A, of a using the formula:
for Acceptable Data From n Pairs of Data
n
Number of variables
n-2
Degrees of freedom
Minimum r H
A 5 D x̄ 2 ~ 11τ ! 1
S xy
b J (A1.19)
3 1 0.9999
4 2 0.9900 the variance, σn2, of the fitted line at xL using the formula:
5 3 0.9587
6 4 0.9172
σ n 2 5 A12BxL 1CxL2 (A1.20)
7 5 0.8745 2
8 6 0.8343
the error variance, σε , for y using the formula:
9 7 0.7977 σ ε2 5 2λσ δ2 (A1.21)
10 8 0.7646
11 9 0.7348 2
the total variance, σy , for future values, yL, for y at xL using
12 10 0.7079
13 11 0.6835 the formula:
14 12 0.6614
15 13 0.6411
σ 2y 5 σ 2n 1σ ε2 (A1.22)
16 14 0.6226
17 15 0.6055
A1.4.5.5 Calculate the estimated standard deviation, σy, for
18 16 0.5897 yL using the equation:
19 17 0.5751
20 18 0.5614 σ y 5 ~ σ 2n 1σ ε2 ! 0.5 (A1.23)
21 19 0.5487
22 20 0.5368 and the predicted value, yL, for y at xLusing the relationship:
23 21 0.5256
24 22 0.5151
y L 5 a1bxL (A1.24)
25 23 0.5052
26 24 0.4958
where a and b have the values obtained in accordance with
27 25 0.4869 (Eq A1.9) and (Eq A1.10).
32 30 0.4487
37 35 0.4182 A1.4.6 Calculation and Confidence Intervals:
42 40 0.3932 A1.4.6.1 Calculate the lower 95 % prediction interval,
47 45 0.3721
52 50 0.3542
yL 0.95, predicted for yL using the equation:
62 60 0.3248 y L 0.95 5 y L 2 t v σ y (A1.25)
72 70 0.3017
82 80 0.2830
92 90 0.2673
where:
102 100 0.2540 yL = the value obtained in accordance with (Eq A1.24) when
xL is, as applicable, the value in accordance with (Eq
A1.11) appropriate to a design life of, for example, 50
and then: years (that is, xL = 5.6415 (in h)) or to a time at which
it is desired to predict with 95 % confidence the
a 5 ȳ 2 bx̄ (A1.10) minimum value for the next observation of V,
NOTE A1.1—Since y = log10V and x = log10t, hence V = 10y, t = 10x and σy = the value obtained in accordance with (Eq A1.23), and
the implified relationship for V in terms of t is therefore:
tv = the applicable value for Student’s t for v = n − 2 degrees
V 5 10~ a1b3log10 t ! of freedom, as given in Table A1.2 for a two sided 0.05
A1.4.5 Calculation of Variances: level of significance (that is, mean 6 2.5 %).
A1.4.5.1 If tL is the applicable time to failure, then set: A1.4.6.2 Calculate the corresponding lower 95 % prediction
x L 5 log10t L (A1.11) limit for V using the relationship:
V L 0.95 5 10Y L 0.95 (A1.26)
A1.4.5.2 Calculate, in turn, the following sequence of sta-
tistics. For i= 1 to i = n, the best fit, ξi, for true x, the best fit, A1.4.6.3 The predicted mean value of V at time tL, that is,
Yi, for true y and the error variance, σδ2, for x using (Eq A1.12), VL, is given by the relationship:
(Eq A1.13), and (Eq A1.14) respectively:
V L 5 10Y L (A1.27)
ξ i 5 $ λx i 1 ~ y i 2 a ! b % /2λ (A1.12)
where:
Y i 5 a1bξ i (A1.13)
YL = the value obtained in accordance with (Eq A1.24).
σ δ2 5 $ ( ~ y 2 Y ! 1λ ( ~ x 2 ξ ! % / $ λ ~ n 2 2 ! %
i i
2
i i
2
(A1.14) A1.4.6.4 Setting σy2 = σn2 in (Eq A1.22) will produce a
A1.4.5.3 Calculate the following quantities: confidence interval for the line rather than a prediction interval
for a future observation.
τ 5 bσ δ /2S xy (A1.15)
2
D 5 2λbσ /nSxy δ (A1.16)
A1.5 Example Calculation
B 5 2Dx̄ ~ 11τ ! (A1.17)
A1.5.1 Basic Data—The example data given in Table A1.3,
A1.4.5.4 Calculate the following variances: the variance, C, together with the example analysis given in this subsection, can
of b using the formula: be used to validate statistical packages or procedures. Because
C 5 D ~ 11τ ! (A1.18) of rounding errors, it is unlikely that there will be exact

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TABLE A1.2 Student’s “t” Value TABLE A1.3 Example Data for Example Calculation
(Two-Sided 0.05 Level of Significance) Data Time, Strain, Log Time, Log Strain,
n n-2 Student’s Point t %v x y
Number of variables Degrees of freedom t(0.05)
3 1 12.706 1 25.9 1.151 1.41330 0.06108
4 2 4.303 2 34.7 1.125 1.54033 0.05115
5 3 3.182 3 260.4 1.077 2.41564 0.03222
6 4 2.776 4 424.3 1.041 2.62767 0.01745
7 5 2.571 5 95.3 1.028 1.97909 0.01199
8 6 2.447 6 157.1 1.027 2.19618 0.01157
9 7 2.365 7 46.7 0.911 1.66932 −0.04048
10 8 2.306 8 124.7 0.902 2.09587 −0.04479
11 9 2.262 9 766.8 0.885 2.88468 −0.05306
12 10 2.228 10 1064 0.880 3.02694 −0.05552
13 11 2.201 11 1013 0.879 3.00561 −0.05601
14 12 2.179 12 2770 0.794 3.44248 −0.10018
15 13 2.160 13 12408 0.768 4.09370 −0.11464
16 14 2.145 14 4981 0.747 3.69732 −0.12668
17 15 2.131 15 3780 0.706 3.57749 −0.15120
18 16 2.120 16 4427 0.699 3.64611 −0.15552
19 17 2.110 17 28272 0.678 4.45136 −0.16877
20 18 2.101 18 16943 0.657 4.22899 −0.18244
21 19 2.093
22 20 2.086
23 21 2.080
24 22 2.074
25 23 2.069
26 24 2.064
27 25 2.060
r = 0.9023764
32 30 2.042 A1.5.4 Functional Relationships:
37 35 2.030
42 40 2.021
47 45 2.014
52 50 2.009 λ = 6.852660 × 10−3
62 60 2.000 b = −8.278079 × 10−2
72 70 1.994
82 80 1.990
a = 0.1800067
92 90 1.987 A1.5.5 Calculated Variances:
102 100 1.984

D = 9.266935× 10−5
agreement, but acceptable procedures should agree within B = −2.839595 × 10−4
60.1 % of the results given in A1.5.6. C (variance of b) = 9.830865 × 10−5
A1.5.2 Sums of Squares: A (variance of a) = 8.919367 × 10−4
σn2 (error variance for x) = 8.168303× 10−4
Sxx = 0.8578342 σε2 (error variance for y) = 1.29122 × 10−3
Syy = 5.878446 × 10−3 A1.5.6 Confidence Limits—For N = 18 and Student’s t of
Sxy = −0.064080 2.1199, the estimated mean and confidence and prediction
A1.5.3 Coeffıcient of Correlation: intervals are given in Table A1.4.

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TABLE A1.4 Confidence Limits
Time, h Mean Lower Confidence Lower Prediction
Interval Interval

1 1.51 1.31 1.20


10 1.25 1.13 1.04
100 1.03 0.97 0.86
1000 0.85 0.82 0.71
10 000 0.71 0.66 0.59
100 000 0.58 0.52 0.47
438 000 0.52 0.45 0.41

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D3681 – 12ɛ1) that may impact the use of this standard. (August 1, 2018)

(1) Clarified the intent and use of data for reconfirmation (3) Revised Tables A1.1 and A1.2 to unify range of variables
testing –Section 10. considered.
(2) Eliminated instances of non-mandatory language.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3753 − 19

Standard Specification for


Fiberglass (Glass-Fiber-Reinforced Thermosetting-Resin)
Manholes and Wetwells1
This standard is issued under the fixed designation D3753; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* Electrical Insulating Materials


1.1 This specification covers “fiberglass” (glass fiber- D790 Test Methods for Flexural Properties of Unreinforced
reinforced thermosetting-resin) manholes and wetwells fabri- and Reinforced Plastics and Electrical Insulating Materi-
cated with polyester, vinyl ester, or epoxy resin for use als
primarily in sanitary, storm, and industrial sewer applications. D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plas-
1.2 The values given in inch-pound units are to be regarded tics
as the standard. The values in parentheses are provided for D2412 Test Method for Determination of External Loading
information purposes only. Characteristics of Plastic Pipe by Parallel-Plate Loading
1.3 The following precautionary caveat pertains only to the D2583 Test Method for Indentation Hardness of Rigid Plas-
test methods portion, Section 8, of this specification: This tics by Means of a Barcol Impressor
standard does not purport to address all of the safety concerns, D2584 Test Method for Ignition Loss of Cured Reinforced
if any, associated with its use. It is the responsibility of the user Resins
of this standard to establish appropriate safety, health, and D3892 Practice for Packaging/Packing of Plastics
environmental practices and determine the applicability of
regulatory limitations prior to use. 3. Terminology
NOTE 1—There is no known ISO equivalent to this standard. 3.1 General—Definitions are in accordance with Terminol-
ogy D883 and the abbreviations are in accordance with
1.4 This international standard was developed in accor-
Terminology D1600 unless otherwise indicated.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 3.2 bench and invert, n—internal flow channel with a sloped
Development of International Standards, Guides and Recom- bench extending from the edge of the flow channel to the
mendations issued by the World Trade Organization Technical manhole wall designed to facilitate the flow of liquid through
Barriers to Trade (TBT) Committee. the manhole between the pipe connectors.
3.3 bottom, n—a flat, domed, dished, or other shaped bottom
2. Referenced Documents designed to make the manhole or wetwell watertight at its base.
2.1 ASTM Standards:2 3.4 expanded base manhole, n—a manhole with a larger
C581 Practice for Determining Chemical Resistance of diameter base section and reduced diameter riser section. (See
Thermosetting Resins Used in Glass-Fiber-Reinforced Fig. 1 for a typical manhole and an expanded base manhole.)
Structures Intended for Liquid Service 3.5 expanded base reducer, n—a portion of the manhole,
D695 Test Method for Compressive Properties of Rigid between the manway reducer and bottom, that changes from
Plastics one diameter to another in the cylindrical portion of the
D785 Test Method for Rockwell Hardness of Plastics and structure.
3.6 manway reducer, n—the top portion of the manhole
1
through which entrance to the manhole is made and where the
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced diameter increases from the entrance way to the larger manhole
Plastic Piping Systems and Chemical Equipment. cylinder.
Current edition approved Sept. 1, 2019. Published September 2019. Originally
approved in 1979. Last previous edition approved in 2012 as D3753 – 12ε1. DOI:
3.7 manhole, n—a constant diameter cylinder attached to a
10.1520/D3753-19. manway reducer designed to handle a manhole cover and ring.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.8 manhole cover and frame, n—those accessories used
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on with the manhole to close the manway entrance (includes grade
the ASTM website. adjustment rings).

*A Summary of Changes section appears at the end of this standard


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D3753 − 19

FIG. 1 Typical Manhole and Expanded Base Manhole

3.9 manhole cylinder, n—the portion below the manway permitted to be added as required by the specific manufacturing
reducer that extends in a constant diameter to the manhole process to be used to meet the requirements of this standard.
base. The resulting reinforced-plastic material shall meet the require-
3.10 pipe connectors, n—connectors that provide access for ment of this specification. Use of fillers is permitted when
the sewer pipe into the manhole. agreed upon between fabricator and purchaser. See Note 2.
3.11 resin rich, adj—describes that portion of the glass NOTE 2—The use of paints, coatings, pigments, dyes, colorants and
fiber-reinforced thermosetting-resin material where the resin- fillers may interfere with visual inspection of the laminate.
to-glass ratio is significantly greater than in other portions of 4.5 Other Materials—The use of polyester filaments, poly-
the manhole. ester scrim, glass fiber scrim, or similar material as processing
3.12 wetwell, n—a cylindrical structure which is permitted aids is permitted. The resulting reinforced-plastic material shall
to be open at the top or include a top. meet the requirement of this specification.
3.13 wetwell top, n—a flat, domed, dished or other shaped 4.6 Ribs—When used, ribs are permitted to be manufactured
top attached at the top of a wetwell structure. The top may as a solid construction or with materials applied over a
include ribs or other structures to add stiffness. Stiffening structural or non-structural form. The resulting reinforced-
features are permitted to be added to the interior or exterior plastic material shall meet the requirement of this specification.
surface, and may be integral or added as a secondary feature.
It is permitted to use a similar top on manholes. 5. Manufacture
5.1 Manholes, wetwells, manway reducers, eccentric or
4. Materials concentric reducers, connectors, tops and bottoms shall be
4.1 Resin—The resins used shall be a commercial grade produced from glass fiber-reinforced thermosetting resin with
thermosetting unsaturated polyester, vinyl ester or epoxy resin. construction determined by the particular process of manufac-
4.2 Reinforcing Materials—The reinforcing materials shall ture and configuration. The process is permitted to include
be commercial grade of E-type glass fibers in the form of mat, contact molding, compression molding, pultrusion, filament
continuous roving, chopped roving, or roving fabric, having a winding, resin transfer molding, spray up, hand lay-up, cen-
coupling agent that will provide a suitable bond between the trifugal casting, vacuum bagging, or other methods. Ribs are
glass reinforcement and the resin. permitted to be attached to the interior or the exterior surface.
4.3 Surfacing Material—If reinforcing material is used on 5.2 Interior Access—All manholes and wetwells shall be
the surface exposed to the contained substance, it shall be a designed so that a ladder or step system can be supported by
commercial grade chemical-resistant glass or organic surfacing the installed manhole or wetwell.
mat having a coupling agent that will provide a suitable bond 5.3 Manway Reducer—Manway reducers are permitted to
with the resin. be eccentric or concentric with respect to the larger portion of
4.4 Fillers and Additives—Fillers, such as sand, calcium the manhole.
carbonate, etc., when used, shall be inert to the environment 5.4 Cover and Ring Support—Manholes shall provide an
and manhole or wetwell construction. Additives, such as area from which a typical ring and cover plate can be supported
thixotropic agents, catalysts, promoters, pigments, etc., are without damage to the manhole.

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5.5 Assembly Joints—Product segments are permitted to be 6.4 Manhole Performance Test—One complete manhole
joined together to form a complete manhole or wetwell. manufactured in a manner consistent in every way with this
5.6 Manhole or Wetwell Bottom—Bottom shall be designed specification shall meet the performance criteria in 6.4.1 –
to be water tight and withstand the external hydraulic pressure 6.4.3. If a change in materials or methods of manufacturing is
of water to grade. The bottom design is permitted to include made and that change may affect the results of these tests, then
methods to anchor the bottom to a concrete base or other the testing shall be repeated. These tests are to be conducted on
external structure to provide the required resistance to external a representative manhole to qualify the finished product
pressure. characteristics. They are not considered to be a quality control
procedure and are not required for production parts.
5.7 Bench and Invert—Bench and invert are permitted to be 6.4.1 Load Rating—The complete manhole shall have a
produced from glass fiber-reinforced thermosetting resin or minimum dynamic-load rating of 16 000 lbf (71 172 N) when
other material suitable for the contents of the manhole. The tested in accordance with 8.4. To establish this rating, the
bench and invert are permitted to include one or more 1⁄2-in. complete manhole shall not leak, crack, or suffer other damage
diameter ports to allow the equalization of pressure between when load tested to 40 000 lbf (177 929 N) and shall not
the manhole interior and the cavity under the bench and invert. deflect vertically downward more than 0.25 in. (6.35 mm) at
Use of larger ports is permitted to allow the field installation of the point of load application when loaded to 24 000 lb (106 757
concrete or grout in the cavity under the bench and invert. N).
6.4.2 Stiffness—The manhole cylinder shall have the mini-
6. Requirements mum pipe-stiffness values shown in Table 1 when tested in
6.1 Workmanship: accordance with 8.5. It is permitted to interpolate stiffness
6.1.1 Exterior Surface—The exterior surface shall be rela- requirements for other manhole lengths between the values in
tively smooth with no sharp projections. Hand-work finish is Table 1.
acceptable if enough resin is present to saturate all fibers. The 6.4.3 Soundness—The manholes shall not leak when tested
exterior surface shall be free of blisters larger than 0.5 in. (12.7 in accordance with 8.6.
mm) in diameter and delamination. Fibers loosely attached 6.5 Wetwell Stiffness—The wetwell cylinder shall have the
(can be removed with wire brush) are allowed if not excessive. minimum pipe-stiffness value shown in Table 1 when tested in
6.1.2 Exterior Paint or Pigmentation—Use of exterior accordance with 8.5. It is permitted to interpolate stiffness
paints, coatings, pigments and colorants is permitted when requirements for other wetwell lengths between the values in
agreed upon between fabricator and purchaser. See Note 2. Table 1. These tests are to be conducted on a representative
6.1.3 Interior Surface—The interior surface shall be resin wetwell to qualify the finished product characteristics. They
rich with no exposed fibers. The surface shall be free of are not considered to be a quality control procedure and are not
crazing, delamination, blisters larger than 0.5 in. (12.7 mm) in required for production parts.
diameter, and wrinkles of 0.125 in. (3.2 mm) or greater in
depth. Surface pits shall be permitted up to 6/ft2 (60/m2 ) if they NOTE 3—Table 1 values are based upon a surrounding soil modulus of
750 psi or greater. This value is representative of moderately compacted
are less than 0.75 in. (19 mm) in diameter and less than 0.0625 fine grain sand.
in. (1.6 mm) deep. Voids that cannot be broken with finger
pressure and that are entirely below the resin surface shall be 6.6 Chemical Resistance—Manhole or wetwell samples
permitted up to 4/ft2 (40/m2) if they are less than 0.5 in. (12.7 manufactured in a manner consistent in every way with this
mm) in diameter. specification shall be tested in accordance with 8.7. The log of
6.1.4 Interior Paint or Pigmentation—Use of interior paints, percent retention of each property after immersion testing
coatings, pigments, and colorants are permitted when agreed when plotted against the log of immersion time, and extrapo-
upon between fabricator and purchaser. See Note 2. lated to 100 000 h shall assure retention of at least 50 % of
6.1.5 Indentations—Indentations or other shape imperfec- initial properties. If a change is made in the manhole construc-
tions that will not affect performance are allowed. tion and that change may affect the results of the chemical
resistance testing, then the testing shall be repeated. Chemical
6.2 Repairs—Any manhole or wetwell is permitted to be testing is conducted to determine the applicability of the
repaired to meet all requirements of this specification. materials used in the manufacture of the manhole to the
6.3 Dimensions—The dimensions shall be as shown below specified use conditions. It is not considered to be a quality
when measured in accordance with 8.3.1. control procedure.
6.3.1 Minimum cylinder internal diameter of the manhole or
wetwell shall be 42 in. (1057 mm). The minimum manway
reducer inside diameter shall be 21 in. (533 mm). TABLE 1 Stiffness Requirements
6.3.2 Manhole or wetwell lengths shall be in 6-in. (152-mm) Manhole or Wetwell Length, ft F/∆Y, psi (kPa)
(mm)
increments 62 in. (51 mm).
6 (1829) 0.72 (4.96)
6.3.3 Nominal inside diameters shall be 42 in. (1067 mm), 12 (3658) 1.26 (8.69)
48 in. (1219 mm), 54 in. (1372 mm), 60 in. (1524 mm), 66 in. 20 (6096) 2.01 (13.86)
(1676 mm), and 72 in. (1829 mm). Tolerance on the inside 25 (7620) 3.02 (20.82)
35 (10668) 5.24 (36.13)
diameter shall be 61 %. Other diameters are allowed and are 50 (15240) 8.42 (58.81)
covered by this specification.

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6.7 Material Properties—The following properties shall be Make a minimum of one thickness reading per 34 ft2 (3 m2) of
established for each type of construction used in the manhole surface in areas of constant thickness. Through regions of wall
or wetwell. If a change in materials or methods of manufac- taper, make sufficient checks to establish the actual thickness.
turing is made and that change may affect the results of the 8.4 Load Rating:
following tests, then the testing shall be repeated. Material 8.4.1 Load Test—The manhole tested shall be long enough
properties tests are conducted to qualify the finished product to include at least one of all unique or repetitive features of the
characteristics. They are not considered to be a quality control cylinder wall such as: bonded joints, adhesive seams, gasketed
procedure and are not required for production parts. joints, etc., except for reducers and cylinder sections of a
6.7.1 Material Composition—The material composition of different diameter than the manhole. In any case, the minimum
the manhole or wetwell in percent by weight shall be deter- length of the manhole cylinder shall not be less than 36 in. (914
mined in accordance with 8.8.1. mm) for each cylinder diameter.
6.7.2 Compressive Strength—The compressive strength in 8.4.1.1 Concentric Manholes—The manhole to be tested
the hoop and axial directions of the manhole or wetwell shall shall be complete with cover and supporting ring installed.
be determined in accordance with 8.8.2. Apply the specified load eccentrically (see Fig. 2 for typical
6.7.3 Flexural Strength and Modulus—The flexural strength test model) on a 6 in. by 6 in. by 1⁄2 in. (152 mm by 152 mm
and flexural modulus of elasticity, in the hoop and axial by 12.7 mm) steel plate resting on the manhole cover. Locate
directions of the manhole or wetwell, shall be determined in the steel loading plate so that the center of the plate is within
accordance with 8.8.3. Where component geometry will ad- 4 in. (102 mm) from the edge of the cover. Load in 2000-lbf
versely affect the test results (an example would be flexural (8896-N) increments with close inspection between increases.
testing on curved samples taken in the hoop direction), hand Maintain the specified load for not less than 15 min.
fabricated samples made consistent with the materials and 8.4.1.2 Eccentric Manholes—The manhole to be tested shall
construction of the manhole or wetwell are permitted for be complete with cover and supporting ring installed. Apply
testing. the specified load eccentrically (see Fig. 3 for typical test
6.8 Hardness—The surface hardness of the manhole or model) 6 in. by 6 in. by 1⁄2 in. (152 mm by 152 mm by 12.7
wetwell shall be determined in accordance with 8.8.4. mm) steel plate resting on the manhole cover. Locate the steel
6.9 Thickness—The thickness of each manhole or wetwell loading plate so that the center of the plate is within 4 in. (102
component part shall be determined in accordance with 8.3.2. mm) from the edge of the cover at a point where the edge of the
cover is nearest to the axis of the manhole cylinder. Load in
6.10 Field Vacuum Test Capability—Each manhole or 2000-lbf (8896-N) increments with close inspection between
wetwell shall be designed to be structurally capable of with- increases. Maintain the specified load for not less than 15 min.
standing a field applied test vacuum of -5 psi (-34 kPa) gauge 8.4.2 Deflection Test—When load tested according to the
after installation and backfilling. This design requirement is not procedure as outlined in 8.4.1.1 and 8.4.1.2 the top of the
to imply that a field vacuum test must be performed. manhole(s) shall not deflect vertically downward more than
7. Quality Control
7.1 Examination—Each manhole or wetwell component
part shall be examined for workmanship dimensions, hardness,
and thickness in accordance with Section 6.
7.2 Composition Control—Controls on glass and resin con-
tent shall be maintained for all manhole or wetwell manufac-
turing processes. Records shall be maintained as needed to
ensure products meet the requirements of the specification.
Proper glass content by glass usage checks, by periodic glass
and resin application rate checks, or by periodic material
composition testing in accordance with 8.8.1 is permitted.
8. Test Methods
8.1 Conditioning—Specimens tested shall be representative
of the actual manufacturing process. Conditioning of the
specimens is not allowed unless specified by this specification.
8.2 Test Conditions—Conduct at ambient temperature with-
out any special controls on temperature unless otherwise Table of Dimensions
specified.
in. (mm)
8.3 Dimensions:
8.3.1 Measure dimensions other than thickness with a steel A 21 min (533 min)
B 42 min (1067 min)
tape with graduations of 0.125 in. (3 mm) or less. C 6 by 6 by 1⁄2 (152 by 152 by 12.7)
8.3.2 Thickness—Measure to the nearest 0.01 in. (0.25 mm)
with a micrometer, caliper, gauge, or other suitable instrument. FIG. 2 Concentric Manhole Load Test Model

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8.7.1 Test Specimen Construction—Make the basic test
specimen in a manner consistent in every way with the
manhole or wetwell construction. This includes, among other
considerations, percent glass, type of glass, resin type, catalyst
system, post-cure (if any), fillers and additives (if any), and the
exclusion or not of air from the laminate surfaces. Test
specimens shall be tested in their as-manufactured state with no
conditioning. Each specimen shall be large enough to allow a
minimum of three individual flexural test samples.
8.7.1.1 If the specimen is to be tested in an environment
simulating a contained substance, use of a resin-rich layer is
permitted to be added to the exterior portion of the specimen.
This second resin-rich surface, not present in the manhole
itself, shall be of the same construction and thickness; and
made with the same considerations (that is, exclusion of air) as
the primary layer on the opposite side of the specimen. Where
a dual-resin construction is used, this second resin-rich layer
shall employ the same resin as the primary layer. Seal cut edges
Table of Dimensions with the resin used in the resin-rich surfaces.
in. (mm) 8.7.1.2 If the specimen is to be tested in an environment
simulating soil conditions, it shall be that described in 8.7.1.
A 21 min (533 min)
B 42 min (1067 min)
Seal cut edges of the specimen with that resin used in the outer
C 6 by 6 by 1⁄2 (152 by 152 by 12.7) surface of the manhole.
8.7.2 Test Intervals—Test specimens after one, three, six,
FIG. 3 Eccentric Manhole Load Test Model
and twelve months immersions in each test medium. It is
permitted to include an extra specimen at the time of initial
immersion in the event it is necessary to extend the test interval
0.25 in. (6.35 mm) when measured at the point of load
beyond one year because of inconclusive results at that time.
application when the specified load is 24 000 lbf (106 757 N).
Cut each specimen into at least three samples for flexural tests.
8.4.3 Where expanded base manholes have had their man-
hole portion tested in accordance with 8.4.1 and 8.4.2, it is 8.7.3 Test Media—Test media shall represent as completely
permitted to include reducers and attached cylinder sections as possible the actual environment of the manhole or wetwell
designed by the manufacturer to carry the loads in 8.4.1 in service. Throughout the test period, change the test media as
without load testing. Use of generally accepted design methods required to maintain the properties of the test media.
including closed form solutions, or finite element analysis 8.7.3.1 Interior Surface—The required test medium for the
(FEA), or both is permitted. The calculations shall show that interior surface shall be the material to be contained in the
the entire expanded base manhole will meet the requirements manhole or wetwell. When the manhole or wetwell is intended
of 8.4.2. to be placed in a raw sanitary sewage environment, a 5 %
sulfuric acid solution shall be used to simulate this environ-
8.5 Stiffness—Test a section of the cylinder portion of the ment.
manhole or wetwell in accordance with Test Method D2412. 8.7.3.2 Exterior Surface—Test the following media repre-
The section tested shall be free of any joints, repetitive senting the exterior surface environment:
features, or repairs. For manholes or wetwells larger than 72 in. (a) Sodium chloride, saturated solution.
(1829 mm) diameter, the use of generally accepted design (b) Standard buffer aqueous solution at 73°F (22.8°C)
methods including closed-form solutions, finite element analy- simulating alkaline soil (pH of 10).
sis (FEA), or both is permitted. (c) Standard buffer aqueous solution at 73°F (22.8°C)
8.6 Manhole Soundness—In order to determine soundness, simulating acidic soil (pH of 4).
apply an air or water pressure test, or both to the manhole test 8.7.4 Test Temperatures—The temperature of each test me-
sample described in 8.4.1. The test pressure shall not be less dium used in corrosion-resistance verification of the manhole
than 3 psig (20.68 kPa) or greater than 5 psig (34.47 kPa). or wetwell interior shall be the maximum suggested service
While holding at the established pressure, inspect the entire temperature for that medium. All media representing soil
manhole for leaks. Any leakage through the laminate, joints, or conditions and sanitary sewage shall be 73°F (22.8°C).
repairs is cause for failure of the test. (Warning—Care shall be 8.7.5 Interpretation of Results:
taken in the air test ensuring that the test is run in an isolated 8.7.5.1 Properties to be determined initially and after each
or confined area. The preferred method is to fill the manhole test period are flexural strength and flexural modulus (both in
with water and add air pressure.) accordance with Test Methods D790, Method I, Procedure A),
8.7 Chemical Resistance—The testing procedure for mea- and Barcol hardness (in accordance with Test Method D2583)
suring chemical resistance shall conform with Practice C581 of the interior of the laminate. The specimen shall not be cured
with the exceptions noted below. and shall represent the as-manufactured state of cure.

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8.7.5.2 Note any effect upon the immersion medium or 9. Inspection
specimen observed during visual inspection and use to aug- 9.1 Inspection of finished manholes and wetwells shall be
ment physical data in determining the suitability of the made as agreed upon between the purchaser and the supplier as
manhole or wetwell in any given medium. part of the purchase contract.
8.7.5.3 Plot the average log of percent retention of each
property (see 8.7.5.1) for all samples (at least three samples per 10. Rejection and Rehearing
specimen, see 8.7.3.2) after immersion testing (versus initial)
10.1 Manholes or wetwells that fail to conform to the
against the log of immersion time in hours (see Fig. 4).
requirements of this specification may be rejected. Rejection
8.8 Material Properties—Specimens taken from a manhole shall be reported to the manufacturer or supplier promptly and
or wetwell shall be used, if possible, to establish material in writing. In case of dissatisfaction with the results of any test,
properties. If it is not possible to take the specimens from a the manufacturer or supplier is permitted to make a claim for
manhole or wetwell because of dimensional requirements for a rehearing.
testing, make the specimens independently but, in any case,
they shall be consistent in all respects with the construction of 11. Certification
the manhole or wetwell. Test specimens shall be tested in their 11.1 When requested by the purchaser on his order, a
as-manufactured state with no conditioning. certification shall be made the basis of acceptance. This shall
8.8.1 Material Composition—Determine composition in ac- consist of a copy of the manufacturer’s test report or a
cordance with Test Method D2584. For specimens with fillers statement by the supplier, accompanied by a copy of the test
or additives, or both, separate the residue into its components results, that the manhole or wetwell has been tested, and
(glass, sand, etc.) to determine the glass content. inspected in accordance with the provisions of this specifica-
8.8.2 Compressive Strength—Determine compressive tion and meets all requirements. Each certification so furnished
strength in accordance with Test Method D695. shall be signed by an authorized agent of the supplier or
8.8.3 Flexural Strength and Modulus—Determine flexural manufacturer.
strength and flexural modulus of elasticity in accordance with
Test Methods D790. Where strength property test methods 12. Packaging and Package Marking
require flat specimens, specimens shall be constructed consis-
tently with the method of fabrication selected for the manhole 12.1 The manholes or wetwells shall be marked with the
or wetwell. following information:
8.8.4 Hardness—Determine Rockwell hardness in accor- 12.1.1 This ASTM designation,
dance with Test Method D785 or Barcol hardness in accor- 12.1.2 Manufacturer’s name or trademark,
dance with Test Method D2583. The frequency of checks shall 12.1.3 If available, manufacturing serial number, and
not be less than three random points per component part. The 12.1.4 Manhole or wetwell total length.
minimum acceptable value of cure shall not be less than 90 % 12.2 All packing, packaging, and marking provisions of
of the resin manufacturer’s minimum value for the cured resin. Practice D3892 shall apply to this specification.

SUMMARY OF CHANGES

FIG. 4 Chemical Test Property Retention

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D3753 − 19
Committee D20 has identified the location of selected changes to this standard since the last issue
(D3753 - 12ε1) that may impact the use of this standard. (September 1, 2019)

(1) The title and several sections have been revised to allow for (12) Subsection 6.3.3 – Language was revised to clarify that
the use of vinyl ester and epoxy resins. additional diameters are allowed and covered under this
(2) Figure 1 – Graphic presentation of an expanded base standard.
manhole has been added. (13) Table 1 – Maximum length is increased to 50-feet (15240-
(3) Subsection 3.4 – Definition of “expanded base manhole” mm) and the associated minimum stiffness requirement is
was revised. provided.
(4) Subsection 3.5 – Definition of “expanded base reducer” (14) Note 2 – Assumed minimum soil modulus has been added
was added. as explanation for stiffness values provided in Table 1.
(5) Subsection 3.13 – Definition of “wetwell top” was added. (15) Subsection 6.10 – Clarifies language and specifies condi-
(6) Subsection 4.4 – Language was added to allow for use of tions upon which a vacuum test must be performed.
fillers upon agreement between fabricator and user.
(16) Subsection 7.2 – The word “periodic” has been added to
(7) Note 1 – Supplemental language was added to support
clarify that this practice is not a continuous requirement.
subsections 4.4, 6.1.2, and 6.1.4.
(17) Subsection 8.4.1 – Specifies that the “cylinder” sidewall
(8) Subsection 5.7 – Terminology was changed from “area” to
“cavity” under bench and invert. Option to allow for grout of the structure is to be tested and that fittings are not intended
ports has been added. to be inclusive in this test requirement.
(9) Subsection 6.1.2 – Language was revised to allow for use (18) Subsection 8.5 – Allows for calculating stiffness at diam-
of external coatings, pigments and other additives upon agree- eters greater than 72-in. (1829 mm).
ment between fabricator and user. (19) Subsection 8.7.3.1 – Requires a 5 % sulfuric acid solution
(10) Subsection 6.1.4 – Specification of maximum void thick- to simulate a raw sanitary sewage environment.
ness within laminate was removed. (20) Editorial changes are provided in multiple locations to
(11) Subsection 6.1.5 – Language was revised to allow for use correct the usage of the word “may.”
of internal coatings, pigments and other additives upon agree- (21) Figures and tables have been re-numbered to accommo-
ment between fabricator and user. date additions.

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of infringement of such rights, are entirely their own responsibility.

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Designation: D3754 − 19

Standard Specification for


“Fiberglass” (Glass-Fiber-Reinforced Thermosetting-Resin)
Sewer and Industrial Pressure Pipe1
This standard is issued under the fixed designation D3754; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 2. Referenced Documents


1.1 This specification covers machine-made fiberglass pipe, 2.1 ASTM Standards:2
8 in. (200 mm) through 156 in. (4000 mm), for use in pressure C33 Specification for Concrete Aggregates
systems for conveying sanitary sewage, storm water, and many C581 Practice for Determining Chemical Resistance of
industrial wastes, and corrosive fluids. Both glass-fiber- Thermosetting Resins Used in Glass-Fiber-Reinforced
reinforced thermosetting-resin pipe (RTRP) and glass-fiber- Structures Intended for Liquid Service
reinforced polymer mortar pipe (RPMP) are fiberglass pipes. D638 Test Method for Tensile Properties of Plastics
This standard is suited primarily for pipes to be installed in D695 Test Method for Compressive Properties of Rigid
buried applications, although it may be used to the extent Plastics
applicable for other installations such as, but not limited to, D790 Test Methods for Flexural Properties of Unreinforced
jacking, tunnel lining and slip-lining and rehabilitation of and Reinforced Plastics and Electrical Insulating Materi-
existing pipelines. Pipe covered by this specification is in- als
tended to operate at internal gage pressures of 450 psi (3103 D883 Terminology Relating to Plastics
kPa) or less. D1600 Terminology for Abbreviated Terms Relating to Plas-
tics
NOTE 1—For the purposes of this standard, polymer does not include
natural polymers. D2290 Test Method for Apparent Hoop Tensile Strength of
Plastic or Reinforced Plastic Pipe
1.2 The values given in inch-pound units are to be regarded D2412 Test Method for Determination of External Loading
as the standard. The values given in parentheses are provided Characteristics of Plastic Pipe by Parallel-Plate Loading
for information purposes only. D2584 Test Method for Ignition Loss of Cured Reinforced
1.3 The following precautionary caveat pertains only to the Resins
test method portion, Section 8, of this specification: This D2992 Practice for Obtaining Hydrostatic or Pressure De-
standard does not purport to address all of the safety concerns, sign Basis for “Fiberglass” (Glass-Fiber-Reinforced
if any, associated with its use. It is the responsibility of the user Thermosetting-Resin) Pipe and Fittings
of this standard to establish appropriate safety, health, and D3567 Practice for Determining Dimensions of “Fiberglass”
environmental practices and determine the applicability of (Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
regulatory limitations prior to use. Fittings
D3681 Test Method for Chemical Resistance of “Fiberglass”
NOTE 2—There is no known ISO equivalent to this standard. (Glass–Fiber–Reinforced Thermosetting-Resin) Pipe in a
1.4 This international standard was developed in accor- Deflected Condition
dance with internationally recognized principles on standard- D3892 Practice for Packaging/Packing of Plastics
ization established in the Decision on Principles for the D4161 Specification for “Fiberglass” (Glass-Fiber-
Development of International Standards, Guides and Recom- Reinforced Thermosetting-Resin) Pipe Joints Using Flex-
mendations issued by the World Trade Organization Technical ible Elastomeric Seals
Barriers to Trade (TBT) Committee. F412 Terminology Relating to Plastic Piping Systems
F477 Specification for Elastomeric Seals (Gaskets) for Join-
ing Plastic Pipe
1
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced
2
Plastic Piping Systems and Chemical Equipment. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2019. Published December 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1979. Last previous edition approved 2014 as D3754 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D3754-19. the ASTM website.

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D3754 − 19
TABLE 1 General Designation Requirements for Fiberglass Pressure Pipe
Desig-
Property Cell LimitsA
nation
1 Type 1 2 3 4
glass-fiber-reinforced glass-fiber-reinforced glass-fiber-reinforced glass-fiber-reinforced
thermosetting polyesterB resin thermosetting polyesterB resin thermosetting epoxy resin thermosetting epoxy resin
mortar (RPMP polyester)B (RTRP polyester)B mortar (RPMP epoxy) (RTRP epoxy)
2 Liner 1 2 3 4
reinforced thermoset liner non-reinforced thermoset liner thermoplastic liner no liner
3 Grade 1 2 3 4 5 6
Polyester resin polyesterB resin polyesterB resin and epoxy resin epoxy resin No surface
surface layer— surface layer— sand surface layer surface layer— surface layer— layer
reinforcedB nonreinforcedB nonreinforced reinforced nonreinforced
4 ClassC C50 C100 C150 C200 C250 C300 C350 C400 C450
5 Pipe Stiffness A B C D
psi (kPa) 9 (62) 18 (124) 36 (248) 72 (496)ABC
A
The cell-type format provides the means of identification and specification of piping materials. This cell-type format, however, is subject to misapplication since
unobtainable property combinations can be selected if the user is not familiar with commercially available products. The manufacturer should be consulted.
B
For the purposes of this standard, polyester includes vinyl ester resin.
C
Based on operating pressure in psig (numerals).

2.2 ISO Standard: 3.2.8 rigid joint—a joint that is not capable of axial dis-
ISO 1172 Textile Glass Reinforced Plastics—Determination placement or angular rotation.
of Loss on Ignition3
3.2.9 surface layer—a resin layer, with or without filler or
2.3 AWWA Standard: reinforcement, or both, applied to the exterior surface of the
AWWA C-950 Glass-Fiber Reinforced Thermosetting Resin pipe structural wall.
Pressure Pipe4

3. Terminology 4. Classification

3.1 Definitions: 4.1 General—This specification covers fiberglass sewer and


3.1.1 General—Definitions are in accordance with Termi- industrial pressure pipe defined by raw materials in the
nology D883 or Terminology F412 and abbreviations with structural wall (type) and liner, surface layer material (grade),
Terminology D1600, unless otherwise indicated. operating pressure (class), and pipe stiffness. Table 1 lists the
types, liners, grades, classes, and stiffnesses that are covered.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 fiberglass pipe—a tubular product containing glass NOTE 3—All possible combinations of types, liners, grades, classes, and
fiber reinforcements embedded in or surrounded by cured stiffness may not be commercially available. Additional types, liners,
thermosetting resin. The composite structure may contain grades, and stiffnesses may be added as they become commercially
aggregate, granular or platelet fillers, thixotropic agents, available. The purchaser should determine for himself or consult with the
manufacturer for the proper class, type, liner, grade, and stiffness of pipe
pigments, or dyes. Thermoplastic or thermosetting liners or to be used under the installation and operating conditions that will exist for
coatings may be included. the project in which the pipe is to be used.
3.2.2 flexible joint—a joint that is capable of axial displace- 4.2 Designation Requirements—The pipe materials designa-
ment or angular rotation, or both. tion code shall consist of the standard designation, ASTM
3.2.3 industrial pipe—pipe designed for internal, or external D3754, followed by type, liner, and grade in arabic numerals,
environments, or both, commonly encountered in industrial class by the letter C with two or three arabic numerals, and pipe
piping systems used for many process solutions or effluents. stiffness by a capital letter. Table 1 presents a summary of the
3.2.4 liner—a resin layer, with or without filler or designation requirements. Thus a complete material code shall
reinforcement, or both, forming the interior surface of the pipe. consist of ASTM D3754, three numerals, C...and two or three
3.2.5 qualification test—one or more tests used to prove the numerals, and a capital letter.
design of a product. Not a routine quality control test. NOTE 4—Examples of the designation codes are as follows: (1) ASTM
3.2.6 reinforced polymer mortar pipe—a fiberglass pipe D3754-1-1-3-C50-A for glass-fiber-reinforced aggregate and polyester
with aggregate. resin mortar pipe with a reinforced thermoset liner and an unreinforced
polyester resin and sand surface layer, for operation at 50 psi (345 kPa),
3.2.7 reinforced thermosetting resin pipe—a fiberglass pipe and having a minimum pipe stiffness of 9 psi (62 kPa). (2) ASTM
without aggregate. D3754-4-2-6-C200-C for glass-fiber-reinforced epoxy resin pipe with an
unreinforced thermoset liner, no surface layer, for operation at 200 psi
(1380 kPa) and having a minimum pipe stiffness of 36 psi (248 kPa).
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., NOTE 5—Although the “Form and Style for ASTM Standards” manual
4th Floor, New York, NY 10036, http://www.ansi.org. requires that the type classification be roman numerals, it is recognized
4
Available from American Water Works Association (AWWA), 6666 W. Quincy that few companies have stencil-cutting equipment for this style of type,
Ave., Denver, CO 80235, http://www.awwa.org. and it is therefore acceptable to mark the product type in arabic numbers.

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D3754 − 19
5. Materials and Manufacture 5.4.2.7 Mechanical Coupling, an elastomeric sealed cou-
5.1 General—The thermosetting resins, glass fiber pling with supplemental restraining elements.
reinforcements, fillers, and other materials, when combined as NOTE 6—Other types of joints may be added as they become commer-
a composite structure, shall produce piping products that meet cially available.
the performance requirements of this specification. NOTE 7—Restrained joints typically increase service loads on the pipe
to greater than those experienced with unrestrained joints. The purchaser
5.2 Wall Composition—The basic structural wall composi- is cautioned to take into consideration all conditions that may be
tion shall consist of a thermosetting resin, glass-fiber encountered in the anticipated service and to consult the manufacturer
reinforcement, and, if used, an aggregate filler. regarding the suitability of a particular type and class of pipe for service
5.2.1 Resin—A thermosetting polyester or epoxy resin, with with restrained joint systems.
or without filler. 5.5 Gaskets—Elastomeric gaskets, when used with this
5.2.2 Aggregate—A siliceous sand conforming to the re- pipe, shall conform to the requirements of Specification F477,
quirements of Specification C33, except that the requirements except that composition of the elastomer shall be as agreed
for gradation shall not apply. upon between the purchaser and the supplier for the particular
5.2.3 Reinforcement—A commercial grade of glass fibers exposure to oily or aggressive-chemical environments.
compatible with the resin used.
5.3 Liner and Surface Layers—A liner or surface layer, or 6. Requirements
both, when incorporated into or onto the pipe shall meet the 6.1 Workmanship:
chemical and structural requirements of this specification. 6.1.1 Each pipe shall be free from all defects including
5.4 Joints—The pipe shall have a joining system that shall indentations, delaminations, bubbles, pinholes, cracks, pits,
provide for fluid tightness for the intended service condition. A blisters, foreign inclusions, and resin-starved areas that due to
particular type of joint may be restrained or unrestrained and their nature, degree, or extent, detrimentally affect the strength
flexible or rigid depending on the specific configuration and and serviceability of the pipe. The pipe shall be as uniform as
design conditions. commercially practicable in color, opacity, density, and other
5.4.1 Unrestrained—Pipe joints capable of withstanding physical properties.
internal pressure but not longitudinal forces. 6.1.2 The inside surface of each pipe shall be free of bulges,
5.4.1.1 Coupling or Bell-and-Spigot Gasket Joints, with a dents, ridges, or other defects that result in a variation of inside
groove either on the spigot or in the bell to retain an diameter of more than 1⁄8 in. (3.2 mm) from that obtained on
elastomeric gasket that shall be the sole element of the joint to adjacent unaffected portions of the surface. No glass-fiber
provide watertightness. For typical joint details see Fig. 1. reinforcement shall penetrate the interior surface of the pipe
5.4.1.2 Mechanical Coupling Joint, with elsastomeric seals. wall.
5.4.1.3 Butt Joint, with laminated overlay 6.1.3 Joint sealing surfaces shall be free of dents, gouges, or
5.4.1.4 Flanged Joint, both integral and loose ring. other surface irregularities that will affect the integrity of the
5.4.2 Restrained—Pipe joints capable of withstanding inter- joints.
nal pressure and longitudinal tensile loads.
5.4.2.1 Joints similar to those in 5.4.1.1 with supplemental 6.2 Dimensions:
restraining elements. 6.2.1 Pipe Diameters—The pipe shall be supplied in the
5.4.2.2 Butt Joint, with laminated overlay. nominal diameters shown in Table 2 or Table 3. The pipe
5.4.2.3 Bell-and-Spigot, with laminated overlay. diameter tolerances shall be as shown in Table 2 or Table 3,
5.4.2.4 Bell-and-Spigot, adhesive-bonded-joint: Three types when measured in accordance with 8.1.1.
of adhesive-bonded joints are premitted by this standard as 6.2.2 Lengths—The pipe shall be supplied in nominal
follows: lengths of 10, 20, 30, 40, and 60 ft (3.05, 6.10, 9.15, 12.19, and
(1) Tapered bell-and-spigot, an adhesive joint that is manu- 18.29 m). The actual laying length shall be the nominal length
factured with a tapered socket for use in conjunction with a 62 in. (651 mm), when measured in accordance with 8.1.2. At
tapered spigot and a suitable adhesive. least 90 % of the total footage of any one size and class,
(2) Straight bell-and-spigot, an adhesive joint that is manu- excluding special-order lengths, shall be furnished in the
factured with an untapered socket for use in conjunction with nominal lengths specified by the purchaser. Random lengths, if
an untapered spigot and a suitable adhesive. furnished, shall not vary from the nominal lengths by more
(3) Tapered bell and straight spigot, an adhesive joint that than 5 ft (1.53 m), or 25 %, whichever is less.
is manufactured with a tapered socket for use with an unta- 6.2.3 Wall Thickness—The average wall thickness of the
pered spigot and a suitable adhesive. pipe shall not be less than the nominal wall thickness published
5.4.2.5 Flanged Joint, both integral and loose ring. in the manufacturer’s literature current at the time of purchase,
5.4.2.6 Threaded Joints. and the minimum wall thickness at any point shall not be less

FIG. 1 Typical Joints

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TABLE 2 Nominal Inside Diameters (ID) and Tolerances Inside Diameter Control Pipe
Nominal Nominal Metric ID Range,B mm ToleranceB on
Tolerances, in. Declared ID,
Diameter,A in. Diameter,B mm Minimum Maximum mm

8 ±0.25 200 196 204 ±1.5


10 ±0.25 250 246 255 ±1.5
12 ±0.25 300 296 306 ±1.8
14 ±0.25 400 396 408 ±2.4
15 ±0.25 500 496 510 ±3.0
16 ±0.25 600 595 612 ±3.6
18 ±0.25 700 695 714 ±4.2
20 ±0.25 800 795 816 ±4.2
21 ±0.25 900 895 918 ±4.2
24 ±0.25 1000 995 1020 ±5.0
27 ±0.27 1200 1195 1220 ±5.0
30 ±0.30 1400 1395 1420 ±5.0
33 ±0.33 1600 1595 1620 ±5.0
36 ±0.36 1800 1795 1820 ±5.0
39 ±0.39 2000 1995 2020 ±5.0
42 ±0.42 (2200) 2195 2220 ±6.0
45 ±0.45 2400 2395 2420 ±6.0
48 ±0.48 (2600) 2595 2620 ±6.0
51 ±0.51 2800 2795 2820 ±6.0
54 ±0.54 (3000) 2995 3020 ±6.0
60 ±0.60 3200 3195 3220 ±7.0
66 ±0.66 (3400) 3395 3420 ±7.0
72 ±0.72 3600 3595 3620 ±7.0
78 ±0.78 (3800) 3795 3820 ±7.0
84 ±0.84 4000 3995 4020 ±7.0
90 ±0.90 ... ... ... ...
96 ±0.96 ... ... ... ...
102 ±1.00 ... ... ... ...
108 ±1.00 ... ... ... ...
114 ±1.00 ... ... ... ...
120 ±1.00 ... ... ... ...
132 ±1.00 ... ... ... ...
144 ±1.00 ... ... ... ...
156 ±1.00 ... ... ... ...
A
Inside diameters other than those shown shall be permitted by agreement between purchaser and supplier.
B
Values are taken from International Standards Organization documents. Parentheses indicate non-preferred diameters.

than 87.5 % of the nominal wall thickness when measured in strain level must fall at or above the lower 95 % confidence
accordance with 8.1.3. limit of the originally determined regression line, b) no
6.2.4 Squareness of Pipe Ends—All points around each end specimen-failure times may be sooner than the lower 95 %
of a pipe unit shall fall within 61⁄4 in. (6.4 mm) or 60.5 % of prediction limit of the originally determined regression line,
the nominal diameter of the pipe, whichever is greater, to a and c) one-third or more of the specimen failure times must be
plane perpendicular to the longitudinal axis of the pipe, when on or above the originally determined regression line.
measured in accordance with 8.1.4.
NOTE 10—Determine the lower 95 % confidence limit and the lower
6.3 Chemical Requirements:
95 % prediction limit in accordance with to Annex A2.
6.3.1 Sanitary Sewer Service:
6.3.1.1 Long-Term—Pipe specimens, when tested in accor- 6.3.1.4 When the alternative method of 8.2.1.5 is used,
dance with 8.2.1 shall be capable of being deflected, without failure shall not occur in any specimen.
failure, at the 50 year strain level given in Table 4 when 6.3.2 Industrial Service—The resin component of the liner
exposed to 1.0 N sulfuric acid. or of the surface layer, or both, shall be a commercial-grade
NOTE 8—See Appendix X1 for derivation of the minimum sanitary corrosion-resistant thermoset that has either been evaluated in
sewer pipe chemical requirements given in Table 4. a laminate by test, in accordance with 8.2.2, or that has been
NOTE 9—The calculations in Table 4 and Appendix X1 assume that the determined by previous documented service to be acceptable
neutral axis is at the pipe wall midpoint. For pipe wall constructions that
produce an altered neutral axis position, it is necessary to evaluate results for the service conditions. Where service conditions have not
and establish requirements substituting 2y for t. (y is the maximum been evaluated, a suitable resin may also be selected by
distance from the neutral axis to the pipe surface.) agreement between the manufacturer and purchaser.
6.3.1.2 Control Requirements—Test pipe specimens peri-
NOTE 11—The results obtained by this test shall serve as a guide only
odically in accordance with 8.2.1.3, following the procedure of in the selection of a pipe material for a specific service application. The
8.2.1.4, or alternatively, the procedure of 8.2.1.5. purchaser is cautioned to evaluate all of the various factors that may enter
6.3.1.3 When the procedure of 8.2.1.4 is used, the following into the serviceability of a pipe material when subjected to chemical
three criteria must be met: a) the average failure time at each environment, including chemical resistance in the strained condition.

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TABLE 3 Nominal Outside Diameters (OD) and Tolerances
NOTE 1—The external diameter of the pipe at the spigots shall be within the tolerances given in the table, and the manufacturer shall declare his
allowable maximum and minimum spigot diameters. Some pipes are manufactured such that the entire pipe meets the OD tolerances while other pipes
meet the tolerances at the spigots, in which case, if such pipes are cut (shortened) the ends may need to be calibrated to meet the tolerances.

Metric Ductile Iron Pipe Tolerance Upper, Tolerance Lower, International O.D., Tolerance Upper, Tolerance Lower,
Pipe Size, mm Equivalent, mm mm mm mm mm mm
200 220.0 +1.0 0.0 ... ... ...
250 271.8 +1.0 -0.2 ... ... ...
300 323.8 +1.0 -0.3 310 +1.0 -1.0
350 375.7 +1.0 -0.3 361 +1.0 -1.2
400 426.6 +1.0 -0.3 412 +1.0 -1.4
450 477.6 +1.0 -0.4 463 +1.0 -1.6
500 529.5 +1.0 -0.4 514 +1.0 -1.8
600 632.5 +1.0 -0.5 616 +1.0 -2.0
700 718 +1.0 -2.2
800 820 +1.0 -2.4
900 924 +1.0 -2.6
1000 1026 +2.0 -2.6
1200 1229 +2.0 -2.6
1400 1434 +2.0 -2.8
1600 1638 +2.0 -2.8
1800 1842 +2.0 -3.0
2000 2046 +2.0 -3.0
2200 2250 +2.0 -3.2
2400 2453 +2.0 -3.4
2600 2658 +2.0 -3.6
2800 2861 +2.0 -3.8
3000 3066 +2.0 -4.0
3200 3270 +2.0 -4.2
3400 3474 +2.0 -4.4
3600 3678 +2.0 -4.6
3800 3882 +2.0 -4.8
4000 4086 +2.0 -5.0

TABLE 4 Minimum Sanitary Sewer Pipe Chemical Requirements


εscv
Pipe Stiffness, Minimum Strain
psi (kPa) 6 min 10 h 100 h 1 000 10 000 50 years
9 (62) 0.97 (t/de) 0.84 (t/d) 0.78 (t/d) 0.73 (t/d) 0.68 (t/d) 0.60 (t/d)
18 (124) 0.85 (t/d) 0.72 (t/d) 0.66 (t/d) 0.61 (t/d) 0.56 (t/d) 0.49 (t/d)
36 (248) 0.71 (t/d) 0.60 (t/d) 0.55 (t/d) 0.51 (t/d) 0.47 (t/d) 0.41 (t/d)
72 (496) 0.56 (t/d) 0.48 (t/d) 0.44 (t/d) 0.41 (t/d) 0.38 (t/d) 0.34 (t/d)

Where: t and d are the nominal total wall thickness and the mean diameter (inside diameter plus t) as determined in accordance with 8.1.

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6.4 Soundness—Unless otherwise agreed upon between pur- TABLE 6 Long-Term Hydrostatic Pressure Categories
chaser and supplier, test each length of pipe up to 96 in. (2400 Minimum Calculated Values of
mm) diameter hydrostatically without leakage or cracking, at Class Long-Term Hydrostatic
Pressure gage, psi (kPa)
the internal hydrostatic proof pressures specified for the
C50 90 (621)
applicable class in Table 5 when tested in accordance with 8.3. C100 180 (1241)
For sizes over 96 in. (2400 mm), the frequency of hydrostatic C150 270 (1862)
leak tests shall be as agreed upon by purchaser and supplier. C200 360 (2482)
C250 450 (3103)
6.5 Hydrostatic Design Basis: C300 540 (3722)
C350 630 (4343)
6.5.1 Long-Term Hydrostatic Pressure—The pressure C400 720 (4963)
classes shall be based on long-term hydrostatic pressure data C450 810 (5584)
obtained in accordance with 8.4 and categorized in accordance
with Table 6. Pressure classes are based on extrapolated
TABLE 7 Minimum Stiffness at 5 % Deflection
strengths at 50 years. For pipe subjected to longitudinal loads
or circumferential bending, the effect of these conditions on the Nominal Pipe Stiffness, psi (kPa)
Diameter, Designation
hydrostatic design pressure classification of the pipe must be in. A B C D
considered.
6.5.2 Control Requirements—Test pipe specimens periodi- 8 ... ... 36 (248) 72 (496)
cally in accordance with the reconfirmation procedures de- 10 ... 18 (124) 36 (248) 72 (496)
12 and greater 9 (62) 18 (124) 36 (248) 72 (496)
scribed in Practice D2992.
NOTE 12—Hydrostatic design basis (HDB—extrapolated value at 50
years) determined in accordance with Procedure A of Practice D2992, may TABLE 8 Ring Deflection Without Damage or Structural Failure
be substituted for the Procedure B evaluation required by 8.4. It is Nominal Pipe Stiffness, psi
generally accepted that the Procedure A value multiplied by 3 is equivalent
9 18 36 72
to the Procedure B value.
6.6 Stiffness—Each length of pipe shall have sufficient Level A 18 % 15 % 12 % 9%
strength to exhibit the minimum pipe stiffness (F/∆y) specified Level B 30 % 25 % 20 % 15 %
in Table 7 when tested in accordance with 8.5. At deflection
level A per Table 8, there shall be no visible damage in the test
specimen evidenced by surface cracks. At deflection level B 6.6.1 For other pipe stiffness levels, appropriate values for
per Table 8, there shall be no indication of structural damage as Level A and Level B deflections (Table 8) may be computed as
evidenced by interlaminar separation, separation of the liner or follows:
surface layer (if incorporated) from the structural wall, tensile
failure of the glass-fiber reinforcement, fracture, or buckling of Level A at new PS 5 S 72
new PS D 0.33

~9! (1)
the pipe wall.
Level B at new PS 5 new Level A÷0.6
NOTE 13—This is a visual observation (made with the unaided eye) for
6.6.2 Since products may have use limits of other than 5 %
quality control purposes only, and should not be considered a simulated
service test. Table 8 values are based on an in-use long-term deflection long-term deflection, Level A and Level B deflections (Table 8)
limit of 5 % and provide an appropriate uniform safety margin for all pipe may be proportionally adjusted to maintain equivalent in-use
stiffnesses. Since the pipe-stiffness values (F/∆y) shown in Table 7 vary, safety margins. For example, a 4 % long-term limiting deflec-
the percent deflection of the pipe under a given set of installation tion would result in a 20 % reduction of Level A and Level B
conditions will not be constant for all pipes. To avoid possible
misapplication, take care to analyze all conditions that might affect
deflections, while a 6 % limiting deflection would result in a
performance of the installed pipe. 20 % increase in Level A and Level B deflection values.
However, minimum values for Level A and Level B deflections
shall be equivalent to strains of 0.6 and 1.0 % respectively (as
computed by Eq X1.1 in Appendix X1).
TABLE 5 Hydrostatic Pressure Test 6.6.3 For high stiffness pipes, 5% deflection will likely be
above the use limit and the adjusted level A test deflection. For
Pressure Hydrostatic Proof Pressure
Class Pipe Diameters Pipe Diameters very high stiffness pipes, 5% deflection may also be greater
up to and >54 in. up to and than the adjusted level B test deflection. In such cases, the
including 54 in. including 96 in.
pipes may be damaged or fail prior to determining the pipe
(psi) psi (kPa) psi (kPa)
C50 100 (689) 75 (517) stiffness at 5% deflection. Therefore, it is permitted to set the
C100 200 (1379) 150 (1034) pipe stiffness test deflection equal to the adjusted level A
C150 300 (2068) 225 (1551)
C200 400 (2757) 300 (2068)
deflection, but not greater than 5%. See Note 14 for additional
C250 500 (3447) 375 (2585) information and further clarification.
C300 600 (4136) 450 (3102)
C350 700 (4826) 525 (3619) NOTE 14—Depending upon the product modulus and allowable ring
C400 800 (5515) 600 (4136) bending strain, this will likely begin affecting pipes with stiffness between
C450 900 (6205) 675 (4654) 200 and 400 psi. For example, a pipe with pipe stiffness of PS360 may
have a use limit of 4.3 %, an adjusted level A deflection of 4.5 % and an

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adjusted level B deflection of 7.5 %. Therefore, the new pipe stiffness test 6.9.1 Beam Strength—For pipe sizes up to 27 in. (686 mm),
deflection would be 4.5 %. Another possible product with pipe stiffness of the pipe shall withstand, without failure, the beam loads
PS900 may have a use limit of 2.8 %, an adjusted level A deflection of
2.7% and an adjusted level B deflection of 4.5 %. Therefore, the new pipe
specified in Table 11, when tested in accordance with 8.7.1. For
stiffness test deflection would be 2.7 %. pipe sizes larger than 27 in., and alternatively for smaller sizes,
adequate beam strength is demonstrated by tensile and com-
6.7 Hoop-Tensile Strength—All pipe manufactured under
pression tests conducted in accordance with 8.7.2 and 8.7.3
this specification shall meet or exceed the hoop-tensile strength
respectively, for pipe wall specimens oriented in the longitu-
shown for each size and class in Table 9 and Table 10, when
dinal direction, using the minimum tensile and compression
tested in accordance with 8.6.
strengths specified in Table 11.
6.7.1 Alternative Requirements—When agreed upon by the
6.9.2 Longitudinal Tensile Strength—All pipe manufactured
purchaser and the supplier, the minimum hoop tensile strength
under this specification shall have a minimum axial tensile
shall be as determined in accordance with 8.6.1.
elongation at failure of 0.25% and meet or exceed the longi-
6.8 Joint Tightness—All joints shall meet the laboratory tudinal tensile strength shown for each size and class in Table
performance requirements of Specification D4161. Unre- 12 and Table 13, when tested in accordance with 8.7.2.
strained joints shall be tested with a fixed end closure condition
NOTE 15—The values listed in Table 12 are the minimum criteria for
and restrained joints shall be tested with a free end closure
products made to this standard. The values may not be indicative of the
condition. Rigid joints shall be exempt from angular deflection axial strength of some products, or of the axial strength required by some
requirements of D4161. Rigid joints typically include butt installation conditions and joint configurations.
joints with laminated overlay, bell-and-spigot joints with lami- 6.9.3 Conformance to the requirements of 6.9.1 shall satisfy
nated overlay, flanged, bell-and-spigot adhesive bonded and the requirements of 6.9.2 for those pipe sizes and classes where
threaded. the minimum longitudinal tensile strength values of Table 11
6.9 Longitudinal Strength: are equal to the values of Table 12. Conformance to the

TABLE 9 Minimum Hoop Tensile Strength of Pipe Wall


NOTE 1—The values in this table are equal to 2PD, where P is the pressure class in psi and D is the nominal diameter in inches.
Inch-Pound Units
Hoop Tensile Strength, lbf/in. Width
Nominal
Pressure Class
Diameter
(in.) C50 C100 C150 C200 C250 C300 C350 C400 C450
(psi) (psi) (psi) (psi) (psi) (psi) (psi) (psi) (psi)
8 800 1600 2400 3200 4000 4800 5600 6400 7200
10 1000 2000 3000 4000 5000 6000 7000 8000 9000
12 1200 2400 3600 4800 6000 7200 8400 9600 10 800
14 1400 2800 4200 5600 7000 8400 9800 11 200 12 600
15 1500 3000 4500 6000 7500 9000 10 500 12 000 13 500
16 1600 3200 4800 6400 8000 9600 11 200 12 800 14 400
18 1800 3600 5400 7200 9000 10 800 12 600 14 400 16 200
20 2000 4000 6000 8000 10 000 12 000 14 000 16 000 18 000
21 2100 4200 6300 8400 10 500 12 600 14 700 16 800 18 900
24 2400 4800 7200 9600 12 000 14 400 16 800 19 200 21 600
27 2700 5400 8100 10 800 13 500 16 200 18 900 21 600 24 300
30 3000 6000 9000 12 000 15 000 18 000 21 000 24 000 27 000
33 3300 6600 9900 13 200 16 500 19 800 23 100 26 400 29 700
36 3600 7200 10 800 14 400 18 000 21 600 25 200 28 800 32 400
39 3900 7800 11 700 15 600 19 500 23 400 27 300 31 200 35 100
42 4200 8400 12 600 16 800 21 000 25 200 29 400 33 600 37 800
45 4500 9000 13 500 18 000 22 500 27 000 31 500 36 000 40 500
48 4800 9600 14 400 19 200 24 000 28 800 33 600 38 400 43 200
51 5100 10 200 15 300 20 400 25 500 30 600 35 700 40 800 45 900
54 5400 10 800 16 200 21 600 27 000 32 400 37 800 43 200 48 600
60 6000 12 000 18 000 24 000 30 000 36 000 42 000 48 000 54 000
66 6600 13 200 19 800 26 400 33 000 39 600 46 200 52 800 59 400
72 7200 14 400 21 600 28 800 36 000 43 200 50 400 57 600 64 800
78 7800 15 600 23 400 31 200 39 000 46 800 54 600 62 400 70 200
84 8400 16 800 25 200 33 600 42 000 50 400 58 800 67 200 75 600
90 9000 18 000 27 000 36 000 45 000 54 000 63 000 72 000 81 000
96 9600 19 200 28 800 38 400 48 000 57 600 67 200 76 800 86 400
102 10 200 20 400 30 600 40 800 51 000 61 200 71 400 81 600 91 800
108 10 800 21 600 32 400 43 200 54 000 64 800 75 600 86 400 97 200
114 11 400 22 800 34 200 45 600 57 000 68 400 79 800 91 200 10 2600
120 12 000 24 000 36 000 48 000 60 000 72 000 84 000 96 000 108 000
132 13 200 26 400 39 600 52 800 66 000 79 200 92 400 105 600 118 800
144 14 400 28 800 43 200 57 600 72 000 86 400 100 800 115 200 129 600
156 15 600 31 200 46 800 62 400 78 000 93 600 109 200 124 800 140 400

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TABLE 10 Minimum Hoop Tensile Strength of Pipe Wall
SI Units
Hoop Tensile Strength N/mm Width
Pressure
C50 C100 C150 C200 C250 C300 C350 C400 C450
Class
Nominal
345 689 1034 1379 1724 2069 2414 2759 3103
Diameter
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa)
(mm)
200 138 276 414 552 690 828 966 1104 1241
250 173 345 517 690 862 1035 1207 1380 1552
300 207 413 620 827 1034 1241 1448 1655 1862
350 242 482 724 965 1207 1448 1690 1931 2172
375 259 517 776 1034 1293 1552 1811 2069 2327
400 276 551 827 1103 1379 1655 1931 2207 2482
450 311 620 931 1241 1552 1862 2173 2483 2793
500 345 689 1034 1379 1724 2069 2414 2759 3103
550 380 758 1137 1517 1896 2276 2655 3035 3413
600 414 827 1241 1655 2069 2483 2897 3311 3724
700 483 965 1448 1931 2414 2897 3380 3863 4344
750 518 1034 1551 2069 2586 3104 3621 4139 4655
850 587 1171 1758 2344 2931 3517 4104 4690 5275
900 621 1240 1861 2482 3103 3724 4345 4966 5585
1000 690 1378 2068 2758 3448 4138 4828 5518 6206
1100 759 1516 2275 3034 3793 4552 5311 6070 6827
1150 794 1585 2378 3172 3965 4759 5552 6346 7137
1200 828 1654 2482 3310 4138 4966 5794 6622 7447
1300 897 1791 2688 3585 4482 5379 6276 7173 8068
1400 966 1929 2895 3861 4827 5793 6759 7725 8688
1500 1035 2067 3102 4137 5172 6207 7242 8277 9309
1700 1173 2343 3516 4689 5862 7035 8208 9381 10 550
1800 1242 2480 3722 4964 6206 7448 8690 9932 11 171
2000 1380 2756 4136 5516 6896 8276 9656 11 036 12 412
2200 1518 3032 4550 6068 7586 9104 10 622 12 140 13 653
2300 1587 3169 4756 6343 7930 9517 11 104 12 691 14 274
2400 1656 3307 4963 6619 8275 9931 11 587 13 243 14 894
2600 1794 3583 5377 7171 8965 10 759 12 553 14 347 16 136
2800 1932 3858 5790 7722 9654 11 586 13 518 15 450 17 377
2900 2001 3996 5997 7998 9999 12 000 14 001 16 002 17 997
3000 2070 4134 6204 8274 10 344 12 414 14 484 16 554 18 618
3400 2346 4685 7031 9377 11 723 14 069 16 415 18 761 21 100
3600 2484 4961 7445 9929 12 413 14 897 17 381 19 865 22 342
4000 2760 5512 8272 11 032 13 792 16 552 19 312 22 072 24 824

requirements of 6.9.2 shall satisfy the longitudinal tensile basis of acceptance for this test as agreed upon by the
strength requirements of 6.9.1. purchaser and the supplier.
7.3.3 Long-term hydrostatic pressure test.
7. Sampling
7.3.4 Joint-tightness test, see 6.8.
7.1 Lot—Unless otherwise agreed upon by the purchaser 7.3.5 Longitudinal strength test, including:
and the supplier, one lot shall consist of 100 lengths of each
type, grade, and size of pipe produced. 7.3.5.1 Beam strength, and
7.3.5.2 Longitudinal tensile strength.
7.2 Production Tests—Select one pipe at random from each
lot and take one specimen from the pipe barrel to determine 7.4 Control Tests—The following tests are considered con-
conformance of the material to the workmanship, dimensional, trol requirements and shall be performed as agreed upon
and strength requirements of 6.1, 6.2, 6.6, and 6.7 respectively. between the purchaser and the supplier.
Unless otherwise agreed upon between purchaser and supplier, 7.4.1 Soundness Test—102 in. (2600 mm) diameter pipe and
all pipes (up to 54 in. diameter) shall meet the soundness larger.
requirements of 6.4.
7.4.2 Perform sampling and testing for the control require-
7.3 Qualification Tests—Sampling for qualification tests is ments for sanitary sewer service at least once annually.
not required unless otherwise agreed upon by the purchaser and 7.4.3 Perform sampling and testing for the control require-
the supplier. Qualification tests, for which a certification and ments for hydrostatic design basis at least once every two
test report shall be furnished when requested by the purchaser, years.
include the following:
7.3.1 Sanitary sewer service, long-term chemical test. 7.5 For individual orders, conduct only those additional
7.3.2 Industrial service resin component chemical test. A tests and number of tests specifically agreed upon between
copy of the resin manufacturer’s test report may be used as the purchaser and supplier.

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D3754 − 19
TABLE 11 Beam Strength Test Loads
Nominal Minimum Longitudinal Tensile Strength, Minimum Longitudinal Compressive Strength,
Beam Load, P,
Diameter, per Unit of Circumference per Unit of Circumference
in. lbf (kN) lbf/in. (kN/m) lbf/in. (kN/m)
8 800 (3.6) 580 (102) 580 (102)
10 1200 (5.3) 580 (102) 580 (102)
12 1600 (7.1) 580 (102) 580 (102)
14 2200 (9.8) 580 (102) 580 (102)
15 2600 (11.6) 580 (102) 580 (102)
16 3000 (13.3) 580 (102) 580 (102)
18 4000 (17.8) 580 (102) 580 (102)
20 4400 (19.6) 580 (102) 580 (102)
21 5000 (22.2) 580 (102) 580 (102)
24 6400 (28.5) 580 (102) 580 (102)
27 8000 (35.6) 580 (102) 580 (102)
30 ... ... 580 (102) 580 (102)
33 ... ... 640 (111) 640 (111)
36 ... ... 700 (122) 700 (122)
39 ... ... 780 (137) 780 (137)
42 ... ... 800 (140) 800 (140)
45 ... ... 860 (150) 860 (150)
48 ... ... 920 (161) 920 (161)
51 ... ... 980 (171) 980 (171)
54 ... ... 1040 (182) 1040 (182)
60 ... ... 1140 (200) 1140 (200)
66 ... ... 1260 (220) 1260 (220)
72 ... ... 1360 (238) 1360 (238)
78 ... ... 1480 (260) 1480 (260)
84 ... ... 1600 (280) 1600 (280)
90 ... ... 1720 (301) 1720 (301)
96 ... ... 1840 (322) 1840 (322)
102 ... ... 1940 (340) 1940 (340)
108 ... ... 2060 (360) 2060 (360)
114 ... ... 2180 (382) 2180 (382)
120 ... ... 2280 (400) 2280 (400)
132 ... ... 2520 (440) 2520 (440)
144 ... ... 2740 (480) 2740 (480)
156 ... ... 2964 (519) 2964 (519)

8. Test Methods 8.2.1 Sanitary-Sewer Service—Test the pipe in accordance


8.1 Dimensions: with Test Method D3681.
8.1.1 Diameters: 8.2.1.1 Long-Term—To find if the pipe meets the require-
8.1.1.1 Inside Diameter—Take inside diameter measure- ments of 6.3.1, determine at least 18 failure points in accor-
ments at a point approximately 6 in. (152 mm) from the end of dance with Test Method D3681.
the pipe section using a steel tape or an inside micrometer with 8.2.1.2 Alternative Qualification Procedure—Test four
graduations of 1⁄16 in. (1 mm) or less. Take two 90° opposing specimens each at the 10 and 10 000 h minimum strains given
measurements at each point of measurement and average the in Table 4 and test five specimens each at the 100 and 1000 h
readings. minimum strains given in Table 4. Consider the product
8.1.1.2 Outside Diameter—Determine in accordance with qualified if all 18 specimens are tested without failure for at
Test Method D3567. least the prescribed times given in Table 4 (that is, 10, 100,
8.1.2 Length—Measure with a steel tape or gage having 1000 or 10 000 h respectively).
graduations of 1⁄16 in. (1 mm) or less. Lay the tape or gage on 8.2.1.3 Control Requirements—Test at least six specimens
or inside the pipe and measure the overall laying length of the in accordance with one of the following procedures and record
pipe. the results.
8.1.3 Wall Thickness—Determine in accordance with Test 8.2.1.4 Test at least 3 specimens at each of the strain levels
Method D3567. corresponding to the 100- and 1000-h failure times from the
8.1.4 Squareness of Pipe Ends—Rotate the pipe on a man- product’s regression line established in 8.2.1.
drel or trunions and measure the runout of the ends with a dial 8.2.1.5 When the alternative method described in 8.2.1.2 is
indicator. The total indicated reading is equal to twice the used to qualify the product, test at least three specimens each
distance from a plane perpendicular to the longitudinal axis of at the 100 and 1000 h minimum strains given in Table 4 for at
the pipe. Alternatively, when the squareness of the pipe ends is least 100 and 1000 h respectively.
rigidly fixed by tooling, the tooling may be verified and 8.2.1.6 The control test procedures of 8.2.1.5 may be used
reinspected at intervals frequent enough to assure that the as an alternative procedure to the reconfirmation procedure
squareness of the pipe ends is maintained within tolerance. described in Test Method D3681 for those products evaluated
8.2 Chemical Tests: by the alternative qualification procedure described in 8.2.1.2.

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TABLE 12 Longitudinal Tensile Strength of Pipe Wall
Inch-Pound Units
Longitudinal Tensile Strength lbf/in. of Circumference
Nominal
Pressure Class
Diameter
(in.) C50 C100 C150 C200 C250 C300 C350 C400 C450
(psi) (psi) (psi) (psi) (psi) (psi) (psi) (psi) (psi)
8 580 580 580 580 580 624 700 800 900
10 580 580 580 580 650 780 875 1000 1125
12 580 580 580 624 780 936 1050 1200 1350
14 580 580 609 728 910 1092 1225 1400 1575
15 580 580 653 780 975 1170 1313 1500 1688
16 580 580 696 832 1040 1248 1400 1600 1800
18 580 580 783 936 1170 1404 1575 1800 2025
20 580 580 870 1040 1300 1560 1750 2000 2250
21 580 609 914 1092 1365 1638 1838 2100 2363
24 580 696 1044 1248 1560 1800 2100 2400 2700
27 580 783 1175 1404 1688 2025 2363 2700 3038
30 580 870 1305 1560 1875 2250 2625 3000 3375
33 627 957 1436 1716 2063 2475 2888 3300 3713
36 684 1044 1566 1800 2250 2700 3150 3600 4050
39 741 1131 1697 1872 2340 2808 3276 3744 4212
42 798 1218 1827 2016 2520 3024 3528 4032 4536
45 855 1305 1958 2160 2700 3240 3780 4320 4860
48 912 1392 2088 2304 2880 3456 4032 4608 5184
51 969 1479 2219 2448 3060 3672 4284 4896 5508
54 1026 1566 2349 2592 3240 3726 4347 4968 5589
60 1140 1740 2520 2880 3600 4140 4830 5520 6210
66 1254 1914 2673 3036 3795 4554 5313 5808 6534
72 1368 2088 2916 3312 4140 4968 5796 6336 7128
78 1482 2106 3159 3432 4290 5148 6006 6864 7722
84 1596 2268 3402 3696 4620 5292 6174 7056 7938
90 1710 2430 3645 3960 4950 5670 6615 7380 8303
96 1824 2592 3888 4224 5280 6048 7056 7680 8640
102 1938 2754 4131 4488 5610 6426 7497 8160 9180
108 2052 2916 4374 4752 5940 6804 7938 8640 9720
114 2166 3078 4617 5016 6270 7182 8379 9120 10 260
120 2280 3240 4860 5280 6600 7560 8820 9600 10 800
132 2508 3564 5346 5808 7260 8316 9702 10 560 11 880
144 2736 3888 5832 6336 7920 9072 10 584 11 520 12 960
156 2964 4212 6318 6864 8580 9828 11 466 12 480 14 040

8.2.2 Industrial Service—The resin component of the liner 8.4.2 Determine the hydrostatic design basis for the glass-
or of the surface layer, or both, to be subjected to an aggressive fiber reinforcement in accordance with the method in Annex
service environment, shall be tested in accordance with Test A1.
Method C581, except that the specimens tested shall be 8.4.3 Calculate the long-term hydrostatic pressure and cat-
representative of the laminate construction used in the liner or egorize by class in accordance with Table 6. Annex A1.6
surface layer, or both. explains how to calculate the long-term hydrostatic pressure.
8.3 Soundness—Determine soundness by a hydrostatic 8.5 Stiffness—Determine the pipe stiffness (F/∆y) at 5 %
proof test procedure. Place the pipe in a hydrostatic pressure deflection or the adjusted level determined in accordance with
testing machine that seals the ends and exerts no end loads. Fill 6.6.3 for the specimen, using the apparatus and procedure of
the pipe with water, expelling all air, and apply internal water Test Method D2412, with the following exceptions permitted:
pressure at a uniform rate not to exceed 50 psi (345 kPa)/s until
8.5.1 Measure the wall thickness to the nearest 0.01 in.
the test pressure shown in Table 5 for the applicable class is
(0.25 mm).
reached. Maintain this pressure for a minimum of 30 s. The
pipe shall show no visual signs of weeping, leakage, or fracture 8.5.2 Load the specimen to 5 % deflection or the adjusted
of the structural wall. level determined in accordance with 6.6.3 and record the load.
Then load the specimen to deflection level A per Table 8 or to
8.4 Long-Term Hydrostatic Pressure—Determine the long- the adjusted level A determined in accordance with 6.6.1 and
term hydrostatic pressure at 50 years in accordance with 6.6.2 and examine the specimen for visible damage evidenced
Procedure B of Practice D2992, with the following exceptions by surface cracks. Then load the specimen to deflection level B
permitted: per Table 8 or to the adjusted level B determined in accordance
8.4.1 Test at ambient temperatures within the limits of 50°F with 6.6.1 and 6.6.2 and examine for evidence of structural
(10°C) and 110°F (43.5°C) and report the temperature range damage, as evidenced by interlaminar separation, separation of
experienced during the tests. the liner or surface layer (if incorporated) from the structural
NOTE 16—Tests indicate no significant effects on long-term hydrostatic wall, tensile failure of the glass-fiber reinforcement, fracture,
pressure within the ambient temperature range specified. or buckling of the pipe wall. Calculate the pipe stiffness at 5 %

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TABLE 13 Longitudinal Tensile Strength of Pipe Wall
SI Units
Longitudinal Tensile Strength N/mm of Circumference
Pressure
C50 C100 C150 C200 C250 C300 C350 C400 C450
Class
Nominal
345 689 1034 1379 1724 2069 2414 2759 3103
Diameter
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) (kPa)
(mm)
200 102 102 102 102 102 109 123 140 158
250 102 102 102 102 114 137 153 175 197
300 102 102 102 109 137 164 184 210 236
350 102 102 107 127 159 191 215 245 276
375 102 102 114 137 171 205 230 263 296
400 102 102 122 146 182 219 245 280 315
450 102 102 137 164 205 246 276 315 355
500 102 102 152 182 228 273 306 350 394
550 102 107 160 191 239 287 322 368 414
600 102 122 183 219 273 315 368 420 473
700 102 137 206 246 296 355 414 473 532
750 102 152 229 273 328 394 460 525 591
850 110 168 251 301 361 433 506 578 650
900 120 183 274 315 394 473 552 630 709
1000 130 198 297 328 410 492 574 656 738
1100 140 213 320 353 441 530 618 706 794
1150 150 229 343 378 473 567 662 757 851
1200 160 244 366 403 504 605 706 807 908
1300 170 259 388 429 536 643 750 857 965
1400 180 274 411 454 567 652 761 870 979
1500 200 305 441 504 630 725 846 967 1087
1700 220 335 468 532 665 797 930 1017 1144
1800 240 366 511 580 725 870 1015 1110 1248
2000 260 369 553 601 751 902 1052 1202 1352
2200 279 397 596 647 809 927 1081 1236 1390
2300 299 426 638 693 867 993 1158 1292 1454
2400 319 454 681 740 925 1059 1236 1345 1513
2600 339 482 723 786 982 1125 1313 1429 1608
2800 359 511 766 832 1040 1192 1390 1513 1702
2900 379 539 809 878 1098 1258 1467 1597 1797
3000 399 567 851 925 1156 1324 1545 1681 1891
3400 439 624 936 1017 1271 1456 1699 1849 2080
3600 479 681 1021 1110 1387 1589 1853 2017 2270
4000 519 738 1106 1202 1503 1721 2008 2185 2459

deflection or at the adjusted test deflection level determined in determine the specimen width as close to the break as possible.
accordance with 6.6.3. Use the measured width and failure load to calculate the
8.5.3 For production testing, only one specimen need be hoop-tensile strength.
tested to determine the pipe stiffness. 8.6.1 Alternative Minimum Hoop-Tensile Strength
8.5.4 The maximum specimen length may be 12 in. (305 Requirement—As an alternative, the minimum hoop-tensile
mm), or the length necessary to include stiffening ribs if they strength values may be determined through the use of the
are used, whichever is greater. following formula:
NOTE 17—As an alternative to determining pipe stiffness using the F 5 ~ S i /S r ! ~ P r ! (2)
apparatus and procedure of Test Method D2412, the supplier may submit
to the purchaser for approval a test method and test evaluation based on where:
Test Method D790 accounting for the substitution of curved test speci-
mens and measurement of stiffness at 5 % deflection or at the adjusted test F = required minimum hoop-tensile strength, lbf/in.,
deflection level determined in accordance with 6.6.3. Si = initial design hoop tensile stress, psi,
Sr = hoop tensile stress at rated operating pressure, psi,
8.6 Hoop-Tensile Strength—Determine hoop tensile P = rated operating pressure class, psi, and
strength by Test Method D2290, except that the sections on r = inside radius of pipe, in.
apparatus and test specimens may be modified to suit the size
of the specimens to be tested, and the maximum load rate may The value for Si should be established by considering the
not exceed 0.10 in./min (2.54 mm/min). Alternatively, Test variations in glass reinforcement strength and manufacturing
Method D638 may be employed. Specimen width may be methods, but in any case, should not be less than the 95 %
increased for pipe wall thickness greater than 0.55 in (13.97 lower confidence value on stress at 0.1 h, as determined by the
mm). Means may be provided to minimize the bending manufacturer’s testing carried out in accordance with 6.5. The
moment imposed during the test. Three specimens shall be cut value for Sr should be established from the manufacturer’s
from the test sample. Record the load to fail each specimen and hydrostatic design basis.

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NOTE 18—A value of F less than 4 Pr results in a lower factor of safety in letters not less than 1⁄2 in. (12 mm) in height and of bold-type
on short term loading than required by the values in Table 9. style in a color and type that remains legible under normal
8.7 Longitudinal Strength: handling and installation procedures. Include in the marking
8.7.1 Beam Strength—Place a 20-ft (6.1-m) nominal length the nominal pipe size, manufacturer’s name or trademark,
of pipe on saddles at each end. Hold the ends of the pipe round ASTM Specification number D3754, type, liner, grade, class,
during the test. Apply the beam load for the diameter of pipe and stiffness in accordance with the designation code in 4.2.
shown in Table 11 simultaneously to the pipe through two
saddles located at the third points of the pipe (see Fig. 2). 9.2 Prepare pipe for commercial shipment in such a way as
Maintain the loads for not less than 10 min with no evidence of to ensure acceptance by common or other carriers.
failure. The testing apparatus shall be designed to minimize 9.3 All packing, packaging, and marking provisions of
stress concentrations at the loading points. Practice D3892 shall apply to this specification.
8.7.2 Longitudinal Tensile Strength—Determine in accor-
dance with Test Method D638, except the provisions for
10. Keywords
maximum thickness shall not apply.
8.7.3 Longitudinal Compressive Strength—Determine in ac- 10.1 fiberglass pipe; sewer pipe; industrial pipe; pressure
cordance with Test Method D695. pipe; strain corrosion; hydrostatic design basis

9. Packaging, Marking, and Shipping


9.1 Mark each length of pipe that meets or is part of a lot
that meets the requirements of this specification at least once,

ANNEXES

(Mandatory Information)

A1. ALTERNATIVE HYDROSTATIC DESIGN METHOD

A1.1 The following symbols are used: circumferential (hoop) orientation that will cause failure after
S = tensile stress in the glass-fiber reinforcement in 50 years of continuously applied pressure, as described in 8.4
the hoop orientation corrected for the helix angle, psi, and Practice D2992, Procedure B. Strength requirements are
P = internal pressure, psig, calculated using the strength of hoop-oriented glass reinforce-
Pl = long-term hydrostatic pressure, psig, ments only, corrected for the helix angle of the fibers.
D = nominal inside pipe diameter, in.,
th = actual cross-sectional area of glass-fiber rein- A1.3 Hoop-Stress Calculation, derived from the ISO for-
forcement applied around the circumference of the pipe, mula for hoop stress, is as follows:
in.2/in.,
S 5 PD/2 ~ t h sinθ !
θ = plane angle between hoop-oriented reinforcement
and longitudinal axis of the pipe (helix angle), and This stress is used as the ordinate (long-term strength) in
HDB = hydrostatic design basis, psi. calculating the regression line and lower confidence limit in
accordance with Practice D2992, Annexes A1 and A3.
A1.2 The hydrostatic design is based on the estimated NOTE A1.1—The calculated result for S may be multiplied by the factor
tensile stress of reinforcement in the wall of the pipe in the 6.985 to convert from psi to kPa.

FIG. 2 Beam Strength-Test Setup

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TABLE A1.1 Long-Term Hydrostatic Pressure Categories NOTE A1.2—The calculated result P1 may be multiplied by the factor
Minimum Calculated Values of 6.895 to convert from psig to kPa.
Class Long-Term Hydrostatic
Pressure gage, psi (kPa) A1.6 Pressure Class Rating—The classes shown in Table
C50 90 (621) A1.1 are based on the intended working pressure in psig for
C100 180 (1241) commonly encountered conditions of water service. The pur-
C150 270 (1862)
C200 360 (2482)
chaser should determine the class of pipe most suitable to the
C250 450 (3103) installation and operating conditions that will exist on the
C300 540 (3722) project on which the pipe is to be used by multiplying the
C350 630 (4343)
C400 720 (4963)
values of P1 from Table A1.1 by a service (design) factor
C450 810 (5584) selected for the application on the basis of two general groups
of conditions. The first group considers the manufacturing and
testing variables, specifically normal variations in the material,
A1.4 Hydrostatic Design Basis—The value of S is deter- manufacture, dimensions, good handling techniques, and in the
mined by extrapolation of the regression line to 50 years in evaluation procedures in this method. The second group
accordance with Practice D2992. considers the application or use, specifically installation,
environment, temperature, hazard involved, life expectancy
A1.5 Hydrostatic Design Basic Categories—Convert the desired, and the degree of reliability selected.
value of the HDB to internal hydrostatic pressure in psig as NOTE A1.3—It is not the intent of this standard to give service (design)
follows: factors. The service (design) factor should be selected by the design
engineer after evaluating fully the service conditions and the engineering
P 1 5 2 ~ t h sinθ ! ~ HDB! /D properties of the specific pipe material under consideration. Recom-
The pipe is categorized in accordance with Table A1.1. mended service (design) factors will not be developed or issued by ASTM.

A2. CALCULATIONS OF LOWER CONFIDENCE (LCL) AND LOWER PREDICTION (LPL) LIMITS

h LCL 5 ~ a1bfo ! 2 ts Πf o 2 F) 2 1
U
1
N

h LPL 5 ~ a1bfo ! 2 ts Π~fo 2 F!2 1


U
1 11
N

where all symbols are as defined in Annexes A1 and A3 of NOTE A2.1—Of the expected failures at stress (strain) fo 97.5 % will
Practice D2992 except: occur after hLPL. The average failure time at stress (strain) f o will occur
later than hLCL 97.5 % of the time.
f o 5 logof stress ~ strain! level of interest

APPENDIXES

(Nonmandatory Information)

X1. STRAIN CORROSION PERFORMANCE REQUIREMENTS

X1.1 From Molin and Leonhardt, the expression for bend- X1.2 The shape factor, Df, is dependent on both the pipe
ing strain is given as: ε b 5D f ~ t/d ! ~ δv/d ! . With the common stiffness and the installation (for example, backfill material,
acceptance that these pipes must be capable of withstanding backfill density, compaction method, haunching, trench
5 % deflection long-term, the maximum installed bending configuration, native-soil characteristics and vertical loading).
strain may be expressed as: Assuming conservatively, installations achieved by tamped
ε b max 5 ~ 0.05! ~ D f ! ~ t/d ! compaction with inconsistent haunching that will limit long-
term deflections to 5 %, the following values of Df have been
Using the AWWA C-950 long-term bending factor of safety selected to be realistic, representative and limiting. Substituting
of 1.50, the minimum strain corrosion performance extrapo- these values in the above equation for ESCV yields the
lated to 50 years must be: minimum required strain corrosion performances given below
E scv $ ~ 0.075! ~ D f ! ~ t/d ! and in Table 4.

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Pipe Stiffness (psi) Df


Minimum ESCV
Performance ε test $ Df F t
d1δV/2 GF δV
d1δV/2 G (X1.1)

9 8.0 0.60 (t/d) or


18 6.5 0.49 (t/d)
36
72
5.5
4.5
0.41
0.34
(t/d)
(t/d) ε test $ Df ~ t/d ! ~ δV/d ! S 1
11δV/2d D 2
(X1.2)

Df for parallel plate loading is 4.28. Making the other


NOTE X1.1—Products may have used limits of other than 5 % long-
term deflection. In such cases, the requirements should be proportionally substitutions yield:
adjusted. For example, a 4 % long-term limiting deflection would result in Pipe Stiffness (psi) Level B δv ⁄ d (%) Minimum Test
a 50 year requirement of 80 % of Table 4, while a 6 % limiting deflection
would yield a requirement of 120 % of Table 4. 9 30 0.97 (t/d)
18 25 0.85 (t/d)
36 20 0.71 (t/d)
X1.3 Alternative Strain Corrosion Test Requirements: 72 15 0.56 (t/d)
X1.3.1 At 0.1 h (6 min), the required strain corrosion X1.3.2 The minimum strain values at 10, 100, 1000, and
performance is based on the level B deflections from Table 6 as 10 000 h given in Table 4 are defined by a straight line
follows: connecting the points at 6 min and 50 years on a log-log plot.

X2. INSTALLATION

X2.1 This specification is a material performance and pur- and backfill, pipe characteristics, and care in the field construc-
chase specification only and does not include requirements for tion work. The purchaser of the fiberglass pressure pipe
engineering design, pressure surges, bedding, backfill, or the specified herein is cautioned that he must properly correlate the
relationship between earth cover load, and the strength of the field requirements with the pipe requirements and provide
pipe. However, experience has shown that successful perfor- adequate inspection at the job site.
mance of this product depends upon the proper type of bedding

X3. RECOMMENDED METHODS OF DETERMINING GLASS CONTENT

X3.1 Determine glass content as follows: X3.1.2 As a process control, by weight of the glass fiber
X3.1.1 By ignition loss analysis in accordance with Test reinforcement applied by machine into the pipe structure.
Method D2584 or ISO 1172.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3840 − 19

Standard Specification for


“Fiberglass” (Glass-Fiber-Reinforced Thermosetting-Resin)
Pipe Fittings for Nonpressure Applications1
This standard is issued under the fixed designation D3840; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* Development of International Standards, Guides and Recom-


1.1 This specification covers fiberglass pipe fittings in- mendations issued by the World Trade Organization Technical
tended for use in gravity flow systems for conveying sanitary Barriers to Trade (TBT) Committee.
sewage, storm water, and those industrial wastes for which the
2. Referenced Documents
fittings are determined to be suitable. Elbows, tees, laterals,
crosses, reducers, and adapters are included. Both glass-fiber- 2.1 ASTM Standards:2
reinforced thermosetting-resin pipe (RTRP) and glass-fiber- D638 Test Method for Tensile Properties of Plastics
reinforced polymer mortar pipe (RPMP) are fiberglass pipes. D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plas-
NOTE 1—For the purposes of this standard, polymer does not include tics
natural polymers.
D1763 Specification for Epoxy Resins
1.2 This specification is intended to cover only dimensions, D2290 Test Method for Apparent Hoop Tensile Strength of
material properties, and workmanship rather than the structural Plastic or Reinforced Plastic Pipe
design of the fittings. The structural design of the fittings shall D3262 Specification for “Fiberglass” (Glass-Fiber-
be as agreed upon between purchaser and supplier, and needs Reinforced Thermosetting-Resin) Sewer Pipe
to take into consideration the anticipated conditions of instal- D3567 Practice for Determining Dimensions of “Fiberglass”
lation and service. (Glass-Fiber-Reinforced Thermosetting Resin) Pipe and
1.3 This specification covers only fittings fabricated from Fittings
cut sections of pipe, or from a combination of pipe sections and D3892 Practice for Packaging/Packing of Plastics
contact molded (hand layup), or machine fabricated compo- F412 Terminology Relating to Plastic Piping Systems
nents. F477 Specification for Elastomeric Seals (Gaskets) for Join-
1.4 The values stated in inch-pound units are to be regarded ing Plastic Pipe
as the standard. The values given in parentheses are provided 3. Terminology
for information purposes only.
3.1 Definitions:
1.5 The following safety hazards caveat pertains only to the
3.1.1 General—Definitions are in accordance with Termi-
test method portion, Section 11, of this specification. This
nologies D883 and F412. Abbreviations are in accordance with
standard does not purport to address all of the safety concerns,
Terminology D1600, unless otherwise indicated.
if any, associated with its use. It is the responsibility of the user
of this standard to establish appropriate safety, health, and 3.2 Definitions of Terms Specific to This Standard:
environmental practices and determine the applicability of 3.2.1 fiberglass pipe—a tubular product containing glass
regulatory limitations prior to use. fiber reinforcements embedded in or surrounded by cured
thermosetting resin. It is acceptable for the composite structure
NOTE 2—There is no known ISO equivalent to this standard.
to contain aggregate, granular or platelet fillers, thixotropic
1.6 This international standard was developed in accor- agents, pigments or dyes. It is acceptable to include thermo-
dance with internationally recognized principles on standard- plastic or thermosetting liners or coatings.
ization established in the Decision on Principles for the
3.2.2 reinforced polymer mortar pipe—a fiberglass pipe
with aggregate.
1
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced
2
Plastic Piping Systems and Chemical Equipment. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Aug. 1, 2019. Published August 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1979. Last previous edition approved in 2014 as D3840 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D3840-19. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D3840 − 19
3.2.3 reinforced thermosetting resin pipe—a fiberglass pipe increase uniformly in width to provide the specified minimum
without aggregate. total width of overlay that shall be centered on the seam. Table
3.2.4 qualification—One or more tests used to prove the 1 shows minimum widths of overlays required. The ends of
design of a product. Not a routine quality control test. each layer of reinforcement shall be overlapped a minimum of
1 in. (25 mm). Crevices between joined sections shall be filled
NOTE 3—Qualification requirements appear in 6.1, 7.2, and 12.3. with a filled resin paste, leaving a smooth inner surface. The
interior of the seams shall also be sealed by covering with not
4. Materials less than a 0.03 in. (0.76 mm) thickness of reinforced resin-rich
4.1 Laminating Resin: surface that provides corrosion resistance suitable for the
4.1.1 Type 1—Polyester thermosetting resin, with or without intended service. Alternatively, when it is necessary to fabri-
fillers or thixotropic agents or both. cate a fitting where the size and configuration do not allow
NOTE 4—For the purpose of this standard, polyester includes vinyl ester
adequate access to interior seams, the cut edges of sections
resins. shall be sealed prior to assembly and any reinforcing overlay
protected by a resin-rich surface that provides corrosion
4.1.2 Type 2—Epoxy resin, conforming to the requirements
resistance suitable for the intended service.
of Specification D1763, with or without fillers or thixotropic
5.2.3 Components of dissimilar materials, such as steel to
agents, or both.
polyester or epoxy laminates, or polyester to epoxy laminates,
4.2 Reinforcement: shall be bonded with a resin compound capable of adhering to
4.2.1 Grade 1—A commercial grade of glass fibers with a both materials. The resin compound shall contact the joining
polyester-compatible finish. surfaces of both components with the spaces between the
4.2.2 Grade 2—A commercial grade of glass fibers with an components filled. The excess resin compound that extrudes
epoxy-compatible finish. from the seam shall be removed, leaving a smooth fillet.
4.3 Gaskets—The elastomeric gaskets used with the fittings Sealing laminates and reinforcing overlays shall be applied
joined to pipe shall conform to the requirements of Specifica- where required (see 5.1.1, 5.2.1, and 5.2.2).
tion F477.
6. Joints
5. Fabrication 6.1 The fitting joints shall be coupling or bell-and-spigot in
5.1 Permissible Components: accordance with the joint requirements of Specification D3262,
5.1.1 Fittings covered under this specification shall be unless otherwise specified. It is acceptable to qualify joint
fabricated from cut section of pipe that conform to the designs on straight sections of pipe.
requirements of Specification D3262, or from a combination of
7. Physical Requirements
such pipe sections and contact molded (hand layup) or machine
fabricated components. 7.1 Properties of structural laminates, used either as seam
5.1.2 It is acceptable to incorporate saddles, wrappers, reinforcing overlays or as contact molded or machine fabri-
necked flanges, and other components of metal or other cated components, other than cut sections of pipe, shall be as
dissimilar materials, as agreed upon between purchaser and shown in Table 1, when tested in accordance with 11.1.
supplier, provided the materials of such components are 7.2 Shear Strength—The minimum shear strength of seam
resistant to the corrosive effects of the internal and external reinforcing overlays shall be 500 psi (3.45 MPa) when tested in
environments anticipated in service, or are lined or coated or accordance with 11.2.
both with materials that provide equivalent protection.
5.2 Bonding and Laminate Overlay Reinforcements: 8. Dimensions and Permissible Variations
5.2.1 Sections of the fitting shall be aligned and bonded 8.1 Wall Thickness—The wall thickness of any area of the
together using polyester (Type 1) or epoxy (Type 2) resin fitting furnished under this specification shall not at any point
materials with or without fiberglass reinforcement. Fiberglass be less than 87.5 % of the nominal wall thickness published in
reinforcement materials shall be compatible with the laminat- the manufacturers’ literature current at the time of purchase
ing resin; Grade 1 reinforcements shall be used with Type 1 when measured in accordance with 11.3.1.
laminating resin, and Grade 2 reinforcements shall be used 8.2 Fitting Diameters—Fittings shall be supplied in nominal
with Type 2 laminating resin. diameters as given in Specification D3262. The fitting diameter
5.2.2 It is acceptable to apply laminated reinforcing over- tolerances shall be as given in Specification D3262, when
lays of bonded seams to either the outside or inside surface of measured in accordance with 11.3.2 or 11.3.3 as applicable.
the fitting, or to both inside and outside surfaces. The laminate
shall be of chemically resistant construction suitable for the 8.3 Lengths—The tolerance for the laying length and other
purpose and shall provide the additional strength necessary to significant dimensions shall be 62 in. (651 mm) or 61 % of
meet the physical requirements shown in Table 1. Finished the dimension, whichever is greater, when measured in accor-
seam overlays shall be built up in two or more successive dance with 11.3.4. See Tables 2-6 and Figs. 1 and 2 for typical
layers of reinforcement and shall be as crevice free as minimum laying lengths.
described in this paragraph and 5.2.3. The width of the first 8.4 Angular Dimensions—Angular dimensions shall have a
layer shall be 2 in. (50 mm) minimum. Successive layers shall tolerance of 61° when measured in accordance with 11.3.5.

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D3840 − 19
TABLE 1 Minimum Properties of Structural Laminates
Nominal Diameter, in. (mm) Minimum Hoop Tensile Minimum Axial Tensile Minimum Total Width of
Strength, lbf/in. (kN/m) of Strength, lbf/in. (kN/m) Overlay, in. (mm)B
widthA of circumferenceA

8 (203) 1600 (280) 1600 (280) 4 (100)


10 (254) 1600 (280) 1600 (280) 4 (100)
12 (305) 1600 (280) 1600 (280) 4 (100)
14 (356) 1600 (280) 1600 (280) 4 (100)
15 (381) 1600 (280) 1600 (280) 4 (100)
16 (406) 1600 (280) 1600 (280) 4 (100)
18 (457) 1600 (280) 1600 (280) 4 (100)
20 (508) 1600 (280) 1600 (280) 4 (100)
21 (533) 1600 (280) 1600 (280) 4 (100)
24 (610) 1600 (280) 1600 (280) 4 (100)
27 (686) 1600 (280) 1600 (280) 4 (100)
30 (762) 1600 (280) 1600 (280) 4 (100)
33 (838) 1700 (300) 1700 (300) 6 (150)
36 (914) 1800 (315) 1800 (315) 6 (150)
39 (991) 2000 (350) 2000 (350) 6 (150)
42 (1067) 2100 (368) 2100 (368) 6 (150)
45 (1143) 2300 (403) 2300 (403) 6 (150)
48 (1219) 2400 (420) 2400 (420) 8 (200)
51 (1295) 2600 (455) 2600 (455) 8 (200)
54 (1372) 2700 (473) 2700 (473) 8 (200)
60 (1524) 3000 (525) 3000 (525) 8 (200)
66 (1676) 3300 (578) 3300 (578) 10 (250)
72 (1829) 3600 (630) 3600 (630) 10 (250)
78 (1981) 3900 (683) 3900 (683) 10 (250)
84 (2134) 4200 (736) 4200 (736) 12 (300)
90 (2286) 4500 (788) 4500 (788) 12 (300)
96 (2438) 4800 (841) 4800 (841) 14 (350)
102 (2591) 5100 (893) 5100 (893) 16 (400)
108 (2743) 5400 (946) 5400 (946) 16 (400)
114 (2896) 5700 (998) 5700 (998) 16 (400)
120 (3048) 6000 (1051) 6000 (1051) 16 (400)
132 (3353) 6600 (1156) 6600 (1156) 18 (450)
144 (3658) 7200 (1261) 7200 (1261) 20 (500)
156 (3962) 7800 (1366) 7800 (1366) 22 (550)
A
The values given are minimums only. Sound engineering practice dictates that all fittings be designed to withstand the loads and conditions anticipated in the service for
which they are intended.
B
The dimensions given are minimums for“ butt-and-strap’’ type joints.

9. Workmanship, Finish, and Appearance 9.5 Fittings shall show good workmanship, including uni-
9.1 The inside surfaces of each fitting shall blend smoothly formity from item to item.
and shall be free of bulges, dents, ridges, or other irregularities 10. Sampling
that result in a variation of more than 1⁄8 in. (3.2 mm) from that
obtained on adjacent portions of the surface. 10.1 Lot—Unless otherwise agreed upon between purchaser
and supplier, one lot shall consist of 100 fittings of each type,
NOTE 5—This requirement is concerned with roughness and waviness grade, and construction of laminate overlay reinforcement, or
and does not apply to diameter tolerances or thickness of internal seam contact molded or machine fabricated component, or both.
reinforcement if present. See 8.2 for inside diameter tolerances, including
internal reinforcement. 10.2 Unit Sample—Select one fitting from each lot. Prepare
9.2 Joint sealing surfaces shall be free of dents, gouges, a sample or representative laminate and test specimens to
cracks, and other surface imperfections that will affect the determine conformance with the requirements of 7.1 for
integrity of the joints. ultimate tensile strength.
9.3 The inner surface of each reinforced plastic fitting 11. Test Methods
component and connecting seam shall be composed of resin 11.1 Ultimate Tensile Strength—Determine the ultimate ten-
with or without reinforcement, aggregate, or filler. No glass sile strength of sample laminate specimens cut from seam
fiber-reinforcement shall penetrate the interior surface of the reinforcing overlays or contact molded or machine fabricated
fitting wall. components, or from specimens of a laminate fabricated to be
9.4 Internal and external reinforcements shall be free of consistent in every way with the construction used in the
voids, dry spots, cracks, and crazing. Some waviness in the reinforcing overlay or component of the fitting. One or both of
internal reinforcement is permissible so long as the surface is the following test methods shall be employed at the manufac-
smooth. Unless otherwise agreed upon between purchaser and turer’s option:
supplier, all fittings shall meet the visual and repair criteria of 11.1.1 Test Method D2290, using Type B specimens, except
Tables 7 and 8. that the size of the specimens shall be permitted to be modified

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D3840 − 19
TABLE 2 0° to 30° ElbowA TABLE 3 31° to 60° ElbowA

Pipe Size, in. (mm) Dimension AB , in. (mm)

Pipe Size, in. Dimension CB , R1 (45°), in.


(mm) in. (mm) (mm)
8 (203) 12 (305)
10 (254) 13 (330)
12 (305) 13 (330)
14 (356) 14 (356) 8 (203) 18.5 (470) 12.0 (305)
15 (381) 14 (356) 10 (254) 19.5 (495) 15.0 (381)
16 (406) 15 (381) 12 (305) 20.5 (521) 18.0 (457)
18 (457) 15 (381) 14 (356) 22.0 (559) 21.0 (533)
20 (508) 16 (406) 15 (381) 22.5 (572) 22.5 (572)
21 (533) 16 (406) 16 (406) 23.0 (584) 24.0 (610)
24 (610) 17 (432) 18 (457) 25.0 (635) 27.0 (686)
27 (686) 17 (432) 20 (508) 25.5 (648) 30.0 (762)
30 (762) 18 (457) 21 (533) 26.0 (660) 31.5 (800)
33 (838) 18 (457) 24 (610) 27.5 (699) 36.0 (914)
36 (914) 20 (508) 27 (686) 28.5 (724) 40.5 (1029)
39 (991) 21 (533) 30 (762) 31.0 (787) 45.0 (1143)
42 (1067) 22 (559) 33 (838) 33.0 (838) 49.5 (1257)
45 (1143) 23 (584) 36 (914) 34.5 (876) 54.0 (1372)
48 (1219) 24 (610) 39 (991) 36.5 (927) 58.5 (1486)
54 (1372) 25 (635) 42 (1067) 38.0 (965) 63.0 (1600)
60 (1524) 26 (660) 45 (1143) 40.5 (1029) 67.5 (1715)
66 (1676) 29 (737) 48 (1219) 41.5 (1054) 72.0 (1829)
72 (1829) 29 (737) 54 (1372) 45.0 (1143) 81.0 (2057)
78 (1981) 30 (762) 60 (1524) 48.5 (1232) 90.0 (2286)
84 (2134) 34 (864) 66 (1676) 52.0 (1321) 99.0 (2515)
90 (2286) 36 (914) 72 (1829) 55.5 (1410) 108.0 (2743)
96 (2438) 38 (965) 78 (1981) 59.0 (1499) 117.0 (2972)
102 (2591) 39 (991) 84 (2134) 62.5 (1588) 126.0 (3200)
108 (2743) 41 (1041) 90 (2286) 66.5 (1689) 135.0 (3429)
A 96 (2438) 70.0 (1778) 144.0 (3658)
Fitting end configurations other than the typical bell and spigot shown in the
102 (2591) 73.5 (1867) 153.0 (3886)
figure are acceptable as agreed upon between manufacturer and purchaser. Refer
108 (2743) 77.0 (1956) 162.0 (4115)
to Section 6.
B A
Dimensions given are typical minimum laying lengths. Laying lengths for fittings Fitting end configurations other than the typical bell and spigot shown in the figure
larger than 108 in. diameter shall be as agreed upon between purchaser and are acceptable as agreed upon between the manufacturer and purchaser. Refer to
supplier. Section 6.
B
Dimensions given are typical minimum laying lengths. Laying lengths for fittings
larger than 108 in. diameter shall be as agreed upon between purchaser and
supplier.

and speed of testing and rate of crosshead motion shall not


apply. Record the load to fail of each specimen and determine directions. The ultimate tensile strength of isotropic laminates
the specimen width as close to the break as possible. Use the shall be permitted to be determined in either the hoop or axial
measured width and failure load to calculate the tensile direction.
strength. 11.2 Minimum Shear Strength—Determine the shear
11.1.2 Test Method D638, using flat Type I specimens, strength of axially oriented laminate specimens in accordance
except that the specimens shall be the actual thickness of the with 11.1.2, except that the specimens shall be representative
reinforcing overlay or fabricated component and the other of an overlay reinforced seam joining two cut sections of pipe
dimensions shall be suitable for the specimen thickness and the in straight alignment (See Fig. 3). Calculate the shear strength
testing apparatus. Specimens shall be permitted to be machined by dividing the maximum load by the area of both sides of the
on the edges, but shall not be machined on the surface. Tensile pipe section covered by the reinforcing overlay on one side of
strength shall be the average of five specimens tested at a speed the seam. If the specimen does not fail or if the failure occurs
of 0.20 to 0.25 in. (5 to 6.4 mm)/min. outside of the reinforced area, consider the results satisfactory
11.1.3 Conduct tests of anisotropic laminates to determine provided the shear strength calculated from the maximum load
the ultimate tensile strength in both the hoop and axial exceeds 500 psi (3.45 MPa).

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D3840 − 19
TABLE 4 61° to 90° ElbowA TABLE 5 TeeA

Pipe Size, in. Dimension EB , R2 (90°), in.


(mm) in. (mm) (mm)
Pipe Size, in. Dimension DB , Dimension EB , in.
(mm) in. (mm) (mm)
8 (203) 26.0 (660) 12.0 (305)
10 (254) 28.5 (724) 15.0 (381) 8 (203) 15.0 (381) 30.0 (762)
12 (305) 31.0 (787) 18.0 (457) 10 (254) 16.0 (406) 32.0 (813)
14 (356) 34.5 (876) 21.0 (533) 12 (305) 17.0 (432) 34.0 (864)
15 (381) 35.5 (902) 22.5 (572) 14 (356) 18.0 (457) 36.0 (914)
16 (406) 37.0 (940) 24.0 (610) 15 (381) 18.5 (470) 37.0 (940)
18 (457) 40.5 (1029) 27.0 (686) 16 (406) 19.0 (483) 38.0 (965)
20 (508) 43.0 (1092) 30.0 (762) 18 (457) 20.0 (508) 40.0 (1016)
21 (533) 44.0 (1118) 31.5 (800) 20 (508) 21.0 (533) 42.0 (1067)
24 (610) 46.0 (1219) 36.0 (914) 21 (533) 21.5 (546) 43.0 (1092)
27 (686) 49.0 (1308) 40.5 (1029) 24 (610) 24.0 (610) 48.0 (1219)
30 (762) 53.0 (1422) 45.0 (1143) 27 (686) 25.5 (648) 51.0 (1295)
33 (838) 58.0 (1549) 49.5 (1257) 30 (762) 27.0 (686) 54.0 (1372)
36 (914) 63.0 (1638) 54.0 (1372) 33 (838) 28.5 (724) 57.0 (1448)
39 (991) 68.0 (1778) 58.5 (1486) 36 (914) 30.0 (762) 60.0 (1524)
42 (1067) 71.0 (1854) 63.0 (1600) 39 (991) 31.5 (800) 63.0 (1600)
45 (1143) 77.5 (1969) 67.5 (1715) 42 (1067) 33.0 (838) 66.0 (1676)
48 (1219) 80.0 (2070) 72.0 (1829) 45 (1143) 35.5 (902) 71.0 (1803)
54 (1372) 88.0 (2286) 81.0 (2057) 48 (1219) 37.0 (940) 74.0 (1880)
60 (1524) 95.0 (2489) 90.0 (2286) 54 (1372) 40.0 (1016) 80.0 (2032)
66 (1676) 103.0 (2705) 99.0 (2515) 60 (1524) 43.0 (1092) 86.0 (2184)
72 (1829) 115.0 (2921) 108.0 (2743) 66 (1676) 47.0 (1194) 94.0 (2388)
78 (1981) 123.0 (3137) 117.0 (2972) 72 (1829) 50.0 (1270) 100.0 (2540)
84 (2134) 131.5 (3340) 126.0 (3200) 78 (1981) 53.0 (1346) 106.0 (2692)
90 (2286) 140.0 (3556) 135.0 (3429) 84 (2134) 56.0 (1422) 112.0 (2845)
96 (2438) 148.5 (3772) 144.0 (3658) 90 (2286) 60.0 (1524) 120.0 (3048)
102 (2591) 157.0 (3988) 153.0 (3886) 96 (2438) 63.0 (1600) 126.0 (3201)
108 (2743) 165.5 (4204) 162.0 (4115) 102 (2591) 66.0 (1676) 132.0 (3353)
A
Fitting end configurations other than the typical bell and spigot shown in the figure 108 (2743) 69.0 (1753) 138.0 (3505)
are acceptable as agreed upon between the manufacturer and purchaser. Refer to A
Fitting end configurations other than the typical bell and spigot shown in the
Section 6. figure are acceptable as agreed upon between the manufacturer and purchaser.
B
Dimensions given are typical minimum laying lengths. Laying lengths for fittings Refer to Section 6.
larger than 108 in. diameter shall be as agreed upon between purchaser and B
Dimensions given are minimum laying lengths. Laying lengths for fittings larger
supplier. than 108 in. diameter shall be as agreed upon between purchaser and supplier.

11.3 Dimensions: 11.3.5 Angular Dimensions—Measure with a protractor or


11.3.1 Wall Thickness—Determine in accordance with Prac- other suitable device having graduations of 1 deg or less.
tice D3567. Straightedges, levels, squares, and other devices shall be
11.3.2 Inside Diameter—Determine in accordance with permitted to be employed as required by the configuration of
Practice D3567. the fitting or component. Alternatively, angular dimensions
11.3.3 Outside Diameter—Determine in accordance with shall be permitted to be calculated from linear measurements.
Practice D3567.
11.3.4 Lengths—Determine in accordance with Practice 12. Inspection
D3567. Straightedges, levels, squares, and other devices shall 12.1 Visually and dimensionally inspect each fitting. Dis-
be permitted to be employed as required by the configuration of crepancies shall be corrected or the defective fitting shall be
the fitting or component. rejected, as agreed upon between purchaser and supplier.

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D3840 − 19
TABLE 6 45° WyeA 12.2 If the results of the test for ultimate tensile strength
requirements of 7.1 fall below the required minimums, then, at
the option of the supplier, that test shall be repeated on two
additional sample laminates representative of that same lot,
each of which shall conform to the requirements specified. If
either of these two additional samples fail, the purchaser shall
have the option to reject the lot.
12.3 The initial design of reinforcing overlays and fabri-
cated components shall be qualified by dimensional and visual
inspection and by testing in accordance with the requirements
of 7.1 and 7.2. The overlay or component shall be requalified
when any change occurs in either the resin formulation, the
total amount of the reinforcement, the grade or composition of
the finish (sizing or coating) of the reinforcement, the applica-
tion method, or the technique of fabrication.
Pipe Size, Dimension AB , Dimension BB , Dimension CB , 12.4 Additional inspections and tests shall be as agreed
in. (mm) in. (mm) in. (mm) in. (mm)
upon by the purchaser and the supplier as part of the purchase
contract.
8 (203) 24.0 (610) 13.0 (330) 37.0 (940)
10 (254) 26.5 (673) 13.5 (343) 40.0 (1016)
12 (305) 29.0 (737) 13.5 (343) 42.5 (1080) 13. Packaging, Marking, and Shipping
14 (356) 31.0 (787) 14.0 (356) 45.0 (1143)
15 (381) 32.5 (826) 14.5 (368) 47.0 (1194) 13.1 Fittings shall be marked on the outside surface in
16 (406) 33.5 (851) 14.5 (368) 48.0 (1219) letters not less than 1⁄2 in. in height and of bold type style in a
18 (457) 36.0 (914) 15.0 (381) 51.0 (1295)
20 (508) 38.5 (978) 15.5 (394) 54.0 (1372)
color and type that will remain legible under normal handling
21 (533) 39.5 (1003) 15.5 (394) 55.0 (1397) and installation procedures. The marking shall include this
24 (610) 43.5 (1105) 16.0 (406) 59.5 (1511) ASTM specification number: D3840, manufacturer’s name or
27 (686) 47.0 (1194) 17.0 (432) 64.0 (1626)
30 (762) 50.5 (1283) 17.5 (445) 68.0 (1727) trademark, nominal size, and the words “GRAVITY SEWER.”
33 (838) 54.0 (1372) 18.0 (457) 72.0 (1829)
36 (914) 58.0 (1473) 18.5 (470) 76.5 (1943) 13.2 Fittings shall be prepared for shipment so as to ensure
39 (991) 61.5 (1562) 19.0 (483) 80.5 (2045) acceptance by common or other carriers.
42 (1067) 66.0 (1676) 21.0 (533) 87.0 (2210)
45 (1143) 69.5 (1765) 21.5 (546) 91.0 (2311) 13.3 All packing, packaging, and marking provisions of
48 (1219) 73.5 (1867) 22.0 (559) 95.5 (2426)
54 (1372) 80.5 (2045) 23.5 (597) 104.0 (2642) Practice D3892 shall apply to this specification.
60 (1524) 88.0 (2235) 24.5 (622) 112.5 (2858)
66 (1676) 97.0 (2464) 28.0 (711) 125.0 (3175)
72 (1829) 104.5 (2654) 29.0 (737) 133.5 (3391)
14. Keywords
78 (1981) 111.5 (2832) 30.0 (762) 141.5 (3594) 14.1 dimensions; fabrication; fiberglass; fittings; overlays;
84 (2134) 120.0 (3048) 32.5 (826) 152.5 (3874)
90 (2286) 127.0 (3226) 33.5 (851) 160.5 (4077) pipe
96 (2438) 134.5 (3416) 35.0 (889) 169.5 (4305)
102 (2591) 141.5 (3594) 36.0 (914) 176.5 (4483)
108 (2743) 150.0 (3810) 38.5 (978) 188.5 (4788)
A
Fitting end configurations other than the typical bell and spigot shown in the
figure are acceptable as agreed upon between the manufacturer and purchaser.
Refer to Section 6.
B
Dimensions given are typical minimum laying lengths. Laying lengths for fittings
larger than 108 in. diameter shall be as agreed upon between purchaser and
supplier.

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D3840 − 19

NOTE 1—Fitting end configurations other than the typical bell and spigot shown in the figure are acceptable as agreed upon between the manufacturer
and purchaser. Refer to Section 6.
FIG. 1 Concentric Reducer

NOTE 1—Fitting end configurations other than the typical bell and spigot shown in the figure are acceptable as agreed upon between the manufacturer
and purchaser. Refer to Section 6.
FIG. 2 Eccentric Reducer

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D3840 − 19
TABLE 7 Visual Inspection and Repair Criteria for Inside Surfaces of Fiberglass Pipe Fittings
Indication Description Acceptable Without Repair Permitted Maximum
Maximum Size No./ft2 Repair Repairs/ft2

Air bubble air entrapment within the liner ⁄


1 16 in. in diameter 2/in.2 A
10
(void) rein-
forcement
A
Chip small piece broken from edge or 1⁄4 in. long and 1⁄2 the liner 10 10
sur- thickness
face
A
Crack separation of the laminate none permitted 0 5
extending
through the thickness of the
liner
A
Crazing fine cracks at or under the none permitted 0 10
surface
A
Dry-spot area where reinforcement was not none permitted 0 0.35 ft2 in
thoroughly wetted with resin area
A
Lack of fill-out area where resin has drained 1 in. long and 1⁄2 the liner 5 0.35 ft2 in
from thickness area
reinforcement
A
Pits (pinholes) small craters in surface 1⁄8 in. long and 1⁄2 the liner 15 15
thickness
B
Scratch shallow mark, groove, furrow, or maximum 1⁄4 of the liner no limit no limitB
channel thickness; if exceeds 1⁄2 of the 0.35 ft2 areaA
liner thickness use repairA
Wrinkle an imperfection that has the no limit, provided wrinkle has not no limit none required 0
appear- cracked the structural wall
ance of a wave molded into the
reinforcement material
A
Permitted repairs—Replace liner material in the discrepant area.
B
Permitted repairs—Coat with liner resin.

TABLE 8 Visual Inspection and Repair Criteria for Exterior Surfaces of Fiberglass Pipe Fittings
Indication Description Acceptable Without Repair Permitted Maximum
Maximum Size No./ft.2 Repair Repairs/ft2

A
Burn thermal decomposition evidenced by 5 % of the wall thickness; repair not 5 1
distortion or destruction of the permitted if decomposition
surface, or both extends beyond 35 % of wall
thickness
A
Chip small piece broken from edge or maximum 1⁄4 in. long by 10 % of 2 5
surface wall thickness (NTE 1⁄8 in. deep);
if over 1⁄16 in. deep use repairB
A
Crack separation of the laminate extending none permitted 0 5
through the wall and visible on
opposite surfaces
A
Cut roving broken or cut outer rovings due to none permitted; repair not permitted 0 1
scraping or scuffing during if damage extends beyond 35 %
handling of wall thickness.
A
Crazing fine cracks at or under the surface, none permitted 0 5
exposing reinforcement
C
Drip, resin resin protrusion ⁄ in. high
12 no limit no limit
B
Dry spot area where reinforcement was not none permitted 0 5
thoroughly wetted with resin
C
Fish-eye small globular mass that has not ⁄ in. high
14 no limit no limit
blended completely into the
surrounding material
A
Fracture rupture of laminate surface without none permitted; repair not permitted 0 2
complete penetration if fracture penetrates beyond
outer 1⁄2 of
wall thickness
B
Lack of fill-out area where resin has drained from 2 in. long 5 0.5 ft2 in area
the reinforcement
B
Pits (pinholes) small craters in surface ⁄ in. long with no exposed
18 15 0.5 ft2 in area
reinforcement
B
Scratch shallow mark, groove, furrow, or no exposed reinforcement no limit 20
channel caused by improper
handling
A
Apply a structural overlay extending at least 2 in. beyond the damaged area and resulting in a minimum total wall thickness in the repaired area of the wall thickness of
the fitting or component in the affected area.
B
Coat with resin.
C
Grind excess to within tolerance.

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NOTE 1—It is acceptable to adjust the number of layers (symmetrically applied) and shear area, if desired, to ensure that shear is the failure mode.
FIG. 3 Shear Test Specimen

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D3840 – 14) that may impact the use of this standard. (August 1, 2019)

(1) Revised 8.2, 8.3, and 8.4.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3892 − 15

Standard Practice for


Packaging/Packing of Plastics1
This standard is issued under the fixed designation D3892; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* 2.3 Other Standards:


1.1 This practice covers the packaging and packing of all National Motor Freight Classification4
thermoset and thermoplastic resins and fabricated shapes. Uniform Freight Classification Rules5
1.2 This standard does not purport to address all of the 3. Terminology
safety concerns, if any, associated with its use. It is the 3.1 Definitions—For definitions of technical terms used in
responsibility of the user of this standard to establish appro- this practice pertaining to plastics, see Terminology D883.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 4. Significance and Use
NOTE 1—There is no known ISO equivalent to this standard. 4.1 Packing and packaging provisions are outlined as
1.3 This international standard was developed in accor- needed for adequate transport of resins and finished products
dance with internationally recognized principles on standard- with a minimum of mishaps in shipment.
ization established in the Decision on Principles for the 4.2 Commercial levels are included for all commercial and
Development of International Standards, Guides and Recom- most federal and military shipments. Level A requirements are
mendations issued by the World Trade Organization Technical added for special military purchases only.
Barriers to Trade (TBT) Committee.
5. Procedure
2. Referenced Documents
5.1 Examination of Preparation for Delivery—Examine in
2.1 ASTM Standards:2 accordance with Table 1 to determine that packaging, packing,
D883 Terminology Relating to Plastics and marking comply with requirements specified in the con-
2.2 Federal Standards: tract or order. The sample unit for this examination shall be one
Department of Transportation 19A, Title 49, Code of Federal shipping container fully prepared for delivery.
Regulations, Section 178.190, Wooden Boxes—Glued,
5.2 Packaging—Packaging shall be commercial or Level A,
Plywood Cleated3
as specified.
Department of Transportation 17H, Title 49, Code of Federal
5.2.1 Commercial—The material shall be packaged in ac-
Regulations, Section 178.118, Steel Drums3
cordance with normal commercial practice. The complete
package shall be designed to ensure the item against damage
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and during shipment, handling, and storage.
is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials. 5.2.2 Level A—For Military Procurement Only:
Current edition approved Sept. 1, 2015. Published September 2015. Originally
approved in 1980. Last previous edition approved in 2009 as D3892 - 93 (2009).
5.2.2.1 Sheets, Rods, Tubes, Pipes, Fittings, and Other
DOI: 10.1520/D3892-15. Shapes—Unless otherwise specified in the contract or order,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or individual fabricated shapes shall be packaged in such a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
4
the ASTM website. Available from American Trucking Assn., 1616 P Street, N.W., Washington, DC
3
Available from U.S. Government Printing Office Superintendent of Documents, 20036.
5
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:// Available from Railroad Freight Classification, Room 1106, 222 South River-
www.access.gpo.gov. side Plaza, Chicago, IL 60606.

*A Summary of Changes section appears at the end of this standard


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D3892 − 15
TABLE 1 Examination for Defects in Preparation for Delivery 5.3.2 Level A (For Military Procurement Only):
Examine Defect 5.3.2.1 Sheets, Rods, Tubes, Film, and Other Shapes—The
Packaging Not level specified. Packaging material not as materials packaged as specified in 5.2.2.1 and 5.2.2.2 shall be
specified.
Packing Not level specified. Containers not as specified. packed in plywood cleated boxes conforming to Department of
Count Less than specified or indicated quantity. Transportation (DOT) 19A. All items packed together must be
Weight and cube Gross weight is greater than, or less than, specified of the same technical description.
require-
ments. 5.3.2.2 Resin, Powder, Granules—Unless otherwise
Markings Markings not in accordance with specified specified, the material in the quantity specified shall be packed
requirements.
in metal drums conforming to DOT 17H. Insofar as practical,
containers shall be of uniform shape and size, with minimum
cube and tare consistent with the protection required. All items
manner as to protect the material against physical and mechani- packed together must be of the same technical description.
cal damage and contamination during transit. Only items 5.4 Marking—Marking for interior packages and shipping
comprised of a single National Stock number (NSN) or containers shall be as specified in the contract or order.
identifying number shall be placed in one package. Individual
sheets shall be masked or interleaved. 6. Ordering Information
5.2.2.2 Rolls of Film or Sheeting—These shall be supplied 6.1 All orders shall include the following information:
in rolls. Each roll shall be wrapped with at least one layer of 6.1.1 Title, number, and date of this practice: ASTM D3892,
polyethylene film or kraft paper, and tightly sealed with tape to 6.1.2 Type of material required,
prevent contamination. 6.1.3 Color required, with tolerance and method of
5.3 Packing—Packing shall be commercial or Level A, as determination, including whether determination shall be made
specified. on unprocessed material or molded specimens,
5.3.1 Commercial—The material shall be packed in accor- 6.1.4 Form and uniformity required, when so specified,
dance with normal commercial practice. The packaged mate- 6.1.5 Level of packaging/packing required, and
rial shall be packed to assure acceptance by common carrier 6.1.6 Marking requirements.
and to provide product protection against loss and damage
during multiple shipments, handling, and storage. The shipping 7. Keywords
container shall be in compliance with National Motor Freight 7.1 containers; film; marking; packaging; packing; plastics;
Classification and Uniform Freight Classification Rules. shapes; sheeting

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D3892 - 93
(2009)) that may impact the use of this standard. (September 1, 2015)

(1) Note 1 was updated to use currently approved statement.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3982 − 08 (Reapproved 2014)

Standard Specification for


Contact Molded “Fiberglass” (Glass Fiber Reinforced
Thermosetting Resin) Ducts 1
This standard is issued under the fixed designation D3982; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 2. Referenced Documents


1.1 This specification covers ducts fabricated by contact 2.1 ASTM Standards:2
molding intended for use in handling corrosive fumes and C581 Practice for Determining Chemical Resistance of
process gases. Special attention is given to equipment that Thermosetting Resins Used in Glass-Fiber-Reinforced
operates at temperatures over 180°F (82.2°C) with regard to Structures Intended for Liquid Service
strength and corrosion resistance. C582 Specification for Contact-Molded Reinforced Thermo-
1.2 The material of construction shall be “fiberglass” con- setting Plastic (RTP) Laminates for Corrosion-Resistant
sisting of a polyester, vinyl ester, or other qualified resin-matrix Equipment
systems with fiber reinforcement in accordance with Specifi- D883 Terminology Relating to Plastics
cation C582. D2583 Test Method for Indentation Hardness of Rigid Plas-
tics by Means of a Barcol Impressor
1.3 This specification is not intended to cover selection of D2584 Test Method for Ignition Loss of Cured Reinforced
resins and reinforcements for specific chemical environments. Resins
1.4 This specification covers ducts up to a design pressure F412 Terminology Relating to Plastic Piping Systems
of 65 psig (34.5 Pa). F436 Specification for Hardened Steel Washers (Metric)
1.5 The values stated in inch-pound units are to be regarded F0436_F0436M
as standard. The values given in parentheses are mathematical 2.2 NFPA Standard:
conversions to SI units that are provided for information only NFPA 91 Installation of Blower and Exhaust Systems for
and are not considered standard. Duct, Stack and Vapor Removal or Conveying3
1.6 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.1 Definitions:
priate safety and health practices and determine the applica- 3.1.1 The definitions used in this specification are in accor-
bility of regulatory limitations prior to use. dance with definitions in Terminologies D883 and F412, unless
NOTE 1—There is no known ISO equivalent to this standard.. otherwise specified.
1.7 This international standard was developed in accor- 3.2 Definitions of Terms Specific to This Standard:
dance with internationally recognized principles on standard- 3.2.1 calculated thickness—this description is in accordance
ization established in the Decision on Principles for the with the standard laminate composition tables for Types I and
Development of International Standards, Guides and Recom- II in Specification C582.
mendations issued by the World Trade Organization Technical 3.2.2 contact molding—includes the “hand layup” and the
Barriers to Trade (TBT) Committee. “spray up” methods of manufacture.

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Plastic Piping Systems and Chemical Equipment. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved March 1, 2014. Published March 2014. Originally the ASTM website.
3
approved in 1981. Last previous edition approved in 2008 as D3982 – 08. DOI: Available from National Fire Protection Association (NFPA), 1 Batterymarch
10.1520/D3982-08R14. Park, Quincy, MA 02169-7471, http://www.nfpa.org.

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3.2.3 flange cant—the angle that an entire branch is off from
being perpendicular to the main run centerline (see Fig. 1).
3.2.4 flange flatness—maximum deviation, (see Fig. 2) from
the actual flange face not including warpage or perpendicular-
ity.
3.2.5 flange offset—the amount that an entire branch is off
the main run centerline (see Fig. 3).
3.2.6 flange perpendicularity—maximum angle that the
plane (see Fig. 2) of the flange inside diameter makes with the
perpendicular plane to the duct’s centerline.
3.2.7 flange warpage—the amount that a flange outside
diameter pulls back from the plane of the inside diameter FIG. 2 Flange Tolerance Description
during the cure of the material (see Fig. 2).
3.2.8 hand layup—application of glass plies in sheet form
by hand. Resin can be applied by either brushing, rolling, or
spraying.
3.2.9 minimum thickness—take six thickness readings. The
average of the six readings shall be a minimum of 85 % of the
calculated thickness. This must contain the required layers of
glass.
3.2.10 spray up—fiberglass roving is chopped and blown
onto the mold in conjunction with resin and catalyst.
3.3 Symbols:
3.3.1 M = 11⁄2 oz ⁄ft2 chopped-strand mat.
3.3.2 R = 24 oz/yd2 woven-roving with a 5 by 4 weave.
3.3.3 V = glass or synthetic veil, 0.010 in. (0.25 mm)
calculated thickness.
3.3.4 For additional symbols and abbreviations specific to
design requirements, see 6.2.1.

4. Materials and Manufacture


4.1 Resin—The resin used shall be a commercial-grade
thermoset that has either been evaluated in a laminate by test in FIG. 3 Flange Offset
accordance with Practice C581 or that has been determined by

previous documented service to be acceptable for service


conditions. Where service conditions have not been evaluated
a suitable resin may be selected by agreement between the
manufacturer and the end user.
4.1.1 The resin may contain fillers or pigments in accor-
dance with Specification C582.
4.1.2 A thixotropic agent may be added up to 5 % by weight
of resin.
NOTE 2—The addition of a thixotropic agent may reduce the resistance
of many resin systems to certain corrosive chemical environments. It is the
responsibility of the fabricator, using a thixotropic agent in the resin to
ascertain its compatibility with the corrosive environment when this has
been reported to him by the purchaser.
4.1.3 Fire-retardant additives may be added to resins if
required to reduce flame spread.
NOTE 3—The addition of fire-retardant agents may interfere with the
visual inspection of laminate quality. Use in the inner surface and interior
layer should consider this, and the need for fire retardance should out
weigh any potential visual inspection difficulties. In some cases fire-
retardant agents can also affect the the chemical resistance of the resin. If
this is suspected, then chemical resistance testing of the resin should be
FIG. 1 Flange Cant conducted with fire-retardant additives included. Again the need for fire

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resistance should be balanced with chemical resistance. 6.1.5 Increase all calculated wall thicknesses to the nearest
4.2 Reinforcement—Glass reinforcing material with a binder standard wall thickness. Treat these standard wall thicknesses
and sizing compatible with the resin to be used. Fiber rein- as minimum dimensions.
forcements shall be in accordance with, and meet the require- 6.2 Cylinder Wall Design:
ments of, Specification C582 including composition require- 6.2.1 Symbols and Abbreviations:
ments for Type I and Type II laminates. 6.2.1.1 P—Actual design pressure, psi (MPa).
4.2.1 Corrosion Barrier—Consists of the inner surface fol- 6.2.1.2 PA—Allowable pressure, psi (MPa).
lowed by the interior layer. The corrosion barrier has a
6.2.1.3 Do—Outside diameter of cylinder, in. (mm).
minimum total calculated thickness of 0.096 in. (2.4 mm).
6.2.1.4 D—Inside diameter of cylinder, in. (mm).
4.2.1.1 Inner Surface—Surfacing veil with approximately
90 % resin and 0.010 to 0.020-in. (0.25 to 0.50-mm) calculated 6.2.1.5 S—Ultimate tensile strength, psi (MPa).
thickness. 6.2.1.6 F—Safety factor (see 6.1.1).
4.2.1.2 Interior Layer—A minimum of two plies of 6.2.1.7 T—Cylinder wall thickness, in. (mm).
11⁄2 oz ⁄ft2 chopped-strand mat or chopped roving equivalent 6.2.1.8 E—Tensile modulus of elasticity, psi (MPa).
with a compatible sizing system with approximately 75 % resin 6.2.1.9 L—Cylinder length between joints or elements that
and 0.086-in. (2.2-mm) calculated thickness minimum. Fiber qualify as a stiffener, in. (mm).
length shall be 1⁄2 in. (12.7 mm) minimum to 2 in. (50.8 mm) 6.2.1.10 I—Required moment of inertia for an element to
maximum. qualify as a stiffener, in.3 (mm3).
4.2.2 Structural Layer—Shall consist of chopped-strand mat 6.2.2 Internal Pressure:
plies of nominally 11⁄2 oz ⁄ft2 and have a 1⁄2 in. (12.7 mm) PDF
minimum to 2 in. (50.8 mm) maximum fiber length, or shall T5
2S
consist of a chopped roving equivalent in the spray-up method.
When necessary, woven-roving plies shall be used and shall 6.2.3 External Pressure (Internal Vacuum):
consist of 24 oz/yd2 with a five by four weave or a suitable Calculate:
equivalent agreed on by the end user and the fabricator.
Woven-roving shall be applied alternately with a minimum of 1.73 S D
Do
T
0.5

a 11⁄2 oz ⁄yd2 mat or chopped roving equivalent, finishing with


a mat layer. If result:
4.2.3 Outer Surface—Shall be coated with a resin-rich layer L
,
and containing 0.2 to 0.6 % paraffin wax with a melting point Do
of 122 to 126°F (50.0 to 52.2°C), except when other means are
Then use:
used to prevent air inhibition.

5. Physical Properties
P5
2.2E
F S DT
Do
3

5.1 Minimum wall of (V, M, M, M) shall be maintained If result:


under any circumstances. L
$
5.2 Laminates or portions of laminates comprised only of Do
chopped-strand mat shall have a 25 to 30 % glass content by
Then use:
weight when tested by Test Method D2584.
5.3 Minimum mechanical properties of standard laminates
shall be in accordance with Specification C582. P5
2.6E T
F DoS D 2.5

6. Design Requirements
L
Do
2 0.45
T
Do S D 0.5

6.1 Design Limitations: 6.2.4 Stiffeners to Withstand External Pressure:


6.1.1 Safety Factor—Use five for external pressure, use ten 6.2.4.1 Required Moment of Inertia:
for internal pressure and all other design calculations. PL ~ D o ! 3 F
I5
6.1.2 Maximum Permissible Deflection Under Design 24E
Load—Use 1 % of the span for laminates not exposed to a
6.2.4.2 Material used to attach ring stiffener to cylinder wall
chemical environment and use 1⁄2 % of the span for allowable
may be included when calculating the actual moment of inertia
deflection when a chemical environment will be in contact with
of the stiffener as well as the portion of the cylinder wall
the laminate.
beneath the stiffener and attachment material up to a width of
6.1.3 Secondary Bond Strength—When the load is along the
2x (stiffener width).
surface, use 2000 psi (13.79 MPa) ultimate shear stress for the
bonding surface area. Use a safety factor of ten when calcu- 6.3 Rectangular Duct:
lating allowable secondary bonding stresses. 6.3.1 The largest flat panel shall be designed to withstand
6.1.4 When an extra corrosion barrier is specified, do not the loading conditions and not exceed the design limitations
include this thickness in the design calculations. (see 6.1.2). This can be accomplished with a sufficient wall

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thickness alone or by the incorporation of stiffening ribs to 6.6 All stiffeners, access openings, lifting devices or other
reduce the required wall thickness. appurtenances shall be included as part of the duct design.
6.3.2 Appropriate calculations shall be performed for wall
6.7 Where static electricity has been determined to be a
thickness and stiffening ribs as determined by the manufacturer
problem by the engineer, the inner surface of the ductwork
and the purchaser. Minimum wall thickness in all cases for
shall be grounded with a maximum resistance to ground of
rectangular duct shall be as in Table 1, substituting the longer
106 Ω. The grounding method shall be determined by the
side for the diameter.
manufacturer and the purchaser.
6.3.3 The radial sides of a rectangular elbow shall be
designed as a round cylinder with the same radius.
7. Dimensions
6.4 Follow the requirements of NFPA 91Bulletin, Section
510 when it is required by law or the engineer. 7.1 Standard duct and fitting dimensions are shown on Fig.
4 and are based on inside dimensions.
6.5 Shop Drawings and Design Calculations—The fabri-
cated structure shall be in accordance with the design and 7.2 Standard elbows shall have a centerline radius of
construction details shown on shop drawings and design 11⁄2 times the duct diameter for over 3-in. (76.2-mm) diameter
calculations prepared by the manufacturer and approved by the and two times the duct diameter for 3-in. diameter and under.
purchaser. Details to be covered include, but are not limited to, 7.3 Mitered joints on all elbows 24-in. (609.6-mm) diameter
the following: and under are not permitted except when more room is required
6.5.1 Materials, including a definition of the fiber-resin for bolting or when a diameter is chosen that is not shown on
system, in accordance with types of resins and reinforcing Table 1.
materials of Specification C582,
6.5.2 Dimensions, 7.4 Standard duct flange thickness, drilling patterns, and
6.5.3 Size and location of stiffening ribs, minimum wall thickness are shown in Table 1.
6.5.4 Location of field joints and flanges, and 7.4.1 Vent connections from tanks and fans are normally
6.5.5 Type and location of supports, if supplied by the different from this pattern. Appropriate adjustments to flange
manufacturer. dimensions need to be taken to effect transition.

TABLE 1 Typical Flange Dimensions and Hanger Spacing

NOTE 1—1 in. = 25.4 mm


1 lb/ft = 1.488164 kg/m.
CalculatedA CylinderA FlangeB Flange Recom- Maximum MaximumCD
Inside Wall Wall Thickness, Outside Flange Bolt Bolt Hole Number Bolt mended Bolt Hanger
Thickness, Construction min, in. Bolt Torque, Spacing, ft
Diameter, in. Diameter, in. Circle, in. Diameter, in. Holes Torque, ft/lb
in. ft/lb
1 0.14 Type I ⁄
38 5 3 ⁄8 4 ⁄
7 16 4 20 30 8.0
1 1⁄ 4 0.14 Type I ⁄
38 5 5 ⁄8 4 1 ⁄4 ⁄
7 16 4 20 30 8.0
1 1⁄ 2 0.14 Type I 3⁄8 5 7 ⁄8 4 1 ⁄2 7⁄16 4 20 30 8.5
2 0.14 Type I 1⁄2 6 3 ⁄8 5 7⁄16 4 25 40 8.5
2 1⁄ 2 0.14 Type I 1⁄2 6 7 ⁄8 5 1 ⁄2 7⁄16 4 25 40 9.0
3 0.14 Type I 1⁄2 7 3 ⁄8 6 7⁄16 4 25 40 9.5
4 0.14 Type I 1⁄2 8 3 ⁄8 7 7⁄16 4 25 40 10.0
6 0.14 Type I 1⁄2 103⁄8 9 7⁄16 8 25 40 10.5
8 0.14 Type I 1⁄2 123⁄8 11 7⁄16 8 25 40 11.0
10 0.14 Type I 1⁄2 143⁄8 13 7⁄16 12 25 40 11.5
12 0.14 Type I 1⁄2 163⁄8 15 7⁄16 12 25 40 11.5
14 0.14 Type I 1⁄2 183⁄8 17 7⁄16 12 25 40 12.0
16 0.14 Type I 1⁄2 203⁄8 19 7⁄16 16 25 40 12.5
18 0.14 Type I 1⁄2 223⁄8 21 7⁄16 16 25 40 12.5
20 0.14 Type I 1⁄2 243⁄8 23 7⁄16 20 25 40 13.0
24 0.18 Type I 1⁄2 283⁄8 27 7⁄16 20 25 40 15.0
30 0.18 Type I 5⁄8 343⁄8 33 7⁄16 28 35 50 15.5
36 0.18 Type I 5⁄8 403⁄8 39 7⁄16 32 35 50 16.0
42 0.22 Type II 5⁄8 463⁄8 45 7⁄16 36 35 50 19.0
48 0.22 Type II 5⁄8 543⁄8 52 9⁄16 44 35 50 19.5
54 0.22 Type II 5⁄8 603⁄8 58 9⁄16 44 35 50 20.0
60 0.30 Type II 5⁄8 663⁄8 64 9⁄16 52 35 50 24.0
72 0.30 Type II 3⁄4 783⁄8 76 9⁄16 60 40 60 25.0
84 0.30 Type II 3⁄4 903⁄8 88 9⁄16 72 40 60 25.5
96 0.30 Type II 3⁄4 1023⁄8 100 9⁄16 80 40 60 26.0
A
Based on 10 ft (3.0 m) between stiffeners for 5-in. (127.0 mm) H2O vacuum service. See Specification C582 for wall construction.
B
The flange thicknesses are based on practical experience to resist maximum bolt torquing since these thicknesses are sufficient to resist process conditions. Minimum
flange thickness shall be measured in the spot-faced area.
C
Special design consideration must be given to hanger spacing for rectangular duct.
D
Based on experience involving duct systems not subjected to severe service conditions such as significant additional weight caused by liquid or solids buildup, effects
of wind loading, or possible failure of intermediate hangers. These are maximum spacings that must not be exceeded even when design may indicate a longer spacing.
Shorter spacings may be required due to other loads.

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NOTE 1—FLGs are optional.


NOTE 2—FLG bolt holes straddle major centerlines.
NOTE 3—FLG backs flat for SAE washers unless otherwise specified by purchaser.
NOTE 4—All units are in inches, unless otherwise specified.
Dimensions for Installation
Size IDA A B C F E G H
1 6 10 6 16 – – 6
1 1⁄ 4 6 10 6 16 – – 6
1 1⁄ 2 6 10 6 16 – – 6
2 6 10 6 16 4 15⁄8 6
2 1⁄ 2 7 12 6 18 6 21⁄2 6
3 7 12 6 18 6 2 1⁄ 2 6
4 8 14 6 20 6 2 1⁄ 2 6
6 10 16 8 24 9 33⁄4 8
8 12 20 10 30 12 5 8
10 14 24 10 34 15 61⁄4 10
12 16 26 12 38 18 71⁄2 10
14 18 30 12 42 21 83⁄4 12
16 20 32 14 46 24 10 12
18 21 36 14 50 27 111⁄4 12
20 22 38 16 54 30 121⁄2 12
24 24 42 18 60 36 15 12
30 30 52 20 72 45 185⁄8 15
36 33 62 22 84 54 221⁄2 15
42 36 72 24 96 63 261⁄8 15
48 39 81 26 107 72 297⁄8 15
54 42 91 26 117 81 331⁄2 15
60 45 99 28 127 90 371⁄4 15
72 54 117 34 151 72 297⁄8 18
84 60 136 36 172 84 343⁄4 18
96 66 154 38 192 96 393⁄4 18
A
All units measured in inches.

FIG. 4 Standard Duct Dimensions

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7.5 To determine minimum information for rectangular TABLE 2 Minimum Weld Widths
duct, use the longest side and increase to the nearest standard Minimum Cylinder Wall Thickness Minimum Total Weld Width
round-duct inside diameter. This diameter can be used to in. (mm) in. (mm)
determine the flange thickness, minimum wall thickness and 0.14 (3.6) 4 (101.6)
bolt-hole diameter, or tolerances. 0.18 (4.6) 5 (127.0)
0.22 (5.6) 6 (152.4)
7.6 There is no standard drilling pattern for rectangular duct. 0.30 (7.6) 6 (152.4)
Bolt-hole spacing shall be designed for a proper seal with a
maximum spacing of 41⁄2 in. (114.3 mm).
7.7 All bolt holes straddle major centerlines unless other- 9.2.2 The weld construction and thickness shall be that of
wise specified. the thickest section being joined (see Fig. 5).
9.2.3 All welds shall have a 6:1 taper minimum (see Fig. 5).
8. Tolerances 9.2.4 All gaps between mating ends of duct or fittings to be
less than 3⁄8 in. (9.5 mm).
8.1 Terminology for tolerances is given in 3.2. 9.2.5 All exposed cut edges to be coated in accordance with
8.2 Out of Roundness: 4.2.3.
#6-in. (152.4-mm) inside diameter, tolerance = ±1⁄16 in. (1.6 mm) 9.3 Flanges:
>6-in. inside diameter, tolerance = ±1⁄8 in. (3.2 mm) or ±1 % (whichever
is greater) 9.3.1 See Fig. 6 for flange attachment.
9.3.2 In a “flange on pipe” type flange, the same inner
not to exceed maximum = 3⁄4 in. (19.1 mm) surface and interior layer of the duct shall also be on the flange
8.3 Overall lengths shall be 61⁄4 in. (6.4 mm) maximum. face.
8.4 Cut ends of round duct shall be square within 61⁄8 in. 9.3.3 In an “integral” type flange the same inner surface and
(3.2 mm) for <24-in. (609.6-mm) inside diameter, 63⁄16 in. (4.8 interior layer must continue onto the flange face.
mm) for between 24 and 48-in. (609.6 to 1219.2-mm) inside 9.3.4 Flanges shall be vapor-tight at the design pressure
diameter, and 61⁄4 in. (6.4 mm) for ≥48-in. (1219.2-mm) inside when using a 1⁄8 in. (3.2 mm) thick 60 durometer gasket and
diameter. torqued to the recommended tightness in accordance with
Table 1.
8.5 Flanged or plain ends of duct and fittings must be within 9.3.5 Flanges shall be drilled with the pattern specified in
the following angles from their theoretical location: ≤24 in. Table 1 with bold holes straddling major centerlines unless
(609.6 mm) within 61°, >24 to ≤48 in. (1219.2 mm) within otherwise specified.
63⁄4 °, and >48 in. (1219.2 mm) within 61⁄2 °. 9.3.6 Back of flanges to be flat and parallel to provide a
8.6 Flange warpage = 63°; offset = 61⁄8 in. (3.2 mm); good seat for washers (see 8.8).
flange perpendicularity = 61⁄2 °; cant = 61⁄2 °, and flange 9.3.7 Flange construction shall be Type I or Type II in
flatness = 61⁄32 in. (0.8 mm) for ≤18-in. (457.2-mm) inside accordance with Specification C582.
diameter and 61⁄16 in. (1.6 mm) for >18-in. (457.2-mm) inside
diameter. 10. Inspection
8.7 For rectangular ducting for each side, increase the side 10.1 The finished laminate shall conform to visual accep-
to the nearest standard-round-duct inside diameter and use that tance criteria of Table 5 in Specification C582.
diameter to determine the tolerance for that particular side. 10.2 All dimensions shall be within the acceptable toler-
8.8 Back of flange shall be parallel with the flange face ances in Section 8.
within 61°, otherwise spotface for acceptable washer seating. 10.3 Barcol hardness shall be determined in accordance
(See Specification F436 for washer dimensions.) with Test Method D2583. Finished laminate shall have a
8.9 All corners of rectangular duct shall be radiused with minimum of 90 % of the resin manufacturer’s published Barcol
⁄ -in. (12.7-mm) radius for corners adjoining a wall ≤24 in.
12 hardness for a cured resin.
(609.6 mm) in length, 1-in. (25-mm) radius for corners 10.4 The finished laminate shall not be tacky in accordance
adjoining a wall between 24 and 48 in. (609.6 to 1219.2 mm) with the acetone sensitivity test. This involves application of a
in length, and 11⁄2-in. (38.1-mm) radius for corners adjoining a small amount of acetone to the surface, rubbing with finger
wall ≥48 in. (1219.2 mm) in length. until acetone evaporates and checking for tackiness. It is
recommended that gloves be worn while performing this test.
9. Fabrication
9.1 All reinforcing materials shall be overlapped in accor-
dance with Specification C582. Overlaps in subsequent plies
shall be staggered 2.25 in. (57.2 mm) minimum from overlaps
in the preceding ply.
9.2 Joints:
9.2.1 See Table 2 for minimum total weld widths. The weld
shall be centered on the joint within 1⁄2 in. (12.7 mm). FIG. 5 Weld Width and Thickness

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11.6 Support large sub-assemblies during shipment and
unloading, to prevent excessive deflection and over stressing.
11.7 Protect all flange surfaces with wooden blinds or other
approved material during shipment. Protect all ductwork, and
especially appurtenances that could be easily damaged, to
prevent shipping or handling damage.
11.8 Use full-face gaskets to eliminate any cantilever effect
caused from bolting.
11.9 Tighten bolting on flanged connections following
torque values given in Table 1. Tighten bolts following the
FIG. 6 Flange Attachment
sequential concept shown in Fig. 7. Use washers under bolt
heads and nuts.
10.5 Inspection at the manufacturer’s shop by the end user
is recommended. 11.10 The vendor shall specify the quantity of field-joining
kits subject to the concurrence of the customer. The vendor
11. Shipping, Handling and Installation4,5 shall supply material safety data sheets and field-joining
11.1 See Table 1 for recommended hanger spacing. instructions along with the joining materials.
11.2 Use properly designed hangers. Saddle supports should 11.11 Clean bonding surfaces to remove grease, oil, dirt,
have a minimum of 150° circumferential contact and one third moisture, or any other contaminants. In addition, sand or grind
of the diameter (2 in. (51 mm) minimum) longitudinal contact. surface to remove the surface gloss. Do not use solvents on any
Hanger supports should have 360° circumferential contact and freshly sanded or ground surfaces.
a longitudinal contact equal to diameter/12 with a minimum of 11.12 Anchor all joints to eliminate any movement during
2 in. (51 mm). the welding and curing process.
11.3 All other equipment or service loads shall be supported
independently. Use flexible connections to isolate ductwork 12. Keywords
from vibration caused by air-moving equipment. 12.1 chemical resistance; contact molding; ducts; flanges;
11.4 Because of the light weight of fiberglass ducts the polyester resin; reinforced plastic
primary determinants of the overall dimensions of the sub-
assemblies will be the dimensional shipping limitations. The
dimensions of the sub-assemblies shall be determined by the
manufacturer and the purchaser.
11.5 Unload the equipment with care and store in a location
where it will be free of damage. Impact of a tool or other heavy
object may result in a fracture of the inner lining and may affect
the service life.

4
Store resin, glass reinforcing and curing agents in a cool, dry area to maximize
shelf life.
5
Upon arrival at the installation site the customer shall examine the equipment
for damage in transit. If damage has occurred the customer shall file a claim with the
carrier. FIG. 7 Bolt Tightening Sequence

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4000 − 16

Standard Classification System for


Specifying Plastic Materials1
This standard is issued under the fixed designation D4000; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* responsibility of the user of this standard to establish appro-


1.1 This standard provides a classification system for tabu- priate safety, health, and environmental practices and deter-
lating the properties of unfilled, filled, and reinforced plastic mine the applicability of regulatory limitations prior to use.
materials suitable for processing into parts. 1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
NOTE 1—The classification system serves many of the needs of ization established in the Decision on Principles for the
industries using plastic materials. The standard is subject to revision as the
Development of International Standards, Guides and Recom-
need requires; therefore, the latest revision should always be used.
mendations issued by the World Trade Organization Technical
1.2 The classification system and subsequent line call-out Barriers to Trade (TBT) Committee.
(specification) is intended to be a means of identifying plastic
materials used in the fabrication of end items or parts. It is not 2. Referenced Documents
intended for the selection of materials. Material selection
2.1 ASTM Standards:2
should be made by those having expertise in the plastics field
D149 Test Method for Dielectric Breakdown Voltage and
after careful consideration of the design and the performance
Dielectric Strength of Solid Electrical Insulating Materials
required of the part, the environment to which it will be
at Commercial Power Frequencies
exposed, the fabrication process to be employed, the inherent
D150 Test Methods for AC Loss Characteristics and Permit-
properties of the material not covered in this document, and the
tivity (Dielectric Constant) of Solid Electrical Insulation
economic factors.
D256 Test Methods for Determining the Izod Pendulum
1.3 This classification system is based on the premise that Impact Resistance of Plastics
plastic materials can be arranged into broad generic families D257 Test Methods for DC Resistance or Conductance of
using basic properties to arrange the materials into groups, Insulating Materials
classes, and grades. A system is thus established which, D395 Test Methods for Rubber Property—Compression Set
together with values describing additional requirements, per- D412 Test Methods for Vulcanized Rubber and Thermoplas-
mits as complete a description as desired of the selected tic Elastomers—Tension
material. D471 Test Method for Rubber Property—Effect of Liquids
1.4 In all cases where the provisions of this classification D495 Test Method for High-Voltage, Low-Current, Dry Arc
system would conflict with the referenced ASTM specification Resistance of Solid Electrical Insulation
for a particular material, the latter shall take precedence. D569 Method for Measuring the Flow Properties of Ther-
moplastic Molding Materials (Withdrawn 1995)3
NOTE 2—When using this classification system the two-letter, three-
D570 Test Method for Water Absorption of Plastics
digit suffix system applies.
NOTE 3—When a material is used to fabricate a part where the D573 Test Method for Rubber—Deterioration in an Air
requirements are too specific for a broad material call-out, it is advisable Oven
for the user to consult the supplier to secure a call-out of the properties to D575 Test Methods for Rubber Properties in Compression
suit the actual conditions to which the part is to be subjected. D618 Practice for Conditioning Plastics for Testing
1.5 This standard does not purport to address all of the D624 Test Method for Tear Strength of Conventional Vul-
safety concerns, if any, associated with its use. It is the canized Rubber and Thermoplastic Elastomers

1 2
This classification system is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Materials. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2016. Published April 2016. Originally the ASTM website.
3
approved in 1982. Last previous edition approved in 2013 as D4000 - 13. DOI: The last approved version of this historical standard is referenced on
10.1520/D4000-16. www.astm.org.

*A Summary of Changes section appears at the end of this standard


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D4000 − 16
D635 Test Method for Rate of Burning and/or Extent and D1693 Test Method for Environmental Stress-Cracking of
Time of Burning of Plastics in a Horizontal Position Ethylene Plastics
D638 Test Method for Tensile Properties of Plastics D1784 Specification for Rigid Poly(Vinyl Chloride) (PVC)
D648 Test Method for Deflection Temperature of Plastics Compounds and Chlorinated Poly(Vinyl Chloride)
Under Flexural Load in the Edgewise Position (CPVC) Compounds
D695 Test Method for Compressive Properties of Rigid D1822 Test Method for Tensile-Impact Energy to Break
Plastics Plastics and Electrical Insulating Materials
D706 Classification System and Basis for Specifications for D1929 Test Method for Determining Ignition Temperature
Cellulose Acetate Molding and Extrusion Compounds of Plastics
(CA) D2116 Specification for FEP Resin Molding and Extrusion
D707 Classification System and Basis for Specification for Materials
Cellulose Acetate Butyrate Molding and Extrusion Com- D2137 Test Methods for Rubber Property—Brittleness Point
pounds (CAB) of Flexible Polymers and Coated Fabrics
D747 Test Method for Apparent Bending Modulus of Plas- D2240 Test Method for Rubber Property—Durometer Hard-
tics by Means of a Cantilever Beam (Withdrawn 2019)3 ness
D785 Test Method for Rockwell Hardness of Plastics and D2287 Specification for Nonrigid Vinyl Chloride Polymer
Electrical Insulating Materials and Copolymer Molding and Extrusion Compounds
D787 Specification for Ethyl Cellulose Molding and Extru- D2288 Test Method for Weight Loss of Plasticizers on
sion Compounds Heating (Withdrawn 2010)3
D788 Classification System for Poly(Methyl Methacrylate) D2565 Practice for Xenon-Arc Exposure of Plastics In-
(PMMA) Molding and Extrusion Compounds tended for Outdoor Applications
D789 Test Method for Determination of Relative Viscosity D2583 Test Method for Indentation Hardness of Rigid Plas-
of Concentrated Polyamide (PA) Solutions tics by Means of a Barcol Impressor
D790 Test Methods for Flexural Properties of Unreinforced D2584 Test Method for Ignition Loss of Cured Reinforced
and Reinforced Plastics and Electrical Insulating Materi- Resins
als D2632 Test Method for Rubber Property—Resilience by
Vertical Rebound
D792 Test Methods for Density and Specific Gravity (Rela-
D2843 Test Method for Density of Smoke from the Burning
tive Density) of Plastics by Displacement
or Decomposition of Plastics
D883 Terminology Relating to Plastics
D2863 Test Method for Measuring the Minimum Oxygen
D955 Test Method of Measuring Shrinkage from Mold
Concentration to Support Candle-Like Combustion of
Dimensions of Thermoplastics
Plastics (Oxygen Index)
D1003 Test Method for Haze and Luminous Transmittance
D2951 Test Method for Resistance of Types III and IV
of Transparent Plastics
Polyethylene Plastics to Thermal Stress-Cracking (With-
D1149 Test Methods for Rubber Deterioration—Cracking in
drawn 2006)3
an Ozone Controlled Environment D3012 Test Method for Thermal-Oxidative Stability of
D1203 Test Methods for Volatile Loss From Plastics Using Polypropylene Using a Specimen Rotator Within an Oven
Activated Carbon Methods D3159 Specification for Modified ETFE Fluoropolymer
D1238 Test Method for Melt Flow Rates of Thermoplastics Molding and Extrusion Materials
by Extrusion Plastometer D3222 Specification for Unmodified Poly(Vinylidene Fluo-
D1248 Specification for Polyethylene Plastics Extrusion ride) (PVDF) Molding Extrusion and Coating Materials
Materials for Wire and Cable D3275 Classification System for E-CTFE-Fluoroplastic
D1430 Classification System for Polychlorotrifluoroethylene Molding, Extrusion, and Coating Materials
(PCTFE) Plastics D3307 Specification for Perfluoroalkoxy (PFA) Resin Mold-
D1434 Test Method for Determining Gas Permeability Char- ing and Extrusion Materials
acteristics of Plastic Film and Sheeting D3350 Specification for Polyethylene Plastics Pipe and Fit-
D1435 Practice for Outdoor Weathering of Plastics tings Materials
D1499 Practice for Filtered Open-Flame Carbon-Arc Expo- D3418 Test Method for Transition Temperatures and En-
sures of Plastics thalpies of Fusion and Crystallization of Polymers by
D1505 Test Method for Density of Plastics by the Density- Differential Scanning Calorimetry
Gradient Technique D3638 Test Method for Comparative Tracking Index of
D1525 Test Method for Vicat Softening Temperature of Electrical Insulating Materials
Plastics D3713 Test Method for Measuring Response of Solid Plas-
D1562 Classification System and Basis for Specification for tics to Ignition by a Small Flame (Withdrawn 2000)3
Cellulose Acetate Propionate Molding and Extrusion D3763 Test Method for High Speed Puncture Properties of
Compounds (CAP) Plastics Using Load and Displacement Sensors
D1600 Terminology for Abbreviated Terms Relating to Plas- D3801 Test Method for Measuring the Comparative Burning
tics Characteristics of Solid Plastics in a Vertical Position

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D4000 − 16
D3892 Practice for Packaging/Packing of Plastics D4673 Classification System for and Basis for Specification
D3895 Test Method for Oxidative-Induction Time of Poly- for Acrylonitrile–Butadiene–Styrene (ABS) Plastics and
olefins by Differential Scanning Calorimetry Alloys Molding and Extrusion Materials
D3915 Specification for Rigid Poly(Vinyl Chloride) (PVC) D4745 Classification System and Basis for Specification for
and Chlorinated Poly(Vinyl Chloride) (CPVC) Com- Filled Polytetrafluoroethlyene (PTFE) Molding and Extru-
pounds for Plastic Pipe and Fittings Used in Pressure sion Materials Using ASTM Methods
Applications (Withdrawn 2015)3 D4804 Test Method for Determining the Flammability Char-
D3935 Classification System and Basis for Specification for acteristics of Nonrigid Solid Plastics
Polycarbonate (PC) Unfilled and Reinforced Material D4812 Test Method for Unnotched Cantilever Beam Impact
D3965 Classification System and Basis for Specifications for Resistance of Plastics
Rigid Acrylonitrile-Butadiene-Styrene (ABS) Materials D4894 Specification for Polytetrafluoroethylene (PTFE)
for Pipe and Fittings Granular Molding and Ram Extrusion Materials
D3985 Test Method for Oxygen Gas Transmission Rate D4895 Specification for Polytetrafluoroethylene (PTFE)
Through Plastic Film and Sheeting Using a Coulometric Resin Produced From Dispersion
Sensor D4976 Specification for Polyethylene Plastics Molding and
D4020 Specification for Ultra-High-Molecular-Weight Poly- Extrusion Materials
ethylene Molding and Extrusion Materials D4986 Test Method for Horizontal Burning Characteristics
D4066 Classification System for Nylon Injection and Extru- of Cellular Polymeric Materials
sion Materials (PA) D5021 Specification for Thermoplastic Elastomer–Chlori-
D4067 Classification System and Basis for Specification for nated Ethylene Alloy (TECEA) (Withdrawn 2007)3
Reinforced and Filled Poly(Phenylene Sulfide) (PPS) D5046 Classification for Fully Crosslinked Elastomeric Al-
Injection Molding and Extrusion Materials Using ASTM loys (FCEAs) (Withdrawn 2000)3
Methods D5048 Test Method for Measuring the Comparative Burning
D4101 Classification System and Basis for Specification for Characteristics and Resistance to Burn-Through of Solid
Polypropylene Injection and Extrusion Materials Plastics Using a 125-mm Flame
D4181 Classification for Acetal (POM) Molding and Extru- D5132 Test Method for Horizontal Burning Rate of Poly-
meric Materials Used in Occupant Compartments of
sion Materials (Withdrawn 2005)3
Motor Vehicles
D4203 Specification for and Basis for Specifications for
D5138 Classification System and Basis for Specification for
Styrene-Acrylonitrile (SAN) Injection and Extrusion Ma-
Liquid Crystal Polymers Molding and Extrusion Materials
terials
(LCP)
D4216 Specification for Rigid Poly(Vinyl Chloride) (PVC)
D5203 Specification for Polyethylene Plastics Molding and
and Related PVC and Chlorinated Poly(Vinyl Chloride)
Extrusion Materials from Recycled Post-Consumer
(CPVC) Building Products Compounds
(HDPE) Sources (Withdrawn 2016)3
D4329 Practice for Fluorescent Ultraviolet (UV) Lamp Ap-
D5204 Classification System and Basis for Specification for
paratus Exposure of Plastics
Polyamide-Imide (PAI) Molding and Extrusion Materials
D4349 Classification System and Basis for Specification for D5205 Classification System and Basis for Specification for
Polyphenylene Ether (PPE) Materials Polyetherimide (PEI) Materials
D4364 Practice for Performing Outdoor Accelerated Weath- D5279 Test Method for Plastics: Dynamic Mechanical Prop-
ering Tests of Plastics Using Concentrated Sunlight erties: In Torsion
D4396 Specification for Rigid Poly(Vinyl Chloride) (PVC) D5336 Classification System and Basis for Specification for
and Chlorinated Poly(Vinyl Chloride) (CPVC) Com- Polyphthalamide (PPA) Injection Molding Materials
pounds for Plastic Pipe and Fittings Used in Nonpressure D5420 Test Method for Impact Resistance of Flat, Rigid
Applications Plastic Specimen by Means of a Striker Impacted by a
D4474 Classification System for Styrenic Thermoplastic Falling Weight (Gardner Impact)
Elastomer Injection Molding and Extrusion Materials D5476 Classification System for Thermoplastic Polyure-
(TES) (Withdrawn 2008)3 thane Materials (TPU) (Withdrawn 2005)3
D4507 Specification for Thermoplastic Polyester (TPES) D5575 Classification System for Copolymers of Vinylidene
Materials (Withdrawn 1999)3 Fluoride (VDF) with Other Fluorinated Monomers
D4549 Classification System and Basis for Specification for D5593 Classification for Thermoplastic Elastomers—
Polystyrene and Rubber-Modified Polystyrene Molding Olefinic (TEO) (Withdrawn 2005)3
and Extrusion Materials (PS) D5628 Test Method for Impact Resistance of Flat, Rigid
D4617 Classification System for Phenolic Compounds (PF) Plastic Specimens by Means of a Falling Dart (Tup or
(Withdrawn 2012)3 Falling Mass)
D4634 Classification System and Basis for Specification for D5630 Test Method for Ash Content in Plastics
Styrene-Maleic Anhydride Molding and Extrusion Mate- D5676 Specification for Recycled Polystyrene Molding and
rials (S/MA) Extrusion Materials (Withdrawn 2004)3

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D4000 − 16
D5857 Specification for Polypropylene Injection and Extru- 2.2 Federal Standard:4
sion Materials Using ISO Protocol and Methodology Department of Transportation Federal Motor Vehicle Safety
D5927 Classification System for andBasis for Specifications Standard No. 302
for Thermoplastic Polyester (TPES) Injection and Extru- 2.3 Underwriters Laboratories:5
sion Materials Based on ISO Test Methods UL94 Standards for Tests for Flammability for Parts in
D5990 Classification System for Polyketone Injection Mold- Devices and Appliances
ing and Extrusion Materials (PK) (Withdrawn 2007)3 2.4 IEC and ISO Standards:6
D6314 Specification for Fluorocarbon Perfluoromethoxy IEC 600093 Recommended Methods of Tests for Volume
(MFA) Resin Molding and Extrusion Materials (With- and Surface Resistivities of Electrical Insulation Materials
drawn 2002)3 IEC 600112 Recommended Method for Determining the
D6338 Classification System for Highly Crosslinked Ther- Comparative Tracking Index of Solid Insulation Materials
moplastic Vulcanizates (HCTPV) Based on ASTM Stan- Under Moist Conditions
dard Test Methods IEC 600243 Recommended Methods of Test for Electrical
D6339 Classification System for and Basis for Specifications Strength of Solid Insulating Materials at Power Frequen-
for Syndiotactic Polystyrene Molding and Extrusion cies
(SPS) IEC 600250 Recommended Methods for the Determination
D6358 Classification System and Basis for Specification for of the Permittivity and Dielectric Dissipation Factor of
Poly (Phenylene Sulfide) (PPS) Injection Molding, Extru- Electrical Insulation Materials at Power, Audio, and Radio
sion and Blow Molding Materials Using ISO Methods Frequencies Including Metre Wavelengths
D6360 Practice for Enclosed Carbon-Arc Exposures of Plas- IEC 60695-2-12 Fire Hazard Testing—Part 2–12: Glowing/
tics Hot-Wire Based Test Methods—Glow-Wire Flammability
D6394 Specification for Sulfone Plastics (SP) Test Method for Materials
D6778 Classification System and Basis for Specification for IEC 60695-11-10 Fire Hazard Testing—Part 11-10: Test
Polyoxymethylene Molding and Extrusion Materials Flames—50 W Horizontal and Vertical Flame Tests
(POM) IEC 60695-11-20 Fire Hazard Testing—Part 11-20: Test
D6779 Classification System for and Basis of Specification Flames—500 W Flame Test Methods
for Polyamide Molding and Extrusion Materials (PA) ISO 62 Plastics—Determination of Water Absorption
D6835 Classification System for Thermoplastic Elastomer- ISO 75-1 Plastics—Determination of Temperature of De-
Ether-Ester Molding and Extrusion Materials (TEEE) flection Under Load—Part 1: General Principles
D6869 Test Method for Coulometric and Volumetric Deter- ISO 75-2 Plastics—Determination of Temperature of De-
mination of Moisture in Plastics Using the Karl Fischer flection Under Load—Part 2: Plastics and Ebonite
Reaction (the Reaction of Iodine with Water) ISO 178 Plastics—Determination of Flexural Properties of
D7209 Guide for Waste Reduction, Resource Recovery, and Rigid Plastics
Use of Recycled Polymeric Materials and Products (With- ISO 179 Plastics—Determination of Charpy Impact Strength
drawn 2015)3 of Rigid Materials
E29 Practice for Using Significant Digits in Test Data to ISO 180 Plastics—Determination of Izod Impact Strength of
Determine Conformance with Specifications Rigid Materials
E84 Test Method for Surface Burning Characteristics of ISO 294-4 Plastics—Injection Moulding of Test Specimens
Building Materials of Thermoplastic Materials—Part 4: Determination of
E96/E96M Test Methods for Water Vapor Transmission of Moulding Shrinkage
Materials ISO 527–1 Plastics—Determination of Tensile Properties—
E104 Practice for Maintaining Constant Relative Humidity Part 1: General Principles
by Means of Aqueous Solutions ISO 527-2 Plastics—Determination of Tensile Properties—
E119 Test Methods for Fire Tests of Building Construction Part 2: Test Conditions for Moulding and Extrusion
and Materials Plastics
E162 Test Method for Surface Flammability of Materials ISO 604 Plastics—Determination of Compressive Properties
Using a Radiant Heat Energy Source ISO 868 Plastics—Determination of Indention Hardness by
E662 Test Method for Specific Optical Density of Smoke Means of a Durometer (Shore Hardness)
Generated by Solid Materials
E1354 Test Method for Heat and Visible Smoke Release 4
Available from U.S. Government Printing Office Superintendent of Documents,
Rates for Materials and Products Using an Oxygen Con- 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
sumption Calorimeter www.access.gpo.gov.
5
Available from Underwriters Laboratories (UL), 333 Pfingsten Rd.,
F372 Test Method for Water Vapor Transmission Rate of
Northbrook, IL 60062-2096, http://www.ul.com.
Flexible Barrier Materials Using an Infrared Detection 6
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
Technique (Withdrawn 2009)3 4th Floor, New York, NY 10036, http://www.ansi.org.

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D4000 − 16
ISO 877 Plastics—Determination of Resistance to Change ISO 6721-1 Plastics—Determination of Dynamic Mechani-
Upon Exposure Under Glass to Daylight cal Properties—Part 1: General Principles
ISO 974 Plastics—Determination of the Brittleness Tem- ISO 6721-2 Plastics—Determination of Dynamic Mechani-
perature by Impact cal Properties—Part 2: Torsion-Pendulum Method
ISO 1133 Plastics—Determination of the Melt Mass-Flow ISO 9772 Cellular Plastics—Determination of Horizontal
Rate (MFR) and the Melt Volume-Flow Rate (MVR) of Burning Characteristics of Small Specimens Subjected to
Thermoplastics a Small Flame
ISO 1183 Plastics—Methods for Determining the Density ISO 9773 Plastics—Determination of Burning Behaviour of
and Relative Density of Non-Cellular Plastics Thin Flexible Vertical Specimens in Contact with a
ISO 2039-2 Plastics—Determination of Hardness—Part 2: Small-Flame Ignition Source
Rockwell Hardness ISO 11357-1 Plastics—Differential Scanning Calorimetry—
ISO 3795 Road Vehicles, Tractors, and Machinery for Agri- Part 1: General principles
culture and Forestry—Determination of Burning Behavior ISO 11357-3 Plastics—Differential Scanning Calorimetry—
of Interior Materials Part 3: Determination of Temperature and Enthalpy of
ISO 4577 Plastics—Polypropylene and Propylene— Melting and Crystallization
Copolymers—Determination of Thermal Oxidative Sta- 3. Terminology
bility in Air-Oven Method
3.1 Definitions—The definitions used in this classification
ISO 4589 Plastics—Determination of Flammability by Oxy-
system are in accordance with Terminology D883.
gen Index
ISO 4607 Plastics—Method of Exposure to Natural Weath- 4. Significance and Use
ering 4.1 The purpose of this classification system is to provide a
ISO 4892 Plastics—Methods of Exposure to Laboratory method of adequately identifying plastic materials in order to
Light Sources give industry a system that can be used universally for plastic
ISO 4892–4 Plastics—Methods of Exposure to Laboratory materials. It further provides a means for specifying these
Light Sources—Part 4: Open-flame Carbon-arc materials by the use of a simple line call-out designation.
ISO 5659 Plastics—Smoke Regeneration—Part 2: Determi-
4.2 This classification system was developed to permit the
nation of Optical Density by a Single-Chamber Test
addition of property values for future plastics.
ISO 6603-1 Plastics—Determination of Multiaxial Impact
Behavior of Rigid Plastics—Part 1: Falling Dart Method 5. Classification

TABLE 1 Standard Symbols for Generic Families With Referenced Standards and Cell Tables
Standard Symbol Plastic Family Name ASTMA Standard Suggested Reference Cell Tables for
Materials Without an ASTM StandardB
Unfilled Filled
ABA acrylonitrile-butadiene-acrylate E
ABS acrylonitrile-butadiene-styrene D3965, D4673
AMMA acrylonitrile-methyl methacrylate E
ARP aromatic polyester (see LCP)
ASA acrylonitrile-styrene-acrylate E
CA cellulose acetate D706
CAB cellulose acetate butyrate D707
CAP cellulose acetate proprionate E D
CE cellulose plastics, general E D
CF cresol formaldehyde H H
CMC carboxymethyl cellulose E
CN cellulose nitrate E D
CP cellulose propionate D1562
CPE chlorinated polyethylene F
CPVC chlorinated poly(vinyl chloride) D4396, D1784, D3915, D4216
CS casein H H
CTA cellulose triacetate E D
EC ethyl cellulose D787 E D
E-CTFE ethylene-chlorotrifluoroethylene copolymer D3275
EEA ethylene-ethyl acrylate F
EMA ethylene-methacrylic acid F
EP epoxy, epoxide H H
EPD ethylene-propylene-diene
EPM ethylene-propylene polymer F D
ETFE ethylene-tetrafluoroethylene copolymer D3159
EVA ethylene-vinyl acetate F
FCEA fully crosslinked elastomeric alloy D5046
FEP perfluoro (ethylene-propylene) copolymer D2116
FF furan formaldehyde H H
HCTPV highly crosslinked thermoplastic vulanizates D6338
IPS impact polystyrene (see PS)
LCP liquid crystal polymer D5138

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D4000 − 16
TABLE 1 Continued
Standard Symbol Plastic Family Name ASTMA Standard Suggested Reference Cell Tables for
Materials Without an ASTM StandardB
Unfilled Filled
MF melamine-formaldehyde H H
PA polyamide (nylon) D4066-94, D4066-01, D6779
PAEK polyaryletherketone
PAI polyamide-imide D5204 G G
PARA polyacryl amide
PB polybutene-1 F
PBT poly(butylene terephthalate) (see TPES)
PC polycarbonate D3935
PCTFE polymonochlorotrifluoroethylene D1430
PDAP poly(diallyl phthalate) H H
PE polyethylene D1248, D4976, D3350, D4020, D5203
PEBA polyether block amide
PEEK polyetheretherketone
PEI polyether-imide D5205
PEO poly(ethylene oxide)
PESU polyether sulfone D6394
PET poly(ethylene terephthalate), general (see TPES)
PETG glycol modified polyethylene terephthalate comonomer (see TPES)
PF phenol-formaldehyde D4617
PFA perfluoro alkoxy alkane D3307
PI polyimide G G
PIB polyisobutylene F
PK polyketone D5990
PMMA Poly(methyl methacrylate) D788 D
PMP poly(4-methylpentene-1) F
POM polyoxymethylene (acetal) D4181, D6778
POP polyphenylene oxide (see PPE)
PP polypropylene D4101, D5857
PPA polyphthalamide D5336, D6779
PPE polyphenylene ether D4349
PPH polyphenylene G H
PPOX poly(propylene oxide)
PPS poly(phenylene sulfide) D4067, D6358
PPSU poly(phenyl sulfone) D6394 G G
PS polystyrene D4549, D5676
PTFE polytetrafluoroethylene D1430, D3159, D3222, D3307, D4745,
D4894, D4895, D6314
PUR polyurethane F D
PVAC poly(vinyl acetate) F D
PVAL poly(vinyl alcohol) F D
PVB poly(vinyl butyral) F D
PVC poly(vinyl chloride) D2287 F D
PVDC poly(vinyl idene chloride) F D
PVDF poly(vinyl idene fluoride) D3222
PVF poly(vinyl fluoride) F D
PVFM poly(vinyl formal) F D
PVK poly(vinylcarbazole) F D
PVP poly(vinyl pyrrolidone) F D
SAN styrene-acrylonitrile D4203
SB styrene-butadiene E D
SI silicone plastics G G
S/MA styrene-maleic anhydride D4634
SMS styrene-methylstyrene E D
SP polysulfone D6394
SPS syndiotactic polystyrene D6339
TECEA thermoplastic elastomer-chlorinated ethylene alloy D5021
TEEE thermoplastic elastomer, ether-ester D6835
TEO thermoplastic elastomer-olefinic D5593
TES thermoplastic elastomer-stryenic D4474
TPE thermoplastic elastomer (see individual material)
TPES thermoplastic polyester (general) D4507, D5927
TPU thermoplastic polyurethane D5476
UF urea-formaldehyde H H
UP unsaturated polyester
VDF vinylidene fluoride D5575
A
The standards listed are those in accordance with this classification.
B
Cell Tables A and B have been reserved for the referenced standards and will apply to unfilled and filled materials covered in those standards.

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D4000 − 16
5.1 Plastic materials shall be classified on the basis of their 2 (class) = flame retarded, and 2 (grade) with requirements given in the
broad generic family. The generic family is identified by letter (PC) basic property table of Classification D3935.
NOTE 6—A previous edition of this standard used three digits for group,
designations as found in Table 1. These letters represent the
class, and grade; 0122 is equivalent to what was 122.
standard abbreviations for plastics in accordance with Termi-
nology D1600. 5.1.2 Basic property tables have been developed to sort the
commercially available unreinforced plastics into groups,
NOTE 4—For example: PA = polyamide (nylon), EMA = ethylene- classes, and grades. These tables are found in the standards
methacrylic acid, and EVA = ethylene-vinyl acetate.
listed in Table 1.
5.1.1 The generic family is classified into groups in 5.1.2.1 Where a standard does not exist for this classifica-
accordance, in general, with the chemical composition. These tion system the letter designation for the generic family will be
groups are further subdivided into classes and grades as shown followed by four 0’s and the use of cell table that applies (see
in the basic property table that applies. The letter designation 5.3).
applicable is followed by a four-digit number indicating group,
class, and grade. The first two digits indicate the group, the NOTE 7—Example—PI0000 would indicate a polyimide plastic (PI)
from Table 1, and 0000 indicating no basic property table requirements.
third digit the class, and the fourth digit the grade.
ASTM D4000 Line Call-Out 5.2 Reinforced or filled versions, or both of the basic
1 2 materials are identified by a single letter from Table 2 that
SPECIFIC indicates the reinforcement or filler, or both, used and two
Broad Group Class Grade digits that indicate the nominal quantity in percent by weight.
generic x x x x A second letter from Table 2A may be used to indicate the form
type or structure of the reinforcement or filler, or both, but is neither
1 = Two or more letters identify the generic family based on Terminology D1600.
2 = Four digits identify the specific chemical group, the modification or use necessary nor functional for mixtures. Thus, a letter designa-
class, and the grade by viscosity or level of modification. A basic property table tion G for glass and 33 for percent by weight, G33, specifies a
will provide property values.
reinforced or filled material with 33 percent by weight of glass,
The D4000 line call-out can be used only if the plastic is and another letter designation E following the G (that is, GE33)
listed in Table 1 and has no more than one material standard specifies a filled material with 33 percent by weight of glass in
referenced. If two or more standards are referenced for a the form of beads (or spheres or balls).
material, a direct D4000 line call-out is ambiguous. 5.2.1 The generic family is based on the broad chemical
NOTE 5—An example using the group, class, and grade is as follows: makeup of the base polymer. By its designation, certain
PC0122 would indicate: PC = polycarbonate, 01 (group) = polycarbonate, inherent properties are specified.
ASTM D4000 Line Call-Out
1 2 3 4 5 6 7
SPECIFIC CELL
REQUIREMENTS

Broad Group Class Grade Reinforcement % Table x x x x x Suffix


generic x x x x Reinforcement Physical
type Properties
1 = Two or more letters identify the generic family based on Terminology D1600.
2 = Four digits identify the specific chemical group, the modification or use class, and the grade by viscosity or level of modification. A basic property table will provide
property values.
3 = One letter indicates reinforcement type; an optional second letter indicates form of the reinforcement.
4 = Two digits indicate percent of reinforcement.
5 = One letter refers to a cell table listing of physical specifications and test methods.
6 = Five digits refer to the specific physical parameters listed in the cell table.
7 = Suffix codes indicate special requirements based on the application, and identify special tests (see Section 7).

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D4000 − 16

TABLE 2 Reinforcement-FillerA SymbolsB and Tolerance


Symbol Material Tolerance
C Carbon and graphite ±2 percentage points
D Alumina trihydrate ±2 percentage points
E Clay ±2 percentage points
F Cellulose ±2 percentage points
G Glass ±2 percentage points
H Aramid ±2 percentage points
J Boron ±2 percentage points
K Calcium carbonate ±2 percentage points
L Lubricants (for example, PTFE, graphite, and so forth) Depends upon material and process—to be specified
M Mineral ±2 percentage points
N Natural organic (cotton, sisal, hemp, flax, and so forth) ±2 percentage points
P Mica ±2 percentage points
Q Silica ±2 percentage points
R Combinations of reinforcements or fillers, or both ±3 percentage points
S Synthetic organic ±2 percentage points
T Talcum ±2 percentage points
V Metal ±2 percentage points
W Wood ±2 percentage points
X Not specified To be specified
A
Ash content of filled or reinforced materials, or both may be determined using either Test Method D5630 or ISO 3451–1 where applicable.
B
Additional symbols may be added to this table as required.

TABLE 2A Symbols for the Form or Structure of Fillers and Reinforcing Materials
Symbol Form or Structure
C Chips, cuttings
D Fines, powder
E Beads, spheres, balls
F Fiber
G Ground
H Whisker
K Knitted fabric
L Layer
M Mat (fabric, thick)
N Non-woven (fabric, thin)
P Paper
R Roving
S Flake
T Cord
V Veneer
W Woven fabric
X Not specified
Y Yarn

5.2.2 The requirements for special or reinforced materials entered as the cell number. Likewise, when an acceptable value
will use the classification system as described by the addition is not available in the cell table, the number 9 should be used
of a single letter that indicates the proper cell table in which the and a suffix used indicating the specific value (see 7.3). Thus,
properties are listed. A specific value is designated by the cell the letter designation “A” for cell table and 53380 for property
number for each property in the order in which they are listed values shall always be written A53380. The cell tables that may
in the table. When a property is not to be specified, a zero is be used for each generic family are listed in Table 1.

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D4000 − 16

The following three examples illustrate correct usage of the system. Note that the second example specifies one of two referenced standards shown in Table 1 of
D4000-09b.

The first example is for a cellulose triacetate containing 33 percent glass reinforcement and with the property requirements shown in Table D of ASTM D4000.

ASTM D4000-09b CTA0000 G33 D53380

Basic Requirements
ASTM D4000-09b CTA 00 0 0 G 33
_____ __ ____ __ __ _ _ _ __
| | | | | | |
Plastic Generic Group Class Grade Glass Percent
(cellulos (Other) (Other) (Other) Reinforced Glass
triacetate)

Cell Requirements
D 5 3 3 8 0
_ _ _ _ _ _
| | | | | |
Cell Table Tensile Flexural Izod Deflection Unspeci-
fied
Strength Modulus Impact Tempera-
ture

Requirements from Table D of Classification D4000 - 09b

The second example is for a PET copolymer with 30 percent glass reinforcement with the properties requirements shown in Table A of ASTM D5927-09.

ASTM D5927-09 TPES0310 G30 A22450

Basic Requirements
ASTM D5927-09 TPES 03 1 0 G 30
_____ __ ____ __ __ _ _ _ __
| | | | | | |
Plastic Generic Group Class Grade Glass Percent
(thermo- (polyethyl- (PET G) (Other) Reinforced Glass
plastic ene te-
polyester) rephthalate
copolymer)

Cell Requirements
A 2 2 4 5 0
_ _ _ _ _ _
| | | | | |
Cell Table Tensile Tensile Charpy Deflection Unspeci-
fied
Strength Modulus Impact Tempera-
ture

Requirements from Table A of Classification D5927 - 09

The third example is for a reinforced plastic where the shape or form of the reinforcement is included. The designation D4066 - 94b PA0120G33A53380 indicates
the following with the material requirements from Classification D4066 - 94b:
PA0120 = Nylon 66 heat stabilized from Table PA of Classifica-
tion D4066 - 94b,
G33 = Glass reinforced with 33 % glass, nominal, no require-
ment for shape or form,
A = Table A (D4066) for property requirements,
5 = Tensile strength, 175 MPa, min,
3 = Flexural modulus, 7500 MPa, min,
3 = Izod impact, 75 J/m, min,
8 = Deflection temperature, 235°C, min, and
0 = Unspecified.

NOTE 8—The type and amount of reinforcement are sometimes shown porated in this standard (preceding Section 17). These tables
on the supplier’s technical data sheet. If necessary, additional control of should be used in the same manner as the cell tables that appear
these reinforcements shall be accomplished by the use of the suffix part of
the system (Section 7). in the material specifications.
5.3 To facilitate the identification of new, special, and
reinforced materials where basic property tables are not pro-
vided in a material specification, cell tables have been incor-

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D4000 − 16
5.3.1 Although the values listed in cell tables include the enced standard is to be used. When the requirements for a
range of properties available in existing materials, that does not material are included in this standard, the following sections
imply that every possible combination of properties exists or are applicable.
can be obtained.
8. General Requirements
6. Basic Requirements 8.1 The composition of the specified material shall be
uniform and shall conform to the requirements specified
6.1 The main table or cell tables in the referenced ASTM
herein.
classification standard found in Table 1, are to be used to
develop a line call-out for each Plastic Family Name. A direct 9. Detail Requirements
D4000 line call-out can be used only if the plastic is listed in
Table 1 and has no more than one material standard referenced. 9.1 The material shall conform to the requirements pre-
scribed in the table (basic property, reinforced, cell, and suffix)
6.2 The cell tables included in this standard shall be used to as they apply.
develop a line call-out only for the materials not covered by a
9.2 For the purpose of determining conformance with this
classification standard in Table 1. When the existing main or
classification system, all specified limits, in this standard are
cell tables do not adequately describe the material, then
absolute limits as defined in Practice E29.
suffixes are used in place of, or in addition to, a cell table
designation. 9.3 With the absolute method, an observed value or a
calculated value is not rounded, but is to be compared directly
6.3 A line call-out assembled using this classification sys- with the specified limiting value. Conformance or nonconfor-
tem becomes a specification. The line call-out shall refer to the mance with the specification is based on this comparison.
standard used and contain the broad and specific type of
plastic, together with the appropriate identifiers followed by 10. Sampling
special suffix requirements, as they apply. The following 10.1 Sampling shall be statistically adequate to satisfy the
summarizes the line call-out and the entire system as detailed requirements of 15.4. A lot of material shall be considered as a
in this standard. unit of manufacture as prepared for shipment, and may consist
of a blend of two or more “production runs” or batches.
7. Suffix Requirements
7.1 When requirements are needed that supersede or supple- 11. Numbers of Tests
ment the property table or cell table requirements, they shall be 11.1 The number of tests conducted shall be consistent with
specified through the use of suffixes. In general, the first suffix the requirements of Sections 10.1 and 15.4.
letter indicates the special requirement needed and the second
letter indicates the condition or test method, or both, with a 12. Specimen Preparation
three-digit number indicating the specific requirement. The 12.1 The test specimens shall be molded as specified for the
suffixes that may be used are listed in Table 3 (following 16.1). specific materials under test in the ASTM standard specifica-
tions for the materials.
7.2 Basic requirements from property or cell tables, as they
apply, are always in effect unless these requirements are 13. Conditioning
superseded by special suffix requirements in the line call-out.
13.1 Condition the test specimens at 23 6 2°C and 50 6
NOTE 9—When using the suffixes for additional requirements of the 10 % relative humidity for not less than 40 h prior to testing for
material, the user must keep in mind that not all tests are routinely those tests where conditioning is specified unless otherwise
conducted by the supplier. When these requirements are necessary to
identify particular characteristics important to specific applications they
directed in the ASTM standard specification for the material.
shall be specified. 13.2 Conduct tests in the standard laboratory atmosphere of
7.3 The following is an example of a line call-out specifi- 23 6 2°C and 50 6 10 % relative humidity unless otherwise
cation with suffix for a reinforced nylon: directed in the ASTM standard specification for the material.
Suffix Requirements 13.3 For materials sensitive to atmospheric exposure, spe-
cial preparations for conditioning and test conditions should be
G A 140
| | |
adhered to as provided in the referenced standard for the
Specific Test Requirement material.
Gravity Method
| 14. Test Methods
Requirements from Suffix Table
Acceptable Line call-out format for above 14.1 Determine the properties enumerated in this classifica-
D6779 PA0120 G33 A53380 GA140 tion system by means of the test methods referenced.
ASTM D6779 Referenced Standard, latest issue
PA0120G33 Plastic Material Basic Cell
A53380 A Table Property Requirements 15. Inspection and Certification
GA140 Suffix Requirements
15.1 Inspection and certification of the material supplied
7.4 When a standard for a material is listed in Table 1, the under this classification system shall be for conformance to the
requirements of the referenced standard apply and the refer- requirements specified herein.

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D4000 − 16
15.2 Lot-acceptance inspection shall be the basis on which 15.5 A report of the test results shall be furnished when
acceptance or rejection of the lot is made. The lot-acceptance requested. The report shall consist of results of the lot-
inspection shall consist of those tests which ensure process acceptance inspection for the shipment and the results of the
control during manufacture as well as those necessary to ensure most recent periodic-check inspection.
certifiability in accordance with 15.4.
NOTE 10—If recycled plastics are allowed in the standard, insert the
15.3 Periodic check inspection shall consist of the tests following phrase after the word “shipment” in the last sentence of 15.5:
specified for all requirements of the material under this “and the percent by weight of recycled plastic, as defined in 3.1 of Guide
classification system. Inspection frequency shall be adequate to D7209, if requested.”
ensure the material is certifiable in accordance with 15.4.
15.4 Certification shall be that the material was manufac- 16. Packaging, Packing, and Marking
tured by a process in statistical control, sampled, tested, and 16.1 Provisions of Practice D3892 apply for packaging,
inspected in accordance with this classification system, and
packing, and marking of plastic materials.
that average values for the lot meet the requirements of the
specification (line call-out).

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D4000 − 16
TABLE 3 Suffix Symbols and RequirementsA
Symbol Characteristic
A Color (unless otherwise shown by suffix, color is understood to be natural)
Second letter A = does not have to match a standard
B = must match standard
Three-digit number 001 = color and standard number on drawing
002 = color on drawing
B Fluid resistance
Second letter A = reference fuel A, ASTM D471, aged 70 h at 23 ± 2°C
B = reference fuel C, ASTM D471, aged 70 h at 23 ± 2°C
C = ASTM #1 oil, ASTM D471, aged 70 h at 100 ± 2 °C
D = IRM 902 oil, ASTM D471, aged 96 h at 100 ± 2°C
E = IRM 903 oil, ASTM D471, aged 70 h at 100 ± 2°C
F = Distilled water, ASTM D471, aged 70 h at 100 ± 2°C
Three digit number is obtained from Suffix Table 1. It indicates change in hardness, tensile strength, elongation, and volume.
Example: BC 132 specifies that material, after aging in ASTM #1 oil for 70 h at 100°C, can have changed no more than 2 Shore D points,
5 % tensile strength, 15 % elongation, and 5 % in volume.
C Melting point—softening point
Second letter B = ASTM D1525, load 10 N, Rate A (Vicat)
C = ASTM D1525, load 10 N, Rate B (Vicat)
D = ASTM D3418 (Transition temperature DSC/DTA) (ISO 11357-1 and ISO 11357-3)
G = ISO 306, load 10 N, heating rate 50°C/h (Vicat)
H = ISO 306, load 10 N, heating rate 120°C/h (Vicat)
I = ISO 306, load 50 N, heating rate 50°C/h (Vicat)
J = ISO 306, load 50 N, heating rate 120°C/h (Vicat)
K = ASTM D1525, load 50 N, Rate A (Vicat)
L = ASTM D1525, load 50 N, Rate B (Vicat)
Three-digit number = minimum value °C
E Electrical
Second letter A = dielectric strength (short-time), ASTM D149 (IEC 600243)
Three-digit number × factor of 0.1 = kV ⁄mm, min
B = dielectric strength (step by step), ASTM D149 (IEC 600243)
Three-digit number × factor of 0.1 = kV ⁄mm, min
C = insulation resistance, ASTM D257 (IEC 600093)
Three-digit number × factor of 1014 = Ω, min
D = dielectric constant at 1 MHz, ASTM D150, max (IEC 600250)
Three-digit number × factor of 0.1 = value
E = dissipation factor at 1 MHz, ASTM D150, max (IEC 600250)
Three-digit number × factor of 0.0001 = value
F = arc resistance, ASTM D495, min
Three-digit number = value
G = volume resistivity, ASTM D257 (IEC 600093)
Three-digit number × factor of 1014 = Ω-cm, min
H = comparative tracking index, ASTM D3638, ac frequency, 50 Hz, 0.1 % ammonium chloride (IEC 600112)
Three-digit number = V, min
J = volume resistivity, ASTM D257 (IEC 600093), Ω-cm
K = surface resistivity, ASTM D257 (IEC 600093), Ω (per square)
First digit indicates:
1 = minimum requirement
2 = maximum requirement
Final two digits indicate the exponential value of the base 10
Example: EJ206 specifies a maximum volume resistivity of 106 Ω-cm
F Flammability
Second Letter A = Horizontal Burning Rate ASTM D635, UL94 HB, IEC 60695-11-10, Method A
Report as: (First three digits equal maximum burn rate in mm/min), next three significant digits × factor of
0.1 = thickness of tested sample in mm. If sample burns beyond the 100 mm mark, the samples
are considered to have no rating.
B = Oxygen Index ASTM D2863, ISO 4589
Report as: Value % O2 to three significant figures
C = Flash Ignition ASTM D1929, Procedure A
Report as: Value, °C min to three significant digits rounded to nearest whole number.
D = Self Ignition ASTM D1929, Procedure B
Report as: Value, °C min to three significant digits rounded to nearest whole number.
E = Ignition by a Small Flame ASTM D3713
Letter retired, standard withdrawn without replacement in 2000.
F = Vertical Burn Rating ASTM D3801, UL94 V, IEC 60695-11-10, Method B
Report as: (First digit = rating), next three significant digits × factor of 0.1 = thickness of tested sample in
mm.
Rating designations: 0 = V-0
1 = V-1
2 = V-2
if no rating, do not use “F”
000 = to be specified by user
G = Radiant Panel Test ASTM E162
Report as: Flame Spread
First two digits indicate minimum specimen thickness
00 to be specified 05 3.00 mm

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D4000 − 16
TABLE Continued
Symbol Characteristic
01 0.25 mm 06 6.00 mm
02 0.40 mm 07 9.00 mm
03 0.80 mm 08 12.70 mm
04 1.60 mm 09 >12.70 mm
Third digit indicates the flame spread
1 15 max 5 100 max
2 25 max 6 150 max
3 50 max 7 200 max
4 75 max 8 >200
H = Flame Spread Index ASTM E84
Report as: Flame Spread Index
NOTE 1: Smoke Developed Index may also be reported.
NOTE 2: Classifications may be used as per the International Building Code
Class I: Flame Spread 0–25
Class II: Flame Spread 26–77
Class III: Flame Spread 76–200
J = Automotive Horizontal ASTM D5132, FMVSS 302, ISO 3795
Burn Rate
Report as: (First three digits = maximum burn rate in mm/min), next three significant digits × factor of 0.1 =
thickness of tested sample in mm.
K= ASTM D2843
Letter retired, method no longer in broad commercial use, replaced by ASTM E662.
L= UL (IEC 60695-11-10)
Letter retired, see Appendix X1 for replacement procedures and references to the old requirements.
M = Vertical Burn Rating; FilmASTM D4804, UL94 VTM, ISO 9773
Report as: (First digit = rating), next three significant digits × factor of 0.1 = thickness of tested sample
tested in mm.
Rating designations: 0 = VTM0
1 = VTM1
2 = VTM2
if no rating, do not use “M”
N = Horizontal Burn Rate; ASTM D4986, UL94, ISO 9772
Foam
Report as: (First digit = rating), next three significant digits × factor of 0.1 = thickness of tested sample
tested in mm.
Rating designations: 0 = HBF
1 = HF-1
2 = HF-2
if no rating, do not use “N”
P = Glow Wire Flammability IEC 60695-2-12
Index
Report as: (First three digits are glow wire flammability index reported in °C). Following three significant dig-
its are thickness of sample tested in mm × factor of 0.1.
R = Heat Release Rate ASTM E1354
Report as: Peak Heat Release Rate
Rating Designations: (First three digits are peak heat release rate in kW/m2), next three digits are incident heat flux in
kW times ten (×10).
S = NBS Smoke (Flame or ASTM E662, ISO 5659–2
Smolder Mode)
Report as: (First digit = 1 for Flame mode or 2 for Smolder mode), final three digits = Specific Optical Den-
sity.
T = Fire Rating ASTM E119
Report as: (Fire resistance rating in hours, first two digits). Third digit = “1” for hose stream applied, “0” for
no hose stream applied. Fourth digit is application from table below:
Rating designations: 0: No application designated
1: Bearing Walls and Partitions
2: Nonbearing Walls and Partitions
3: Columns
4: Floors and Roofs
6: Loaded Restrained Beams
7: Protective Membranes in Wall, Partition, Floor, or Roof Assemblies
U = Large Flame Vertical ASTM D5048, UL94 5VA, IEC 60695-11-20
Burn Rating; Plaque
Report as: (First three digits = maximum burn time plus afterglow time in seconds after fifth flame
application), the fourth digit “1” or “0” for flaming drips (1 = yes, 0 = no), next three significant
digits × factor of 0.1 = thickness of tested sample tested in mm. Last digit: “1” or “0” for holes
burned through plaques (1 = yes, 0 = no).
V = Large Flame Vertical ASTM D5048, UL94 5VA, IEC 60695-11-20
Burn Rating; Bar
Report as: (First three digits = maximum burn time plus afterglow time in seconds after fifth flame
application), fourth digit “1” or “0” for flaming drips, last three significant digits × factor of 0.1 =
thickness of tested sample tested in mm.
G Specific gravity
Second letter A = ASTM D792 (tolerance ± 0.02) (ISO 1183 Method A)
B = ASTM D792 (tolerance ± 0.05) (ISO 1183 Method A)

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D4000 − 16
TABLE Continued
Symbol Characteristic
C = ASTM D792 (tolerance ± 0.005) (ISO 1183 Method A)
D = ASTM D1505 (tolerance ± 0.02)
E = ASTM D1505 (tolerance ± 0.05)
F = ASTM D1505 (tolerance ± 0.005)
H = ASTM D792/D 1505D1505 (max)
L = ASTM D792/D 1505D1505 (min)
Three-digit number × factor of 0.010 = requirement value
H Heat resistance, properties at temperature
Second letter A = heat aged for 70 h at 100 ± 2°C, ASTM D573
B = heat aged for 70 h at 150 ± 2°C, ASTM D573
C = heat aged for 70 h at 200 ± 2°C, ASTM D573
Three-digit number is obtained from Suffix Table 1. It indicates change in hardness, tensile strength, elongation and volume.
Second letter D = tested at 100 ± 2°C
E = tested at 125 ± 2°C
F = tested at 150 ± 2°C
Three-digit numbers obtained from Suffix Table 2. It indicates tensile strength, elongation, and tear strength.
Example: HE565 specifies that the material has a minimum of 15 MPA tensile strength, 400 % elongation, and a tear strength of 40 kN/m
when tested at 125°C.
Second letter L = low-temperature brittleness, ASTM D2137
Three-digit number indicates the temperature (°C) above which the material is non-brittle. Example: HL055 material is non-brittle according to
ASTM D2137a, above − 55°C.
I Not to be used at this time
J Hardness
Second letter A = ASTM D2240 (Type A) tolerance ±5 (ISO 868)
B = ASTM D2583 (Barcol), min
D = ASTM D2240 (Type D) tolerance ±3 (ISO 868)
E = ASTM D785 (Rockwell E), min
K = ASTM D785 (Rockwell K), min
L = ASTM D785 (Rockwell L), min (ISO 2039-2)
M = ASTM D785 (Rockwell M), min (ISO 2039-2)
R = ASTM D785 (Rockwell R), min (ISO 2039-2)
Three-digit number = value
K Tensile strength
Second letter B = at break, ASTM D638
C = at rupture, ASTM D412
D = tensile stress at break, ISO 527-1 and ISO 527-2
E = tensile stress at 50 % strain, ISO 527-1 and ISO 527-2
Three-digit number = value, MPa, min
Example: KC040 specifies a tensile strength at rupture of 40 MPa
M = tensile stress, ASTM D412
First digit indicates the elongation at which the tensile stress is measured.
1 = 25 %
2 = 100 %
3 = 300 %
Final two digits = value, MPa, min
N = tensile modulus, ISO 527-1 and ISO 527-2
P = modulus of elasticity, ASTM D638
Three-digit number × factor of 100 = value, MPa, min
S = tensile set, ASTM D412
First digit indicates the elongation at which the set is measured.
1 = 50 %
2 = 100 %
3 = at break
4 = 200 %
Final two digits indicate the maximum percent set.
Example: KS208 specifies a maximum tensile set of 8 % when tested at 100 % extension.
Y = yield, ASTM D638
X = tensile stress at yield, ISO 527-1 and ISO 527-2
Three-digit number = value, MPa, min
L Elongation
Second letter B = break, ASTM D638
C = break, ASTM D412
D = break, ISO 527
Three-digit number = value, %, min
R = resilience, ASTM D2632
First digit:
1 = minimum
2 = maximum
Final two digits indicate percent rebound
Example: LR 150 specifies a minimum rebound of 50 %
T = tear strength, ASTM D624 Die C
Three-digit number = value, kN ⁄m, min
Y = yield, ASTM D638
X = yield, ISO 527
Three-digit number = value, %, min

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D4000 − 16
TABLE Continued
Symbol Characteristic
M Moisture resistance or content
Second letter A = ASTM D570 (24-h immersion) (ISO 62)
B = ASTM D570 (2-h immersion)
C = ASTM D570 (long-term immersion)
D = ASTM D570 (1⁄2-h boiling water immersion)
E = ASTM D570 (48 h at 50°C immersion)
F = ASTM D6869 (ISO 15512, Method B), moisture content
Three-digit number × factor of 0.01 = value, percent max
N Flexural strength
Second letter A = ASTM D790, specimen = 3.2 × 13 × 76 mm, speed = 1.3 mm/min
B = ASTM D790, specimen = 6.4 × 13 × 127 mm, speed = 2.7 mm/min
C = ISO 178, specimen = 80 × 10 × 4 mm, speed = 2 mm/min, 64-mm span
Three-digit number = value, MPa, min
O Not to be used at this time
P Impact resistance
Second letter A = ASTM D256 (Test Method A, Izod)
000 = no break
Three-digit number = value, J ⁄m, min
B = ASTM D256 (Test Method B, Charpy)
Three-digit number = value, J ⁄m, min
C = ASTM D256 (Test Method C)
Three-digit number = value, J ⁄m, min
D = ASTM D256 (Test Method D)
Three-digit number = value, J ⁄m, min
E = ASTM D256 (Test Method E)
Three-digit number = value, J ⁄m, min
F = ASTM D5628
1 = Configuration FA
2 = Configuration FB
3 = Configuration FC
4 = Configuration FD
5 = Configuration FE
Two-digit number × 10 = value, J, min
G = ASTM D5420
1 = ASTM D5420 Configuration GA
2 = ASTM D5420 Configuration GB
3 = ASTM D5420 Configuration GC
4 = ASTM D5420 Configuration GD
5 = ASTM D5420 Configuration GE
Two-digit number × 10 = value, J min
H = ISO 6603-1, specimen = 2-mm thickness
Three-digit number = value, J
J = low-temperature brittleness, ISO 974
Three-digit number = –°C, max
K = ASTM D4812
Three-digit number × factor 10 = value, J/m, min
000 = no break
L = Low temperature brittleness, ASTM D746 (Procedure A)
Three-digit number = –°C, max
M = ISO 180/1A (Izod), specimen = 80 × 10 × 4 mm
N = ISO 179/1A (Charpy), specimen = 80 × 10 × 4 mm
Three-digit number × factor 0.1 = value kJ/m2, min
S = ASTM D1822, Type S, 3 mm thick
T = ASTM D1822, Type L, 3 mm thick
Three-digit number = value, kJ ⁄m2, min
U = ASTM D3763, specimen =3.2 mm thickness
First digit = test velocity
0 = 2.2 m/s
1 = 3.4 m/s
2 = 6.6 m/s
9 = other
Second Digit = Positive or Negative Value of ASTM D3763 Brittleness Temperature
0 = + and greater than
1 = + and less than
2 = - and less than
Third Digit = Brittleness Temperature, °C
0=0
1 = 10
2 = 20
3 = 30
4 = 40
5 = 50
6 = 70
7 = 100
8 = 150

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D4000 − 16
TABLE Continued
Symbol Characteristic
9 = unspecified
V = ASTM D3763, specimen = 3.2 mm thickness
First digit = test temperature, °C
0 = +23°C
1 = +10°C
2 = +0°C
3 = -10°C
4 = -15° C
5 = -20°C
6 = -30°C
7 = -40°C
8 = at ASTM D3763 Brittleness Temperature
9 = unspecified
Second digit = type of energy absorbed
0 = average total energy absorbed
1 = average energy absorbed at maximum load
Third digit = average energy absorbed, in J
0 = <5
1 = $5 and <10
2 = $10 and <20
3 = $20 and <30
4 = $30 and <40
5 = $40 and <50
6 = $50 and <70
7 = $70 and <100
8 = $100 and <150
9 = $150
When Suffix PV is to be reported, Suffix PU must also be reported in order that all test conditions are reported for the ASTM D3763 test.
Q Compressive strength
Second letter A = ASTM D695
B = ISO 604
Three-digit number = value, MPa, min
D = compression deflection, ASTM D575, Test Method A
First digit = % deflection
1=5%
2 = 10 %
3 = 15 %
4 = 20 %
5 = 25 %
6 = 30 %
7 = 40 %
8 = 50 %
Final two digits indicate minimum load in MPa
Example: QD445 specifies a minimum load of 45 MPa when deflected 20 %
S = compression set, ASTM D395, (Test Method B), run for 22 h.
First digit = test temperature
1 = 23± 2°C
2 = 70± 2°C
3 = 100± 2°C
4 = 125± 2°C
5 = 150± 2°C
Final two digits indicate maximum percent set.
R Volatile loss, gas and vapor permeability
Second letter A = ASTM D1203, Test Method A
B = ASTM D1203, Test Method B
C = ASTM D2288
D = ASTM D2584
Three-digit number × factor of 0.01 = value, percent, max
E = ASTM D3985
F = ASTM D1434 (Test Method M)
G = ASTM E96/E96M (Test Method E)
H = ASTM F372
First digit 1 = oxygen
2 = nitrogen
3 = carbon dioxide
4 = water vapor
5 = hydrogen
6 = methane
7 = Fuel C
8 = helium
9 = hydrogen sulfide

Second and third digit = value


00 = between user and producer
01 = 1.0 cm3·mil/m2·24 h·atm, max

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D4000 − 16
TABLE Continued
Symbol Characteristic
02 = 10.0 cm3·mil/m2·24 h·atm, max
03 = 100.0 cm3·mil/m2·24 h·atm, max
04 = 1.0 g·mil ⁄m2·24 h, max
05 = 10.0 g·mil ⁄m2·24 h, max
06 = 100.0 g·mil ⁄m2·24 h, max
(04 to 06 are water vapor units)
These units are currently the industry standard. Conversions to other units may be made using appendixes in ASTM D1434.
S Oxidative stability, mold shrinkage, and shear modulus
Oxidative stability tests
Second letter A = ASTM D3012 at 150°C (ISO 4577)
Three-digit number = value days to failure, min
C = ASTM D3895
Three-digit number = value minutes to failure, min
E = environmental stress crack resistance, ASTM D1693
Three-digit number = f20 h, min
T = thermal stress crack resistance, ASTM D2951
Three-digit number = h (without cracking), min
Mold shrinkage tests
H = ASTM D955 Mold shrinkage
First digit 1 = Compression molded bar
2 = Compression molded disk
3 = Transfer molded bar
4 = Transfer molded disk
5 = Injection molded bar
6 = Injection molded disk
7 = Injection molded plaque, 60 × 60 × 2 mm (ISO 294-4)
Two-digit number × factor 0.001 = value, mm/mm ± 0.001
Shear modulus tests
M = ASTM D5279, +23°C, 1 Hz (ISO 6721-1 and ISO 6721-2)
Three-digit number × factor 100 = value, MPa, min
T Transmission-haze
Second letter A = ASTM D1003, specimen 6.4 mm thick
B = ASTM D1003, specimen 3.2 mm thick
C = ASTM D1003, specimen 1.6 mm thick
First digit 1 = total luminous transmittance, min
2 = diffuse luminous transmittance, min
3 = haze, %, max
Second and third digit = value
U Flexural modulus, stiffness
Second letter A = ASTM D790, specimen = 3.2 by 13 by 76 mm, speed = 1.3 mm ⁄min
B = ASTM D790, specimen = 6.4 by 13 by 127 mm, speed = 2.7 mm ⁄min
C = ASTM D790 (secant modulus), Test Method I, Procedure A, specimen = 3.2 by 13 mm (1 % strain) speed = 1.3 mm/min
Three-digit number × factor 100 = value, MPa, min
D = stiffness, ASTM D747
First digit 1 = −30°C
Second and third digits × 1000 = value, MPa, max
First digit 2 = 23°C
3 = 70°C
Second and third digits × 1000 = value, MPa, min
Second letter E = ASTM D790, specimen-3.2 by 13 by 76 mm, speed − 1.3 mm ⁄min
F = ASTM D790, specimen = 6.4 by 13 by 127 mm, speed = 2.7 mm ⁄min
G = ASTM D790 (secant modulus), Method I, Procedure A, specimen = 3.2 by 13 by 76 (1 % strain) speed = 1.3 mm/min
M = ISO 178, chord modulus, specimen 80 × 10 × 4 mm, speed 2 mm/min, 64 mm span
Three digit number × factor 100 = value, MPa, max
N = ISO 178, chord modulus, specimen 80 × 10 × 4 mm, speed = 2 mm/min, 64-mm span
Three digit number × factor 100 = value, MPa, min
V Viscosity—flow rate
Second Letter A = relative viscosity, ASTM D789
Three-digit number = value, min
Second letter B = ASTM D1238 (ISO 1133)
First digit 1 = Condition 125 ⁄0.325
2 = Condition 125 ⁄2.16
3 = Condition 150 ⁄2.16
4 = Condition 190 ⁄0.325
5 = Condition 190 ⁄2.16
6 = Condition 190 ⁄21.60
7 = Condition 200 ⁄5.0
8 = Condition 230 ⁄1.20
9 = Condition 230 ⁄3.80
0 = Condition 265 ⁄12.5
Second letter C = ASTM D1238 (ISO 1133)
First digit 1 = Condition 275 ⁄0.325
2 = Condition 230 ⁄2.16
3 = Condition 190 ⁄1.05
4 = Condition 190 ⁄10.00

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D4000 − 16
TABLE Continued
Symbol Characteristic
5 = Condition 300 ⁄1.20
6 = Condition 190 ⁄5.0
7 = Condition 235 ⁄1.05
8 = Condition 235 ⁄2.16
9 = Condition 235 ⁄5.0
0 = Condition 250 ⁄2.16
Second letter D = ASTM D1238 (ISO 1133)
First digit 1 = Condition 310 ⁄12.5
2 = Condition 210 ⁄2.16
3 = Condition 285 ⁄2.16
4 = Condition 315 ⁄5.0
For second letters B, C, and D
Second and third digit = value
01 = 0.1 max
02 = >0.1 to 0.3
03 = >1 to 4
04 = >0.3 to 0.5
05 = >4 to 6
06 = >0.5 to 0.7
07 = >6 to 8
08 = >0.7 to 0.9
09 = >8 to 10
10 = >0.9 to 1.1
15 = >10 to 20
25 = >20 to 30
35 = >30 to 40
45 = >40 to 50
55 = >50 to 60
65 = >60 to 70
75 = >70 to 80
85 = >80 to 90
95 = >90 to 100
99 = >100
Second Letter E = flow temperature, ASTM D569
Three-digit number = minimum value °C
W Weather resistance
Second letter A = ASTM D1435 (ISO 4607)
First digit 1 = tensile strength change
2 = flexural strength change
3 = flexural modulus change
4 = weight change
5 = elongation change
6 = dimensional change
Second and third digit = value, percent, max
B = (enclosed carbon-arc type), ASTM D6360
000 = to be specified by user
C = Ozone resistance, ASTM D1149 (100-ppm ozone)
Three-digit number × factor of 10 = h for first crack, min
D = (fluorescent-UV-condensation type) ASTM D4329 (ISO 4892-3)
E = (xenon-arc type) ASTM D2565 (ISO 4892-2)
F = (fresnel concentrator type) ASTM D4364 (ISO 877)
G = (open-flame carbon-arc) ASTM D1499 (ISO 4892-4)
000 = to be specified by user
X Humidity aging and accelerated service
Second letter A = ASTM E104, Test Method A
B = ASTM E104, Test Method B
C = ASTM E104, Test Method C
First digit 1 = tensile strength change
2 = flexural strength change
3 = flexural modulus change
4 = weight change
5 = elongation change
6 = dimensional change
Second and third digit = value, %, max
Y Deflection temperature
Second letter A = ASTM D648, stress 1.82 MPa, unannealed specimen, width, 3.2 mm
B = ASTM D648, stress 1.82 MPa, unannealed specimen, width, 6.4 mm
C = ASTM D648, stress 1.82 MPa, unannealed specimen, width, 13 mm
D = ASTM D648, stress 0.455 MPa, unannealed specimen, width, 3.2 mm
E = ASTM D648, stress 0.455 MPa, unannealed specimen, width, 6.4 mm
F = ASTM D648, stress 0.455 MPa, unannealed specimen, width, 13 mm
G = ISO 75-1 and ISO 75-2, stress 1.80 MPa, unannealed specimen, positioned edgewise
H = ISO 75-1 and ISO 75-2, stress 0.450 MPa, unannealed specimen, positioned edgewise
I = ISO 75-1 and ISO 75-2, stress 1.80 MPa, unannealed specimen, positioned flatwise
J = ISO 75-1 and ISO 75-2, stress 0.450 MPa, unannealed specimen, positioned flatwise

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D4000 − 16
TABLE Continued
Symbol Characteristic
Three-digit number = value, °C, min
Z Other special requirement
Second letter from existing list of symbols where test or requirement is not available.
These characteristics will be spelled out in detail and identified in sequence that is, 01, 02, 03, etc.
Example ZW01
Type I, tensile bars (ASTM D638) when exposed 500 h to Type DH light source per ASTM G151 and G153 shall retain 50 % min of their
original tensile
strength.
Additional suffixes and requirements will be added to this classification system as test methods or requirements are developed or requested,
or both.
A
ISO documents listed in parentheses are similar to the ASTM documents and the same suffix may be applied.

SUFFIX TABLE 1 Property Change Table


Designation
Order Property 0 1 2 3 4 5 6 7 8 9
Number
1 Hardness change, Shore D points unspecified ±2 ±2 ±5 ±5 ±10 ±10 ±20 ±20 specify value
Tensile change, ASTM D412, % change, max unspecified ±5 ±10 ±10 ±20 ±20 ±40 ±40 ±60 specify value
2 Elongation change, ASTM D412, % change, max unspecified ±5 ±10 ±15 ±20 ±30 ±40 ±50 ±70 specify value
3 Volume change, ASTM D471, % change, max unspecified ±2 ±5 ±10 ±15 ±25 ±30 ±40 ±60 specify value
SUFFIX TABLE 2 Tensile, Elongation and Tear Properties
Designation
Order Property 0 1 2 3 4 5 6 7 8 9
Number
1 Tensile strength, ASTM D412, MPa, min unspecified 2 4 6 10 15 20 25 35 specify value
2 Ultimate elongation, ASTM D412, %, min unspecified 100 150 200 250 300 400 500 600 specify value
3 Tear strength, ASTM D624, KN/m, min unspecified 5 10 20 30 40 60 80 100 specify value
Cell Table C Detail Requirements
Designation
Order Property Cell Limits
Number
0 1 2 3 4 5 6 7 8 9
1 Tensile strength, ASTM D638, MPa, minA unspecified 35 45 50 55 65 70 75 85 specify value
2 Flexural modulus, ASTM D790, MPa, minA unspecified 1 500 2 000 2 200 2 300 2 400 2 600 2 900 3 000 specify value
3 Izod impact, ASTM D256, J/m, minB unspecified 15 30 50 135 270 425 670 950 specify value
4 Deflection temperature, ASTM D648, unspecified 80 90 100 110 120 130 140 150 specify value
(1820 kPa), °C, min
5 To be determined unspecified ... ... ... ... ... ... ... ... ...
A
MPa × 145 = psi
B
J/m × 18.73 × 10−3 = ft·lbf ⁄in.
Cell Table D Detail Requirements
Designation
Order Property Cell Limits
Number
0 1 2 3 4 5 6 7 8 9
1 Tensile strength, ASTM D638, MPa, minA unspecified 55 70 80 90 105 115 125 140 specify value
2 Flexural modulus, ASTM D790, MPa, minA unspecified 700 3 000 5 000 7 000 9 000 12 000 14 500 16 000 specify value
3 Izod impact, ASTM D256, J/m, minB unspecified 15 33 50 135 270 425 670 950 specify value
4 Deflection temperature, ASTM D648, unspecified 75 85 95 110 120 130 140 155 specify value
(1820 kPa), °C, min
5 To be determined unspecified ... ... ... ... ... ... ... ... ...
A
MPa × 145 = psi
B
J/m × 18.73 × 10−3 = ft·lbf ⁄in.

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D4000 − 16

Cell Table E Detail Requirements


Designation
Order Property Cell Limits
Number
0 1 2 3 4 5 6 7 8 9
1 Tensile strength, ASTM D638, MPa, minA unspecified 10 20 30 40 50 60 70 80 specify value
2 Flexural modulus, ASTM D790, MPa, minA unspecified 50 1 000 1 500 2 000 2 500 3 000 3 500 4 000 specify value
3 Izod impact, ASTM D256, J/m, minB unspecified 15 30 50 135 270 425 670 950 specify value
4 Deflection temperature, ASTM D648, unspecified 40 50 60 70 85 95 105 115 specify value
(1820 kPa), °C, min
5 To be determined unspecified ... ... ... ... ... ... ... ... ...
A
MPa × 145 = psi
B
J/m × 18.73 × 10−3 = ft·lbf ⁄in.

Cell Table F Detail Requirements


Designation
Order Property Cell Limits
Number
0 1 2 3 4 5 6 7 8 9
1 Tensile strength, ASTM D638, MPa, minA unspecified 3 10 15 25 35 40 50 60 specify value
2 Flexural modulus, ASTM D790, MPa, minA unspecified 10 700 1 000 1 400 1 900 2 400 2 900 3 400 specify value
3 Izod impact, ASTM D256, J/m, minB unspecified 15 30 50 135 270 425 670 950 specify value
4 Deflection temperature, ASTM D648, unspecified 25 40 55 70 80 90 100 110 specify value
(1820 kPa), °C, min
5 To be determined unspecified ... ... ... ... ... ... ... ... ...
A
MPa × 145 = psi
B
J/m × 18.73 × 10−3 = ft·lbf ⁄in.
Cell Table G Detail Requirements
Designation
Order Property Cell Limits
Number
0 1 2 3 4 5 6 7 8 9
1 Tensile strength, ASTM D638, MPa, minA unspecified 15 40 65 85 110 135 160 185 specify value
2 Flexural modulus, ASTM D790, MPa, minA unspecified 600 3 500 6 500 10 000 13 000 16 000 19 000 22 000 specify value
3 Izod impact, ASTM D256, J/m, minB unspecified 15 30 50 135 270 425 670 950 specify value
4 Deflection temperature, ASTM D648, unspecified 130 160 200 230 260 300 330 360 specify value
(1820 kPa), °C, min
5 To be determined unspecified ... ... ... ... ... ... ... ... ...
A
MPa × 145 = psi
B
J/m × 18.73 × 10−3 = ft·lbf ⁄in.
Cell Table H Detail Requirements
Designation
Order Property Cell Limits
Number
0 1 2 3 4 5 6 7 8 9
1 Tensile strength, ASTM D638, MPa, minA unspecified 15 55 95 135 175 215 255 290 specify value
2 Flexural modulus, ASTM D790, MPa, minA unspecified 200 4 500 9 000 13 000 17 000 20 000 25 000 30 000 specify value
3 Izod impact, ASTM D256, J/m, minB unspecified 15 30 50 135 270 425 670 950 specify value
4 Deflection temperature, ASTM D648, unspecified 35 100 160 230 290 350 420 480 specify value
(1820 kPa), °C, min
5 To be determined unspecified ... ... ... ... ... ... ... ... ...
A
MPa × 145 = psi
B
J/m × 18.73 × 10−3 = ft·lbf ⁄in.

17. Keywords
17.1 classification; classification system; line call-out;
plastic; plastic materials

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D4000 − 16
APPENDIX

(Nonmandatory Information)

X1. CODING OF FORMER SECTION “FL” IN TABLE 3

X1.1 In previous editions of this standard, section FL used


a three-digit code to designate performance. This code is as
follows:

L= UL (IEC 60695-11-10)
First digit indicates minimum specimen thickness.
Molding Materials Thin Films
mm µm
0 to be specified to be specified
1 0.25 25.0
2 0.40 50.0
3 0.80 75.0
4 1.60 100.0
5 2.50 125.0
6 3.00 150.0
7 6.00 175.0
8 12.70 200.0
9 >12.70 >200.0
Second digit indicates type of flame test
1 = Vertical (V) [Now Section FF]
2 = Horizontal (H) [Now Section FA]
3 = 125 mm flame (5V) [Now Section FU, FV]
4 = Vertical thin materials (VTM) [Now Section FM]
Third digit indicates the flame rating
0 = (94V ⁄94VTM) 0 - refer to UL94
1 = (94V ⁄94VTM) 1 - refer to UL94
2 = (94V ⁄94VTM) 2 - refer to UL94
3 = (94HB) 1 - burn rate < 40 mm/min
4 = (94HB) 2 - burn rate < 75 mm/min
5 = (94-5V) A no holes on plaques
6 = (94-5V) B with holes on plaques
7 = (94 foam) 1 refer to UL94
8 = (94 foam) 2 refer to UL94
9 = (94 foam) H refer to UL94

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4000 - 13)
that may impact the use of this standard. (April 1, 2016)

(1) Table 3, Suffix KP was added.

This section identifies the location of selected changes to this classification system. For the convenience of the
user, Committee D20 has highlighted those changes that may impact the use of this classification system. This
section may also include descriptions of the changes or reasons for the changes, or both.

D4000 – 13: (3) Removed a number of references in 2.1 because they refer
(1) Table 3, Suffixes FA, FJ, FU, FV: Burn rate was changed to to shapes or chemical resistance rather than thermoplastic
“maximum” burn rate. materials. The same references were also removed from Table
(2) Table 3, Suffixes FA, FJ, FU, FV, FF, FM, FN: Wording of 1. The standards referenced in Table 1 refer to material
next three significant digits were clarified to prevent confusion. standards only.
D4000 – 12: (4) Retained “withdrawn” material standards in Table 1 be-
(1) Rearranged table layout so that Tables 1, 2, and 2a all cause decades pass before they are forgotten.
appear in Section 5, which was extensively revised. (5) Listed two revision years of D4066 because they are not
(2) Placed Table 3 (suffixes) and cell tables between Sections identical in call-out identifications.
16 and 17.

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D4000 − 16
(6) Revised Section 5 to simplify the flow of material, arrang- (1) Revised paragraph 15.4.
ing things in order from the simpler to the more complex line (2) Added Note 10.
call-outs. D4000 – 03:
(7) Added a diagram showing the structure of the line call-out (1) Added ISO 1133 as an alternative test method to Test
for an unfilled material in 5.1.1. An example of such a call-out Method D1238.
is found in Note 5. (2) Editorially added to Table 1: ASTM Test Method D6779 to
(8) Subsection 5.2 introduces the call-out systems in use for PA, and Test Method D6778 to POM.
filled or reinforced plastics. Subsection 5.2.1 illustrates the D4000 – 01a:
structure of the call-outs used, and subsection 5.2.2 shows (1) Table 2 replaced with new data.
examples of line call-outs for three different, reinforced mate- (2) Table 2A added.
rials. (3) Revised 5.3 to address option of using Table 2A for shape
(9) Introduced the use of suffixes in Section 7, and the example or form.
shown in 7.3 has been rewritten to clarify the intent. (4) Added new Note 10 and renumbered subsequent notes.
(10) A number of minor editorial changes have been made. (5) Deleted “GA140” from the example in 5.1.1.
D4000 – 11: (6) Changed reference from “Specification” to Classification”
(1) Added examples to Note 4. in Note 9.
(2) In 5.1.1, added statements concerning usage of D4000 and (7) Editorially changed 2.1 and Table 1 to include new stan-
altered examples to illustrate correct usage. dards.
(3) In Sections 6.1, 6.3, and 7.4, added statements concerning (8) Editorially corrected Note 7.
correct usage of D4000. D4000 – 01:
(4) In Note 6, Note 9, Note 10, and in 7.3, corrected examples (1) Second letters J and K added for Symbol E in Table 3.
to conform to statements in 5.1.1. (2) Second letter G added for Symbol W in Table 3.
(5) Revised relative humidity tolerance requirements to con- (3) Referenced Documents were updated to reflect the revi-
form with Condition A of the latest issue of Practice D618. sions to Table 3.
D4000 – 09b: D4000 – 00a:
(1) Replaced reference to Guide D5033 with Guide D7209. (1) Referenced Documents were updated to reflect the revi-
(2) Revised Note 10 to reflect the replacement of Guide D5033. sions to Table 3.
D4000 – 09a: (2) Table 3, Symbol B: ES 27 was removed; incorporated in
(1) Added D3763 under Section 2. Test Method D471.
(2) In Table 3, Suffix Symbols under Symbol P added second (3) Table 3, Symbol C: Removed second letters A and E and
letter U = ASTM D3763 and definition of numbers. added second letters K and L for Test Method D1525, 50-N
(3) In Table 3, Suffix Symbols under Symbol P added second load.
letter V = ASTM D3763 and definition of numbers. (4) Table 3, Symbol D: Removed.
D4000 – 09: (5) Table 3, Symbol E: Added expression of results for second
(1) Revised suffix MF in Table 3. letter H.
D4000 – 08: (6) Table 3, Symbol F: Substituted IEC reference for Second
(1) Added polyphenylene (PPH) to Table 1. Letter A to replace withdrawn ISO standard. Deleted repetition
D4000 – 07: of the second letter L which referenced a deleted ASTM
(1) Revised parts A, F, J, N, P, U, and V of Table 3’s Section F. standard, Test Method F814.
Thickness was rounded to the nearest 0.1 mm, and will be (7) Table 3, Symbol K: Changed second letter M from tensile
reported to three significant digits in mm ×10. modulus to tensile stress.
(2) Revised parts C and D of Table 3’s Section F. The (8) Table 3, Symbol M: Added ISO reference for second letter
temperature was reported in whole numbers to three significant F.
digits. (9) Table 3, Symbol S: Deleted references to withdrawn
(3) Revised parts U and V of Table 3’s Section F. The time of standards, ASTM Test Method D2445 and ISO 537. Added
flaming and afterglow were reported in seconds. ISO 6721-1 and -2 as references for second letter M. Deleted
(4) An appendix was added for historical reference to deleted second letter P as it was a repeat of second letter M.
codes in Table 3. (10) Table 3, Symbol U: Added second letter N to permit
D4000 – 04: expression of flexural modulus by ISO 178 as a minimum
(1) Changed symbol FB from value % max to value % min in value.
Table 3. (11) Table 3, Symbol W: Added new ASTM standards for
D4000 – 03a: evaluating weather resistance.

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D4000 − 16
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of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4020 − 18

Standard Specification for


Ultra-High-Molecular-Weight Polyethylene Molding and
Extrusion Materials1
This standard is issued under the fixed designation D4020; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* tion system based on various characteristics and a range of viscosity


numbers determined in accordance with ISO 1628-3.
1.1 This specification provides for the identification of
1.8 This international standard was developed in accor-
virgin, natural color, unmodified homopolymer ultra-high-
dance with internationally recognized principles on standard-
molecular-weight polyethylene (UHMWPE) plastics molding
ization established in the Decision on Principles for the
and extrusion materials. This identification is made in such a
Development of International Standards, Guides and Recom-
manner that the seller and purchaser can agree on the accept-
mendations issued by the World Trade Organization Technical
ability of different commercial lots or shipments.
Barriers to Trade (TBT) Committee.
1.2 This specification also provides guidance for the char-
acterization of UHMWPE materials based on various 2. Referenced Documents
mechanical, thermal, electrical, and other analyses. 2.1 ASTM Standards:2
1.3 It is not intended to differentiate between various D883 Terminology Relating to Plastics
molecular weight grades of ultra-high-molecular-weight poly- D1601 Test Method for Dilute Solution Viscosity of Ethyl-
ethylene commercially available. ene Polymers
2.2 ISO Standards:3
1.4 It is not the function of this specification to provide
ISO 11542-1 Plastics—Ultra High Molecular-Weight Poly-
specific engineering data for design purposes.
ethylene (PE-UHMW) Moulding and Extrusion
1.5 Ultra-high-molecular-weight polyethylenes, as defined Materials—Part 1: Designation System and Basis for
in this specification, are those linear polymers of ethylene Specification
which have a relative viscosity of 1.44 or greater, in accor- ISO 1628-3 Plastics—Determination of Viscosity Number
dance with the test procedures described herein. and Limiting Viscosity Number—Part 3: Polyethylenes
1.6 The values stated in SI units are to be regarded as the and Polypropylenes
standard. The values given in parentheses are for information
3. Terminology
only.
1.7 The following precautionary caveat pertains only to the 3.1 Definitions—Definitions of terms used in this specifica-
test method portions in Section 7 and the Annex and tion are in accordance with Terminology D883.
Appendixes, of this specification: This standard does not 3.2 Definitions of Terms Specific to This Standard:
purport to address all of the safety concerns, if any, associated 3.2.1 ultra-high-molecular-weight polyethylene molding
with its use. It is the responsibility of the user of this standard and extrusion materials—as defined by this specification, those
to establish appropriate safety, health, and environmental substantially linear polyethylenes which have a relative viscos-
practices and determine the applicability of regulatory limita- ity of 1.44 or greater, at a concentration of 0.02 %, at 135°C, in
tions prior to use. decahydronaphthalene.
NOTE 1—This standard and ISO 11542-1 address the same subject
3.2.1.1 Discussion—It has been common practice to refer to
matter, but differ in technical content. ISO 11542-1 provides a classifica- the “molecular weight” of UHMWPE resins. The following
calculations shall be used to approximate the specific viscosity

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Materials. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Aug. 1, 2018. Published August 2018. Originally the ASTM website.
3
approved in 1981. Last previous edition approved in 2011 as D4020 - 11. DOI: Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D4020-18. 4th Floor, New York, NY 10036, http://www.ansi.org.

*A Summary of Changes section appears at the end of this standard


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(ηsp), reduced viscosity (ηred or R.S.V.), intrinsic viscosity (η 5. Materials and Manufacture
or I.V.), and the approximate nominal viscosity average mo- 5.1 The molding and extrusion material shall be UHMWPE
lecular weight of virgin resin. The calculations are shown as polyethylene in the form of powder or granules.
follows:
5.2 The molding and extrusion materials shall be as uniform
S
Relative viscosity 5 η r 5 t s 2
k
tsDS
/ to 2
k
to D (1)
in composition and size and as free of contamination as can be
achieved by good manufacturing practice. If necessary, the
level of contamination shall be agreed upon between the seller
Specific viscosity 5 η sp 5 η r 2 1
and the purchaser.
η sp 5.3 Unless controlled by requirements specified elsewhere
Reduced viscosity 5 η red 5 in this specification, the color and translucence of molded or
C
extruded pieces, formed under conditions recommended by the
The intrinsic viscosity is calculated by determining the manufacturer of the material, will be comparable within
reduced viscosity and extrapolating to infinite dilution, that commercial match tolerances to the color and translucence of
is, 0 % concentration. standard molded or extruded samples of the same thickness
Intrinsic Viscosity5 f η g 5 s 2η sp 22hlnhη rel 1⁄2 d ÷C supplied in advance by the manufacturer of the material.
Nominal Viscosity Molecular Weight55.373104 f η g 1.37
5.4 Additional test methods and conditions that are com-
where: monly used to characterize UHMWPE are listed in Table X4.1.
k = kinetic energy correction constant for the particular 5.4.1 Refer to Annex A2 for requirements regarding speci-
viscometer used, men preparation, dimensions, and conditioning requirements
ts = flow time of solution at 135°C, s, for these tests.
to = flow time of pure solvent at 135°C, s, and
C = concentration, %. 6. Sampling
NOTE 2—There are other equations being used in industry to calculate 6.1 A batch or lot shall be considered as a unit of manufac-
the nominal viscosity average molecular weights. Refer to Appendix X2 ture and can consist of a blend of two or more production runs
for the other equations and their relationship to the nominal viscosity of the same material.
average molecular weight equation in 3.2.1.1. The equation in 3.2.1.1 is
the only equation that shall be used for reporting of nominal viscosity
6.2 Unless otherwise agreed upon between the seller and the
average molecular weight. purchaser, prior to packaging, the material shall be sampled
NOTE 3—Use of the solution viscosity test on thermally processed based on adequate statistical sampling.
material is invalid due to inadequate solubility and possible crosslinking
7. Test Method
4. Classification 7.1 Dilute Solution Viscosity—Use Test Method D1601, as
modified in Annex A1.
4.1 It is recognized that dilute solution viscosity measure-
ments can only be made on virgin resin. Therefore, the 8. Keywords
following test and limits shall be used to determine the 8.1 extrusion materials; molding materials; plastics; poly-
properties of virgin polymer only. ethylene; ultra-high-molecular-weight; UHMWPE; viscosity

ANNEXES

(Mandatory Information)

A1. DILUTE SOLUTION VISCOSITY

A1.1 General Description

A1.1.1 The test sequence consists of dissolving UHMWPE A1.2.4 Erlenmeyer Flask, 250-mL, with glass stopper.
in decahydronaphthalene (0.02 g/100 mL) at 150°C and then A1.2.5 Vacuum Drying Oven.
measuring the relative viscosity at 135°C in an Ubbelohde No.
1 viscometer. It is possible to calculate the relative solution A1.2.6 Vacuum Aspirator.
viscosity from these experimental data. A1.2.7 Viscometer, Ubbelohde No. 1.
A1.2.8 Constant-Temperature Bath, 135 6 0.1°C, with a
A1.2. Apparatus 305-mm diameter by 460 mm (12 by 18-in.) tall glass jar as a
A1.2.1 Analytical Balance. container, and having a suitable support for the viscometer.
A1.2.2 Microscope Slide Cover Slip. A1.2.9 Buret, 100-mL capacity, 0.1-mL subdivisions.
A1.2.3 Hot Plate, with magnetic stirrer. A1.2.10 Stopwatch, 0.2-s reading.

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A1.2.11 Still, for decahydronaphthalene. the decahydronaphthalene, with stirring, to 150°C, and drop in
A1.2.12 Glass Funnel, with heating mantle. the UHMWPE and its slide cover slip. Continue stirring at
150°C for 1 h, with the flask lightly stoppered.
A1.3. Reagents A1.4.4 Viscosity Measurement:
A1.3.1 Decahydronaphthalene (Decalin), freshly distilled. A1.4.4.1 Place the clean viscometer into the constant-
A1.3.2 Tetrakis [methylene 3-(3',5'-di-tert-butyl-4'- temperature bath, fill with stabilized decahydronaphthalene,
hydroxyphenyl) propionate] methane (CAS No. 668-19-8). and allow the viscometer and solvent to come to thermal
equilibrium at 135 6 0.1°C. Determine the viscosity of the
NOTE A1.1—This may also be referred to as Tetrakis-(methylene-(3,5-
solvent. Clean the viscometer as directed in A1.4.2. It is
di-(tert)-butyl-4-hydrocinnamate))methane
essential that the whole viscometer be dry.
A1.4. Procedure A1.4.4.2 Meanwhile, place the flask of polymer solution
A1.4.1 Stabilized Decahydronaphthalene Preparation— into the 135°C bath and allow it to equilibrate. Transfer
Distill in accordance with Test Method D1601 and add 0.2 % sufficient solution to fill the viscometer to the mark (see Note
tetrakis [methylene 3-(3',5'-di-tert-butyl-4'-hydroxyphenyl) A1.2) and determine the viscosity of the solution.
propionate] methane. A1.4.4.3 Between uses, clean the viscometer as described in
A1.4.2. Prolonged waits between uses (overnight, etc.) will
A1.4.2 Cleaning the Viscometer—Empty the viscometer
require the use of the H2SO4 – K2Cr2O7 cleaning solution.
thoroughly by vacuum and completely refill the viscometer
with distilled, filtered, non-stabilized decahydronaphthalene. NOTE A1.2—Filling of the viscometer is made easier by the use of a
Place the viscometer into the 135°C hot oil constant tempera- glass funnel warmed with a heating mantle. This helps to prevent the
ture bath for at least 15-20 min. Completely drain the viscom- UHMWPE from precipitating.
eter and dry with dry air or nitrogen just prior to the next
measurement in order to prevent dilution and an erroneous A1.5. Calculation
measurement result. A1.5.1 Calculate the relative solution viscosity as follows:
A1.4.3 Solution Preparation—Dry the UHMWPE in a η r 5 ~ t s 2 k/t s ! / ~ t o 2 k/t o ! (A1.1)
vacuum oven for 2 h at 60°C. Weigh 14 to 17 mg of the dry
where:
UHMWPE onto a slide cover slip. Use the buret to transfer the
stabilized decahydronaphthalene at room temperature into the k = kinetic energy correction constant for the particular
Erlenmeyer flask, measuring, in milliliters, a volume equal to viscometer used,
4.5 times the UHMWPE weight in milligrams, for example, 15 ts = flow time of solution at 135°C, and
mg of UHMWPE and 67.5 mL of decahydronaphthalene. Heat to = flow time of pure solvent at 135°C.

A2. TEST SPECIMEN PREPARATION, DIMENSIONS, AND CONDITIONING REQUIREMENTS

A2.1 Test Specimens A2.2.1 Specimen dimensions shall conform to the require-
A2.1.1 Test specimen sheets shall be prepared from powder ments of the individual tests.
or granules and molded in accordance with the following A2.3 Conditioning
conditions.
Molding pressure 6.9 to 10.3 MPa A2.3.1 Condition the notched specimens at 23 6 2°C for
Platen temperature 196 to 210°C not less than 16 h prior to test.
Heating time 20 min at 196 to 210°C
Platen cooling rate 15 ± 2°C/min from 150 to 90°C
Below 90°C Maintain pressure and cool as quickly
A2.4 Test Conditions
as possible to <30°C
Platen temperature for demolding <30°C A2.4.1 Conduct the test in the standard laboratory atmo-
sphere of 23 6 2°C.
A2.2 Specimen Dimensions

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A3. IMPACT TEST METHOD FOR ULTRA-HIGH-MOLECULAR-WEIGHT POLYETHYLENE

A3.1 Scope

A3.1.1 This test method covers determination of the impact


strength of UHMWPE, which is extremely impact resistant.
When tested in accordance with Test Method D256, Method A,
UHMWPE generally gives the NBF type of failure, rendering
the test result invalid. This test method specifies the same type
of pendulum impact test machine as that given in Test Method
D256 but introduces a much higher degree of stress concen-
tration into the specimen by double notching with a razor
blade. Application of this test method shall be limited to the mm in.
A 6.35 ± 0.38 A 0.250 ± 0.015
characterization of virgin, unmodified UHMWPE resins, not B 12.70 ± 0.10 B 0.500 ± 0.004
commercially processed products. It is advised that the user be C 31.75 ± 0.25 C 1.250 ± 0.010
familiar with Test Method D256 before attempting to use this D 63.50 ± 0.38 D 2.500 ± 0.015
E 4.57 ± 0.08 E 0.180 ± 0.003
test method. F 0.00 ± 0.13 F 0.000 ± 0.005
θ 90° ± 2° θ 90° ± 2°
A3.1.2 The values stated in SI units are to be regarded as the
standard. FIG. A3.1 Dimensions of Double-Notched Izod Test Specimens
NOTE A3.1—This test method and Annex B of ISO 11542-2 address the
same subject matter, but differ in technical content and results shall not be
compared between the two test methods. direction of application of molding pressure: if applicable. The
A3.2. Referenced Documents impact resistance of a plastic material may be different if the
notch is perpendicular to, rather than parallel to, the direction
A3.2.1 ASTM Standards:2 of molding. The same is true for specimens cut with or across
D256 Test Methods for Determining the Izod Pendulum the grain of an anisotropic sheet or plate.
Impact Resistance of Plastics
A3.2.2 ISO Standards:3 A3.5.2 Notching shall be performed in a suitable machine
ISO 180 Determination of Izod Impact Strength of Rigid by pressing in a 0.23 6 0.03-mm thick single-edge razor blade
Materials with a 14 6 2° included angle at the cutting edge. The notching
ISO 11542-2 Plastics—Ultra-High Molecular Weight Poly- speed shall be less than 500 mm/min. A new blade shall be
ethylene (PE-UHMW) Moulding and Extrusion used after notching 40 specimens.
Materials—Part 2: Preparation of Test Specimens and A3.5.3 The calibration of the notching machine shall be
Determination of Properties checked by direct measurement of the notch depth,
perpendicularity, and offset of the two notches. One of the
A3.3. Apparatus possible measurement methods is given in Annex A4.
A3.3.1 The Izod-type impact machine that conforms to the
requirements of Test Method D256, including the calibration A3.6. Conditioning
and checking methods, shall be used. A3.6.1 Conditioning—Condition the notched specimens at
23 6 2°C for not less than 16 h prior to test.
A3.4. Test Specimen
A3.6.2 Test Conditions—Conduct the test in the standard
A3.4.1 The geometry and dimensions of the specimen are laboratory atmosphere of 23 6 2°C.
given in Fig. A3.1.
A3.4.2 The specimens shall be cut from a sheet compression A3.7. Procedure
molded in accordance with the conditions described in A2.1. A3.7.1 At least five and preferably ten individual determi-
A3.4.3 The width of the specimen shall be the thickness of nations of impact value must be made on each sample to be
the sheet if the sheet thickness is within 6.00 to 6.75 mm. Sheet tested under the conditions prescribed in A3.6.
material thicker than 6.75 mm shall be machined down to 6.35 A3.7.2 Measure the width of each specimen in the region of
6 0.25 mm. Sheet material thicker than 7.65 mm shall not be the notches twice with a micrometer to the nearest 0.025 mm,
used. and record its average width. Use an optical microscope to
A3.4.4 Each specimen shall be free of twist and shall be measure the distances between the notch roots on the two side
bounded by mutually perpendicular pairs of plane parallel surfaces of the specimen. Record the average value and
surfaces, free from scratches, pits, and sink marks. multiply this number by the width of the specimen to obtain the
remaining unnotched cross-section area, AR. Also record the
A3.5 Notching of Specimens identifying markings of the specimen.
A3.5.1 In the case of compression molding, the two notches A3.7.3 Estimate the breaking energy for the specimen and
(or width of two notches) shall be perpendicular to the select a pendulum of suitable energy. Start the test with a

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pendulum of 11 J if no prior test data are available. Use the indicated breaking strength of the specimen. If a pendulum of
lightest standard pendulum that is expected to break each improper energy was used, discard the result and make
specimen in the group with a loss of not more than 85 % of its additional tests on new specimens with the proper pendulum. If
energy. the proper pendulum was used, divide the net value so found
A3.7.4 Before testing the specimens, perform the following by the unnotched area AR of the specimen as measured in
operations on the machine: A3.7.2 to obtain its impact strength in kilojoules per square
A3.7.4.1 With the excess energy indicating pointer in its meter.
normal starting position, but without a specimen in the vise, A3.7.8 Record the type of failure for each specimen as one
release the pendulum from its normal starting position and note of the two coded categories defined as follows:
the position that the pointer attains after the swing as one (1) C, Complete Break—A break in which the specimen
reading of Factor A. separates into two pieces.
A3.7.4.2 Without resetting the pointer, raise the pendulum (2) NB, Non-Break—A break in which the specimen does
and release again, which will move the pointer up the scale an not separate into two pieces.
additional amount. Repeat this step if the pointer does not A3.7.9 Calculate the average impact strength and standard
move. Repeat this procedure until a swing causes no additional deviation of the group of specimens that results in complete
movement of the pointer, and note the final reading as one breakage. This test method requires that the specimen breaks
reading of Factor B. completely. The results obtained from unbroken specimens
A3.7.4.3 Repeat the above two operations several times, shall be considered a departure from standard and shall not be
and calculate and record the average A and B readings. reported as a standard result.
A3.7.5 Position the specimen precisely and rigidly but not
clamped too tightly in the vise. The relationship of the vise, A3.8. Report
specimen, and striking edge of the pendulum to one another is A3.8.1 Report the following information:
given in Fig. A3.2. Note that the top plane of the vise shall be
A3.8.2 Complete identification of the material tested, in-
0.13 6 0.13 mm below the notches.
cluding type, source, manufacturer’s lot number, and previous
A3.7.6 Release the pendulum and note and record the history;
excess energy remaining in the pendulum after breaking the
A3.8.3 Compression molding conditions;
specimen.
A3.8.4 Capacity of the pendulum, J;
A3.7.7 From the breaking strength of the specimen and
Factors A and B, determine the energy loss of the pendulum A3.8.5 Total number of specimens tested;
due to windage and friction using the correction charts from the A3.8.6 Number of those specimens that result in complete
commercial testing machine supplier. If these charts are not break;
available, use the method given in Appendix X2 or X3 of Test
A3.8.7 Average impact strength, kJ/m2;
Method D256. Subtract the correction so calculated from the
A3.8.8 Standard deviation; and
A3.8.9 Percent of specimens failing in each category, suf-
fixed by the corresponding letter code from A3.7.8.

A3.9. Precision and Bias


A3.9.1 Table A3.1 is based on a round robin conducted by
seven laboratories. For each material, all of the test specimens
were compression molded and machined at one source. Each
participating laboratory notched and tested five specimens of
each material.

TABLE A3.1 Precision of the Double-Notched Izod Impact Test


Method
Intrinsic Values, kJ/m2
Material Viscosity,
dl/g Mean SrA SRB IrC IRD
A 24 128.0 6.5 27.6 18.4 78.2
B 27 120.0 5.4 25.8 15.2 73.1
C 22 103.9 4.1 21.2 11.6 59.9
D 28 56.1 2.2 9.6 6.2 27.2
E 25 63.5 2.7 12.6 7.7 35.5
A
Sr = within-laboratory standard deviation of the average.
B
SR = between-laboratories standard deviation of the average.
C
Ir = 2.83 Sr.
FIG. A3.2 Relationship of Vise, Specimen, and Strike Edge to One D
IR = 2.83 SR.
Another

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A3.9.1.1 Repeatability, Ir(Comparing two test results for the A3.9.1.2 Reproducibility, IR(Comparing two test results for
same material, obtained by the same operator using the same the same material, obtained by different operators using differ-
equipment on the same day)—The two test results are judged ent equipment on different days)—The two test results are
not equivalent if they differ by more than the Ir value for that judged not equivalent if they differ by more than the IR value
material. for that material.

A4. MEASUREMENT METHOD OF IMPERFECTIONS IN SPECIMEN NOTCHING

A4.1 The following is one of the possible test methods for A4.2.2 Eyepiece, with a crosshair.
measuring the imperfections in specimen notching directly,
A4.2.3 Fiber Optic Illumination.
which can be classified into three kinds: (1) deviation from
perpendicularity, (2) incorrect notch-depth, and (3) offset of A4.3 Procedure
notches (Fig. A4.1).
NOTE A4.1—There is no known ISO equivalent to this method. A4.3.1 Lay the specimen on one of its sides and mount it
securely on the X-Y stage.
A4.2 Apparatus
A4.2.1 Reflective Optical Microscope, ocular, 40 to 60×, A4.3.2 The beginning and ending points of the notches are
with an X-Y stage accurate to 0.0025 mm. labeled from A to D in Fig. A4.1. Select one of the edges of the
specimen as the datum line from which the perpendicularity of
the notches to the edges is measured (in this case Line AE ¯ ).
Note that Point E is approximately 6.4 mm from Point A.
A4.3.3 Keep both the microscope and the base of the X-Y
stage stationary. Measure the coordinates of Points A to E with
respect to an arbitrarily selected coordinate system by moving
the X-Y stage and by targeting the points by the crosshair of the
eyepiece.
A4.4 Calculation
A4.4.1 The following equation is used to calculate the
perpendicularity of the notches:
m2 2 m1
/EAB 5 tan21 (A4.1)
11m 2 m 1

where:
¯ and AB
m1 andm2 = slopes of line AE ¯ with respect to the
coordinate system.
m1 and m2 are calculated from
y2 2 y1
m5 (A4.2)
x2 2 x1

where:
m = slope, and
(x1, y1) and (x2, y2) = coordinates of the end points of the
line.
The distance between two points, I, is obtained from the
following equation:
I 5 =~ x 2 2 x 1 ! 2 1 ~ y 2 2 y 1 ! 2 (A4.3)

The amount of offset of the notches is calculated from the


following equation:
FIG. A4.1 Notch Geometry of Double-Notched Izod Specimen ?
offset 5 AD? cos /DAE (A4.4)

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APPENDIXES

(Nonmandatory Information)

X1. ELONGATIONAL STRESS TEST METHOD FOR ULTRA-HIGH MOLECULAR-WEIGHT POLYETHYLENE

X1.1 Scope X1.4.4 Graduated weight set with hooks for suspension
X1.1.1 This test method covers the determination of elon- from the specimen holder. Recommended weights are approxi-
gational stress as a characterization of the melt viscosity of mately 700, 650, 600, 550, 500, 450, 400, 350, 300, 250, 200,
UHMWPE. The melt flow rate in accordance with test method 180, 150, 120, and 100 g.
D1238 cannot be determined for this material because ultra X1.4.5 Measuring instrument capable of measuring to 0.02
high molecular weight polyethylene does not have a melt flow. mm
The elongational stress is also be referred to as ZST and flow X1.4.6 Stopwatch
value, or both.
X1.4.7 Hot bath liquid (for example, silicone oil)
X1.1.2 Application of this test method shall be limited to
virgin, unmodified resin. The elongational stress method is X1.4.8 Compression molding press with controlled rate of
invalid on a previous thermally-processed material due to cooling of 15 6 2°C/min
possible crosslinking. X1.4.9 Positive compression mold with a minimum of 4
NOTE X1.1—This test method is identical to to Annex A of ISO 11542-2 grooves for venting and minimization of residual stress and
in the measurement of elongational stress. It is not equivalent to warpage. Capable of molding plaque or disk 1.4 mm in
ISO 11542-2 in any other measurement or section
thickness.
X1.2. Referenced Documents X1.4.10 Aluminum foil
2
X1.2.1 ASTM Standards: X1.4.11 Analytical balance, accurate to 60.1 g
D4703 Practice for Compression Molding Thermoplastic X1.4.12 Blender, high intensity
Materials into Test Specimens, Plaques, or Sheets
X1.2.2 ISO Standards: X1.5. Reagents
ISO 11542–2 Plastics – Ultra-high-molecular-weight poly-
X1.5.1 The addition of a mixture of a primary and second-
ethylene (PE-UHMW) Moulding and Extrusion – Part 2:
ary antioxidant to reduce the amount of crosslinking taking
Preparation of test specimens and determination of prop-
place in the specimens. The type and amount of antioxidant
erties
used will depend on the lab and the R2 value observed when
results are calculated.
X1.3. Terminology
X1.3.1 elongational stress—(in MPa) the tensile stress NOTE X1.2—A blend of Tris(2,4-di-(tert)butylphenyl)phosphite (CAS
No. 31570-0404) and Tetrakis [methylene 3-(3’,5’-di-tert-butyl-4’-
(force related to the initial cross-sectional area) required to hydroxyphenyl) propionate] methane (CAS No. 6683-19-8) at a 2:1 or 1:1
elongate a test specimen 600 % in a hot oil bath at 150°C in a ratio has been found to work well when added at between 0.4 and 0.75 %
10–min time period. by weight.
X1.3.2 tensile stress—(in MPa) the attached weight cor-
rected for the buoyancy effect divided by the measured initial X1.6. Procedure
cross-sectional area. X1.6.1 Test Plaque Preparation:
X1.6.1.1 Using the analytical balance weigh out the amount
X1.4. Apparatus of UHMWPE virgin material that will be needed to mold the
X1.4.1 Specimen die cutter number of plaques or disks required for the study. Based on the
amount of UHMWPE weighed, weigh the amount of antioxi-
X1.4.2 Specimen holder in accordance with Fig. X1.1 dant necessary to achieve a concentration capable of reducing
X1.4.3 Constant temperature bath with thermoregulator crosslinking. With the high intensity blender, mix the antioxi-
and circulating pump dant homogeneously into the UHMWPE.

FIG. X1.1 Test Specimen

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X1.6.1.2 Place the bottom half of the positive mold on a flat X1.6.4.2 Insert test specimen in the holder, hook the corre-
surface. Cover the bottom half with a piece of aluminum foil. sponding weight to the holder and suspend in bath. The mass
Weigh out the amount of the UHMWPE/antioxidant mix of the holder and weights shall be known to an accuracy of 0.1
necessary to fill the mold, make a full part, and minimize flash g.
and warpage. When this weight is established, this weight X1.6.4.3 After preheating five min, elongate specimen and
60.1 g shall be used consistently to ensure uniform moldings. record specimen elongation time. The elongation of test
Pour the weighed polymer into the mold cavity and spread it specimens does not take place at constant speed.
out into a smooth level surface. Cover with a second piece of X1.6.4.4 Repeat for the remaining specimens. The choice of
aluminum foil, then the upper portion of the positive compres- the six different weights used to load test specimens from the
sion mold. weights listed in X1.4.4 depends upon the molecular weight of
X1.6.1.3 A completely fused test plaque is prepared by the UHMWPE sample. The weights shall be selected so that a
compression molding. The following molding conditions are time of 1 to 20 min gives 600 % elongation in the narrow
proposed as guidelines: 1) 200°C under 12.7 MPa pressure for parallel-sided section of the test specimen.
20 min, 2) cool under pressure at a cooling rate of 15 6
2°C/min and 3) when the plaque or disk has cooled to below X1.7. Calculation
40°C, remove it from the mold. X1.7.1 The tensile stress in MPa on each individual speci-
X1.6.2 Test Specimens—Six specimens in accordance with men is calculated in accordance with the following equation:
Fig. X1.2 shall be die cut out of one test plaque. Each specimen T S 5 $ @ ~ M 1 1M 2 ! 3 0.00981# /A 1 3 B 1 % 3 @ 1 2 ~ ρ m /ρ w ! # (X1.1)
is tested using a different weight as described in X1.6.4.4.
TS = Tensile stress in MPa
X1.6.3 Measurement of Cross-sections—The width and M1 = Mass of selected weight
thickness at the narrow parallel-sided section of each of the six M2 = Mass of specimen holder
specimens shall be measured and recorded to the nearest 0.02 A1 = Initial thickness of test specimen (mm)
mm. B1 = Initial width of test specimen (mm)
X1.6.4 Elongational Stress Determination ρm = Density of the heat bath medium at 150°C
X1.6.4.1 Stabilize the bath at 150 6 2°C. ρw = Density of the metal at 150°C

FIG. X1.2 Specimen Holder

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D4020 − 18
Use log/log scale to plot tensile stress for the six specimens X1.8. Precision
against corresponding times for the 600 % elongation recorded
X1.8.1 The repeatability standard deviation has been deter-
in X1.6.4.4. Draw a best fit line through the six points and from
this graph, read off the tensile stress corresponding to a period mined to be 0.009 MPa for a material having an average
of 10 min. This value represents the elongational stress in MPa. elongational stress value of 0.516 MPa. This is based on a
single laboratory making 45 measurements over a period of
NOTE X1.3—An undue amount of scatter (R2 ≤ 0.95) or zero elongation time on one material. The reproducibility of this test method is
indicates that crosslinking has occurred in the test specimens. If this
occurs, repeat the test using specimens prepared using an increased not yet available.
amount of stabilizer. Increase the stabilizer level at least 50 % from what
was previously used.

X2. NOMINAL VISCOSITY AVERAGE MOLECULAR WEIGHT OF ULTRA-HIGH MOLECULAR-WEIGHT POLYETHYLENE

X2.1 Scope necessarily apply for another manufacturing process. As a


X2.1.1 The measurement of molecular weight of UHM- result, at least five equations have been developed to describe
WPE is nearly impossible to measure by techniques normally the molecular weight of UHMWPE.
used to measure molecular weight of other polymers. Tech- X2.1.3 Fig. X2.1 shows the relationship between the five
niques such as gel permeation chromatography (GPC) and light equations with respect to nominal viscosity average molecular
scattering used for other polymers are not useful for UHM- weight versus intrinsic viscosity.
WPE.
X2.1.2 The dilute viscosity test method can provide satis- X2.1.4 This appendix is being provided only as a reference.
factory correlations for viscosity average molecular weight Only Eq 1 listed in 3.2.1.1 of this specification shall be used to
within a specific manufacturing process, but this does not present data to the industry.

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FIG. X2.1 Known Molecular Weight Equations (Correlating with Intrinsic Viscosity)

X3. ABRASION INDEX OF UHMWPE USING AN ALUMINUM OXIDE SLURRY

X3.1 Scope X3.4.1.1 Motor—capable of maintaining a uniform rota-


X3.1.1 This method is used to determine the resistance of tional speed of 1750 rpm.
materials to abrasion, measured in terms of percent weight loss, X3.4.1.2 Stainless steel testing cups—140 mm (5.5 in.) deep
by rotating test specimens in a slurry consisting of 20 grit and 102 mm (4 in.) inside diameter, for holding specimens and
aluminum oxide and water. aluminum oxide slurry.
X3.1.2 The values stated in SI units are to be regarded as the X3.4.1.3 Stainless steel (SS) shafts—9 mm outside diameter.
standard. The values given in parentheses are for information X3.4.1.4 Metal cup supports—with dimensions of 3.2 mm
only. by 51 mm by 152 mm (1⁄8 in. by 2 in. by 6 in.)
NOTE X3.1—There is no known ISO equivalent to this method. X3.4.1.5 Thermocouple—positioned in the testing cup to
X3.2. Referenced Documents monitor slurry temperature.
X3.4.1.6 Gaskets—fitted into groove at the top of each
X3.2.1 ASTM Standards:2
testing cup to prevent leaking of slurry during motor rotation.
D618 Practice for Conditioning Plastics for Testing
D883 Terminology Relating to Plastics X3.4.1.7 Water bath—plastic glass container having dimen-
D1921 Test Methods for Particle Size (Sieve Analysis) of sions of 55 by 53 by 20 cm. Contains the water to cool the
Plastic Materials testing cups during operation.
D4703 Practice for Compression Molding Thermoplastic X3.4.1.8 Hydraulic jack—for raising the water bath up
Materials into Test Specimens, Plaques, or Sheets under the testing cups.
E691 Practice for Conducting an Interlaboratory Study to X3.4.1.9 Control panel—consisting of a timing device for
Determine the Precision of a Test Method automatic test termination after 2 h and other controls.
X3.3 Terminology X3.4.1.10 Water chiller—to maintain the water bath at 23 6
2°C.
X3.3.1 Definitions—For definitions related to plastics, see X3.4.1.11 Thermocouple—to verify the temperature of the
Terminology D883. water bath.
X3.4. Apparatus X3.4.2 Analytical balance—for weighing test specimens,
X3.4.1 Abrasion tester, consisting of: accurate to 0.0001 g.

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X3.4.3 Pan balance—with approximately a 1000 g capacity
for preparation of slurry.
X3.4.4 Vented rack—for air-drying specimens, to allow for
free circulation of air.

X3.5. Reagents
X3.5.1 Aluminum Oxide (Al2O3)—20 grit
NOTE X3.2—Perform incoming inspection on every lot of aluminum
oxide received by pulling an approximate 50-g sample from every fifth
bag or box of the lot. Perform a particle size analysis in accordance with
Test Methods D1921 using the following sieve sizes: 12, 16, 18, 20, 25,
and pan. The specification for the aluminum oxide shall be as specified in
Table X3.1.

X3.6. Test Specimen


X3.6.1 Test specimen sheets prepared from powder or
granules shall be 6.4 6 0.64 mm (0.25 6 0.025 in.) thick and Nominal Specimen dimensions
molded in accordance with Procedure C of Annex A1 of mm in.
length 69.85 2.75
Practice D4703. width 25.4 1.0
X3.6.2 Test specimens (Fig. X3.1) are machined from the thickness 6.35 0.25
large hole diameter 8.0 0.32
sheets. Dimensions of the test specimens shall be 69.85 6 0.64 small hole diameter 3.5 0.14
mm by 25.4 6 0.64 mm by 6.35 6 0.64 mm (2.75 6 0.025 in.
by 1.00 6 0.025 in. by 0.25 6 0.025 in.). Each specimen has FIG. X3.1 Abrasion Test Specimen Dimensions
a large and a small hole; 8.7 mm (11⁄32 in.) diameter and 3.6 mm
(9⁄64 in.) diameter drill bits, respectively. X3.8.5 Push the testing cup upwards, rotating slightly so the
specimen is fully immersed in the aluminum oxide/water
X3.7. Conditioning mixture.
X3.7.1 Conditioning—Condition the notched specimens at X3.8.6 Move the metal cup support under the cup. Push the
23 6 2°C for not less than 40 h prior to test. support tightly against the cup. Tighten the wing nuts evenly. If
X3.7.2 Test Conditions—Conduct the test in the standard not even, it is possible that the cup will rotate or tilt, leading to
laboratory atmosphere of 23 6 2°C. splattering of the aluminum oxide and result in greater speci-
men wear.
X3.8. Test Procedure
X3.8.7 Set the time to 120 min.
X3.8.1 Weigh each specimen to the nearest 0.0001 g and
record this weight at W1. A minimum of two specimens per X3.8.8 Raise the hydraulic jack so approximately the bot-
sample shall be tested. tom one-third of each testing cup is immersed in the water
bath. Turn on the water chiller.
X3.8.2 Using the pan balance and tared plastic cups, weigh
out in separate cups, 450 g of aluminum oxide and 300 g of X3.8.9 Turn on the main power and push the start button to
water. Pour the contents of each cup into the stainless steel begin the test.
testing cup. Repeat procedure for each of the stainless steel X3.8.10 When the test unit has shut off at the end of 2 h,
testing cups on the unit until all cups contain the aluminum turn off the main power and the water chiller. Lower the water
oxide/water mixture. bath so the testing cups are no longer immersed. Unscrew the
X3.8.3 Attach the specimens to the stainless steel shafts of wing nuts from each testing cup and remove the metal cup
the abrasion. Bolt the specimens to the shaft. Do not over- support. Remove each specimen from the shaft.
tighten the bolts as this will stress the specimen. X3.8.11 Using your fingernail, carefully remove any melted
X3.8.4 Inspect the gasket in each testing cup to insure it is material that remains attached to the specimen.
clean and properly positioned in the groove. X3.8.12 Clean the specimens with water and a brush, and
allow them to air-dry for a minimum of 2 h on the vented rack.
Insure that no water droplets are inside either of the two holes.
TABLE X3.1 Specification for Aluminum Oxide
USA Standard Tyler Equivalent Sieve Opening Specification Percent
X3.8.13 Reweigh the specimens and record this weight as
Sieve Number (mm) Number (µm) Retained W2.
1.70 12 1700 0
1.18 16 1180 20 max X3.9. Calculation
1.00 18 1000 45 min
Contents of 18 + 20 mesh screens—contents of 16 mesh 70 min X3.9.1 Calculate the percent of weight loss using the
screen following equation:
PAN PAN = 3 max
% weight loss 5 @ ~ W1 2 W2 ! /W1 # 3 100 (X3.1)

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D4020 − 18
where: TABLE X3.2 Precision Data, Abrasion Index
W1 = original weight of test specimen Values expressed in Units of %
Material Average SrA SRB,C rD RE,C
W2 = weight of test specimen after test M-19 IV 2.68 0.12 0.25 0.32 0.69
M-28 IV 2.47 0.16 0.20 0.45 0.55
X3.10. Report T-20 IV 2.43 0.16 0.21 0.46 0.59
T-28 IV 2.25 0.10 0.25 0.27 0.71
X3.10.1 Report the following information: A
Sr = Within laboratory standard deviation for the indicated material. It is obtained
X3.10.1.1 Complete identification and description of the by pooling the within-laboratory standard deviation of the test results from all of the
material tested, including source and manufacturer’s code, participating laboratories:
X3.10.1.2 Method of sample preparation, Sr = [[(S1)2 + (S2)2 .... + (Sn)2 ] /n]1/2
B
SR = between-laboratories reproducibility, expressed as standard deviation:
X3.10.1.3 Conditioning of specimens prior to testing, SR = [Sr2 + Sl2]1/2
X3.10.1.4 Length of abrasion time, if other than 120 min, Where
X3.10.1.5 Specimen number, initial weight of specimen Sl = standard deviations of laboratory means.
C
The calculated SR and R values in the table are based on data from three
(W1), final weight of specimen after abrasion (W2), and laboratories, which is insufficient to provide complete statistical data. However, SR
X3.10.1.6 Percent abrasion for each specimen and average and R are provided for information only and should not be used in the normal
percent abrasion for the sample. Report three significant manner.
D
r = within-laboratory critical interval between two test results = 2.8 × Sr
figures. E
R = between-laboratories critical interval between two test results = 2.8 × SR

X3.11. Precision and Bias


X3.11.1 Table X3.2 is based on a round robin4 conducted in X3.11.2 Concept of “r” and “R” in Table X3.2—If Sr and
1999 in accordance with Practice E691, involving four mate- SR have been calculated from a large enough body of data, and
rials tested by three laboratories. For each material, all samples for test results that were averages from testing 6 specimens for
were prepared at one source, but the individual specimens were each test result, then:
prepared at the laboratories which tested them. Each test result X3.11.2.1 Repeatability—Two results obtained within one
was the result of six individual determinations. Each laboratory laboratory shall be judged not equivalent if they differ by more
obtained 12 test results for each material. (Warning—The than the “r” value for the material (“r” is the interval repre-
explanations of “r” and “R” (X3.11.2 – X3.11.2.3) are only senting the critical difference between two test results for the
intended to present a meaningful way of considering the same material, obtained by the same operator using the same
approximate precision of this test method. The data in Table equipment on the same day in the same laboratory).
X3.2 are not to be applied to acceptance or rejection, as these X3.11.2.2 Reproducibility—Two test results obtained by
data apply only to the materials tested in the round robin and different laboratories shall be judged not equivalent if they
are unlikely to be rigorously representative of other lots, differ by more than the “R” value for that material (“R” is the
formulations, conditions, materials, or laboratories. The prin- interval representing the critical difference between two test
ciples outlined in Practice E691 are to be used to generate data results for the same material, obtained by different operators
specific to other materials and laboratories (or between specific using different equipment in different laboratories).
laboratories). The principles of X3.11.2 – X3.11.2.3 would X3.11.2.3 Any judgment in accordance with X3.11.2.1 or
then be valid for this data.) X3.11.2.2 would have an approximate 95 % (.95) probability
of being correct.
4
Supporting data are available from ASTM Headquarters. Request RR:D20- X3.11.3 There are no recognized standards by which to
1212. estimate bias of this method.

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X4. PROPERTIES AND TEST CONDITIONS FOR UHMWPE

TABLE X4.1 Common Properties and Test Conditions for UHMWPE


Properties Standard Specimen Type and Units Test Conditions and Supplementary
Dimensions (mm) Instructions
Rheological
Intrinsic Viscosity Specification D4020, Annex A1 Granules or powder Relative viscosity at 0.02 %
concentration in decalin

Mechanical Properties
Tensile Stress at Yield Test Method D638 and ISO 527-1 Test Method D638, Type 4 MPa 50 mm/min
Tensile Stress at Break ISO 527-1, Type 2 MPa
Tensile Elongation at Yield %
Tensile Elongation at Break % Measured when extensometer is
used
Nominal Strain at Break % Gage length is equal to grip distance
Tensile Modulus MPa ASTM 5 mm/min, 2 % secant
modulus ISO 1 mm/min, chord
modulus between 0.05 % and 0.25 %
strain

Elongational Stress Specification D4020, Appendix X2 Specimen specified in


Appendix X2

Flexural Modulus Test Methods D790 127 by 12.7 by 6.35 MPa 1 % secant, 101.6 mm span, 28 mm/
min crosshead speed

Double Notched Izod Impact Resistance Specification D4020, Annex A3 and 63.5 by 12.7 by 6.35 kJ/m2
Annex A4
Izod Impact Resistance Test Method D256 63.5 by 12.7 by 6.35 J/m
Charpy Impact Resistance ISO 11542-2, Annex B 120 by 15 by 10 KJ/m2
Hardness Test Method D2240, ISO 868 13 by 13 by 6.35 mm D Reading taken after 15 s

Thermal Properties
Deflection Temperature under Flexural Load Test Methods D648 127 by 12.7 by 6.35 °C 0.454 MPa stress, 0.25 mm
deflection,
2°C/min heating rate
Thermal Stress Cracking Test Methods D2951 125 × 6.4 × 1.25 h 6.4 mm diameter mandrels at 100°C
Melting Temperature ISO 3146 powder °C Method C, ramp rate 10°C/min
Coefficient of Linear Expansion ISO 10350 Cut from ISO 3167 multipur- 1/°C TMA, secant value over the tempera-
pose bar ture range of +23°C to +55°C
Flammability Test Method D635, IEC 60695-11-10 125 by 13 by 3 mm/min Linear burning rate of specimens in
horizontal position

Performance Properties
Abrasion Index Specification D4020, Appendix X3 69.8 by 25.4 by 6.35 % 1750 RPM, 2 h in aluminum oxide/
water slurry

Electrical Properties
Relative permittivity IEC 250 >60 by >60 by 1 Frequency 100 Hz and 1 MHz (com-
pensate for electrode edge effect)
Dissipation factor IEC 250 >60 by >60 by 1 Frequency 100 Hz and 1 MHz (com-
pensate for electrode edge effect)
Volume resistivity IEC 93 >60 by >60 by 1 Ω-m Voltage 100 V
Surface resistivity IEC 93 >60 by >60 by 1 Ω Voltage 100 V
Dielectric (Electrical) Strength IEC 243-1 >60 by >60 by 1 KV/mm Use 25 mm/75 mm coaxial-cylinder
>60 by >60 by 3 electrode configuration. Immerse in
IEC 296 transformer oil. Use short
time (rapid rise) test
Comparative Tracking Index (CTI) IEC 112 >15 by >15 by 4 Use solution A

Miscellaneous Properties
Density Test Methods D792, ISO 1183 50 by 12.7 by 6.35 (ASTM) g/cm3 Density by displacement
10 by 10 by 4 (ISO)
Bulk Density Test Methods D1895 Granules or powder g/cm3
Pourability Test Methods D1895 Granules or powder S Method A, tap funnel to start flow
Angle of Repose Test Method C1444 Granules or powder Angle in
degrees
Coefficient of Friction Test Method D1894, ISO 8295 63.5 by 63.5 by 6.35 UHMWPE against metal
Water Absorption ISO 62 50 by 50 by 3 or 50 dia. by 3 % 24 h immersion
disc
Yellowness Index Practice E313 50 by 50 by 6.35 2 degree observer, Illuminant C,
specular included, UV included,
hemispherical configuration

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D4020 − 18
X4.1. Referenced Documents ISO 527-1 Determination of tensile Properties, Part 1 Gen-
2 eral Principles
X4.1.1 ASTM Standards:
ISO 868 Plastics and Ebonite-Determination of Indention
C1444 Test Method for Measuring the Angle of Repose of
Hardness by Means of a Durometer (Shore Hardness)
Free-Flowing Mold Powders (Withdrawn 2005)5
ISO 1183 A Plastics—Methods for Determining the Density
D256 Test Methods for Determining the Izod Pendulum
and Relative Density of Non-cellular Plastics
Impact Resistance of Plastics
ISO 1628-3 Plastics—Determination of Viscosity Number
D635 Test Method for Rate of Burning and/or Extent and
and Limiting Viscosity Number—Part 3: Polyethylenes
Time of Burning of Plastics in a Horizontal Position
and Polypropylenes
D638 Test Method for Tensile Properties of Plastics
ISO 3146 Plastics—Determination of Melting Behavior
D648 Test Method for Deflection Temperature of Plastics
(Melting Temperature or Melting Range) of Semicrystal-
Under Flexural Load in the Edgewise Position
line Polymers
D790 Test Methods for Flexural Properties of Unreinforced
ISO 8295 Plastics—Film and Sheeting-Determination of
and Reinforced Plastics and Electrical Insulating Materi-
Coefficients of Friction
als
ISO 10350 Plastics—Acquisition and presentation of Com-
D792 Test Methods for Density and Specific Gravity (Rela-
parable Single-Point Data
tive Density) of Plastics by Displacement
ISO 11542–2 Plastics—Ultra High Molecular-Weight Poly-
D1894 Test Method for Static and Kinetic Coefficients of
ethylene (PE-UHMW) Moulding and Extrusion
Friction of Plastic Film and Sheeting
Materials—Part 2: Preparation of Test Specimens and
D1895 Test Methods for Apparent Density, Bulk Factor, and
determination of Properties
Pourability of Plastic Materials
X4.1.3 IEC Standards:3
D2240 Test Method for Rubber Property—Durometer Hard-
IEC 93 Recommended Methods of Test for Volume and
ness
Surface Resistivities of Electrical Insulating Materials
D2951 Test Method for Resistance of Types III and IV
IEC 112 Recommended Method for Determining the Com-
Polyethylene Plastics to Thermal Stress-Cracking (With-
parative Tracking Index of Solid Insulation Materials
drawn 2006)5
IEC 243-1 Recommended Methods of Test for Electric
E313 Practice for Calculating Yellowness and Whiteness
Strength of Solid Insulating Material at Power Frequen-
Indices from Instrumentally Measured Color Coordinates
cies
X4.1.2 ISO Standards:3 IEC 250 Recommended Methods for Determination of the
ISO 62 Plastics—Determination of Water Absorption Permittivity and Dielectric Dissipation Factor of Electrical
Insulation Materials at Power, Audio, and Radio Frequen-
cies Including Metre Wavelengths
5
The last approved version of this historical standard is referenced on IEC 60695-11-10 Fire Hazard Testing, Part 11–10 Test
www.astm.org. Flames 50 W Horizontal and Vertical Flames

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4020 - 11)
that may impact the use of this standard. (August 1, 2018)

(1) Updated ASTM and ISO references where appropriate. (5) Revised procedure for dilute solution viscosity to reflect
(2) Updated standard conditioning and test condition require- current practice.
ments. (6) Updated Figure X3.1 to align with impact testing described
(3) Moved Izod Impact Strength test from Appendix (non- in F648.
mandatory) to Annex (mandatory).
(4) Clarified equations and graphs for nominal viscosity aver-
age molecular weight.

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D4020 − 18
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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4024 − 15

Standard Specification for


Machine Made “Fiberglass” (Glass-Fiber-Reinforced
Thermosetting Resin) Flanges1
This standard is issued under the fixed designation D4024; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This specification covers reinforced-thermosetting resin 2.1 ASTM Standards:2
flanges other than contact-molded flanges. Included are re- D618 Practice for Conditioning Plastics for Testing
quirements for materials, workmanship, performance, and D883 Terminology Relating to Plastics
dimensions. D1599 Test Method for Resistance to Short-Time Hydraulic
Pressure of Plastic Pipe, Tubing, and Fittings
1.2 Flanges may be produced integrally with a pipe or
D1600 Terminology for Abbreviated Terms Relating to Plas-
fitting, may be produced with a socket for adhesive bonding to
tics
a pipe or fitting, or may be of the type used in conjunction with
D5421 Specification for Contact Molded “Fiberglass”
either a metallic or nonmetallic backup ring.
(Glass-Fiber-Reinforced Thermosetting Resin) Flanges
1.3 The values stated in inch-pound units are to be regarded D5685 Specification for “Fiberglass” (Glass-Fiber-
as the standard. The values in parentheses are given for Reinforced Thermosetting-Resin) Pressure Pipe Fittings
information only. In cases where materials, products, or equip- F412 Terminology Relating to Plastic Piping Systems
ment are available only in SI units, inch-pound units are 2.2 ANSI Standards:3
omitted. B 16.1 Cast Iron Pipe Flanges and Flanged Fittings
1.4 The following precautionary caveat pertains only to the B 16.5 Pipe Flanges and Flanged Fittings
test methods portion, Section 10, of this specification: This 3. Terminology
standard does not purport to address all of the safety concerns,
if any, associated with its use. It is the responsibility of the user 3.1 Definitions:
of this standard to establish appropriate safety, health, and 3.1.1 General—Definitions are in accordance with Termi-
environmental practices and determine the applicability of nology D883 or Terminology F412. Abbreviations are in
regulatory limitations prior to use. accordance with Terminology D1600, unless otherwise indi-
cated. The abbreviation for reinforced-thermosetting-resin pipe
NOTE 1—Contact molded flanges are covered in Specification D5421 is RTRP.
and referenced in Specification D5685.
NOTE 2—There is no known ISO equivalent to this standard. 4. Classification
1.5 This international standard was developed in accor- 4.1 General—This specification covers machine-made
dance with internationally recognized principles on standard- reinforced-thermosetting-resin flanges defined by type (method
ization established in the Decision on Principles for the of manufacture), grade (generic type of resin), class (configu-
Development of International Standards, Guides and Recom- ration of joining system), and pressure rating. Flanges com-
mendations issued by the World Trade Organization Technical plying with this specification are also given numerical classi-
Barriers to Trade (TBT) Committee. fications relating to burst pressure, sealing test pressure, and
bolt torque limit.

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Plastic Piping Systems and Chemical Equipment. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2015. Published June 2015. Originally the ASTM website.
3
approved in 1981. Last previous edition approved in 2012 as D4024 – 12. DOI: Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D4024-15. 4th Floor, New York, NY 10036, http://www.ansi.org.

*A Summary of Changes section appears at the end of this standard


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D4024 − 15
4.1.1 Types: TABLE 1 Pressure Categories
4.1.1.1 Type 1—Filament-wound flanges manufactured by Pressure Rating
Designation
winding continuous fibrous glass strand roving or roving tape, psi MPa
either preimpregnated or impregnated during winding, into a A 50 0.35
B 75 0.52
flange cavity under controlled tension. C 100 0.69
4.1.1.2 Type 2—Compression-molded flanges made by ap- D 125 0.86
E 150 1.04
plying external pressure and heat to a molding compound that F 175 1.21
is confined within a closed mold. G 200 1.38
4.1.1.3 Type 3—Resin-transfer-molded flanges manufac- H 225 1.55
J 250 1.73
tured by pumping a thermosetting resin into glass reinforce- K 300 2.07
ments that have been cut to size and clamped between matched L 350 2.42
molds. M 400 2.76
N 450 3.11
4.1.1.4 Type 4—Centrifugally-cast flanges are made by P 500 3.45
applying resin and reinforcement to the inside of a mold that is R 550 3.80
rotated and heated, subsequently polymerizing the resin sys- S 600 4.14
T 650 4.49
tem. U 700 4.83
4.1.2 Grades: V 750 5.18
4.1.2.1 Grade 1—Epoxy resin. W 800 5.52

4.1.2.2 Grade 2—Polyester resin.


4.1.2.3 Grade 3—Phenolic resin.
4.1.2.4 Grade 4—Vinylester resin. excess of 600 psi (4.1 MPa), a sealing test pressure of 225 psi
4.1.2.5 Grade 7—Furan resin. (1.6 MPa), and a bolt torque limit greater than 75 lbf·ft (102
4.1.3 Classes: N·m).
4.1.3.1 Class 1—Integrally-molded flange manufactured di- NOTE 3—Flanges with identical classification from different manufac-
rectly on a pipe section, pipe stub, or fitting. turers may not be interchangeable due to nonstandardization of pipe or
4.1.3.2 Class 2—Taper to taper adhesive joint flange manu- socket diameter, socket length, taper angle, or combination thereof.
factured with a tapered socket to be used in conjunction with a 5. Materials and Manufacture
pipe or fitting with a tapered spigot section and a suitable
adhesive. This joining method provides an interference fit over 5.1 Flanges manufactured in accordance with this specifi-
the entire length of the bond line. cation shall be composed of reinforcement imbedded in or
4.1.3.3 Class 3—Straight-taper adhesive joint flange manu- surrounded by cured thermosetting resin. The composite struc-
factured with a tapered socket to be used with a pipe or fitting ture may contain granular or platelet fillers, thixotropic agents,
with an untapered spigot section and a suitable adhesive. This pigments, or dyes.
joining method provides an interference fit at the bottom of the 5.2 The resins, reinforcements, and other materials, when
socket. combined as composite structure, shall produce a flange that
4.1.3.4 Class 4—Straight adhesive joint flange manufac- will meet the performance requirements of this specification.
tured with an untapered socket for use with a pipe or fitting
with an untapered spigot and a suitable adhesive. This joint 6. Performance Requirements
provides a pipe stop and may have an interference fit at the 6.1 The following performance requirements are intended to
bottom of the socket. provide classification and performance criteria for the purpose
4.1.4 Pressure Rating—Pressure rating shall be categorized of qualification testing and rating of prototype constructions
by a single letter designation. Pressure designations are shown and periodic reevaluation of the manufacturer’s stated ratings.
in Table 1. They are not intended as routine quality assurance require-
4.1.5 Burst pressure, sealing test pressure, and bolt torque ments for production runs of rated flanges.
limit shall be categorized by single capital letter designations 6.2 Flanges shall meet the following performance require-
as indicated by the cell classification system of Table 2. ments when joined for testing according to the manufacturer’s
4.2 Designation Code—The flange designation code shall recommended practice for field installation:
consist of the abbreviation RTR, followed by the type, grade, 6.2.1 Sealing—Flanges shall withstand a pressure of at least
and class in arabic numerals, the pressure rating category as a 1.5 times the rated design pressure without leakage when tested
capital letter, and three capital letters identifying the cell in accordance with 10.4.
classification designations of the burst pressure, sealing test 6.2.2 Short-Term Rupture Strength—Flanges shall withstand
pressure, and the bolt torque limit, respectively. Thus, a a hydrostatic load of at least four times their rated design
complete flange designation code shall consist of three letters, pressure without damage to the flange when tested in accor-
three numerals and one letter, and three letters. dance with 10.5.
4.2.1 Example—RTR-112E-EED. This designation de- 6.2.3 Bolt Torque—Flanges shall withstand, without visible
scribes a filament-wound, glass fiber-reinforced epoxy resin sign of damage, a bolt torque of at least 1.5 times that
flange with a taper to taper adhesive joining system. The flange recommended by the manufacturer for sealing of the flange at
has a 150 psi (1.40 MPa) pressure rating, a burst pressure in its rated pressure when tested in accordance with 10.6.

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TABLE 2 Burst Pressure, Sealing Test Pressure, and Bolt Torque Limit
A
Property X A B C D E F G H J K
Burst pressure, psi 200 300 400 500 600 700 800 900 1000 1200
(MPa) 1.38 2.07 2.76 3.45 4.14 4.83 5.52 6.21 6.90 8.27
Sealing test pressure, psi 75 115 150 190 225 265 300 340 375 450
(MPa) 0.52 0.79 1.03 1.31 1.55 1.83 2.07 2.34 2.59 3.10
Bolt torque limit, lbf·ft. 20 30 50 75 100 125 150 175 200 225
(N·m) 27.1 40.7 67.8 101.7 135.6 169.5 203.4 237.3 271.2 305.1

Property L M N P R S T U V W
Burst pressure, psi 1400 1600 1800 2000 2200 2400 2600 2800 3000 3200
(MPa) 9.65 11.03 12.41 13.79 15.17 16.55 17.93 19.31 20.69 22.06
Sealing test pressure, psi 525 600 675 750 825 900 975 1050 1125 1200
(MPa) 3.62 4.14 4.65 5.17 5.69 6.21 6.72 7.24 7.76 8.27
Bolt torque limit, lbf·ft. 250 275 300
(N·m) 339.0 372.9 406.8
A
X = unspecified

7. Content Requirements those contained in ANSI B 16.5. For all size flanges other
7.1 Recycled or Reprocessed Thermosetting Plastics— flange and bolt dimensions which meet internationally recog-
Flanges shall not contain any recylced or reprocessed thermo- nized standards such as ISO, DIN, JIS, BS, or GB can be used
setting plastics which might otherwise be added as fillers. as long as they are agreed to by the buyer and seller.
8.1.2 Flange Face—The flange face shall be perpendicular
8. Dimensions to the axis of the fitting within 1⁄2 °. The sealing surface of flat
8.1 Dimensions and Tolerances: face or serrated face flanges shall be flat to 61⁄32 in. (1 mm) for
8.1.1 Flange and Bolt Dimensions—Flanges of 24 in. (610 sizes up to and including 18 in. (457 mm) diameter and
mm) or smaller diameter shall conform to the values given in 61⁄16 in. (2 mm) for larger diameters.
Table 3A or 3B for bolt circle, number and size of bolt holes, 8.1.3 Washer Bearing Surface—Washer bearing surface
and outside diameter. Flanges larger than 24 in. (610 mm) in shall be flat and parallel to the flange face within 61°.
diameter shall conform to the values for bolt circle, number 8.2 Pipe Stop—Each adhesive joined flange shall provide
and size of bolt holes, and outside diameter for Class 125 cast sufficient taper or a diametric constriction to act as a stop
iron flanges in ANSI B 16.1. The tolerances for the flange during adhesive joining so that the pipe stub cannot project
dimensions provided in Table 3A and 3B shall be the same as beyond the face of the flange.

TABLE 3 A Flange Dimensions, in. (mm)A


Nominal Pipe, Outside Diameter Drilling
SizeB of Flange Diameter of Bolt Circle Diameter of Bolt Holes Number of Bolts Diameter of Bolts


12 3.50 (88.9) 2.38 (60.5) 0.62 (15.75) 4 12⁄ (12.70)

34 3.88 (98.6) 2.75 (69.9) 0.62 (15.75) 4 12⁄ (12.70)
1 4.25 (107.9) 3.12 (79.2) 0.62 (15.75) 4 12⁄ (12.70)
1 1⁄ 4 4.62 (117.3) 3.50 (88.9) 0.62 (15.75) 4 1⁄ 2 (12.70)
1 1⁄ 2 5.00 (127.0) 3.88 (98.6) 0.62 (15.75) 4 1 ⁄2 (12.70)

2 6.00 (152.4) 4.75 (120.6) 0.75 (19.0) 4 ⁄


58 (15.9)
2 1⁄ 2 7.00 (177.8) 5.50 (139.7) 0.75 (19.0) 4 ⁄
58 (15.9)
3 7.50 (190.5) 6.00 (152.4) 0.75 (19.0) 4 5⁄ 8 (15.9)
3 1⁄ 2 8.50 (215.9) 7.00 (177.8) 0.75 (19.0) 8 5⁄ 8 (15.9)
4 9.00 (228.6) 7.50 (190.5) 0.75 (19.0) 8 5⁄ 8 (15.9)
5 10.00 (254.0) 8.50 (215.9) 0.88 (22.4) 8 3⁄ 4 (19.0)
6 11.00 (279.4) 9.50 (241.3) 0.88 (22.4) 8 3⁄ 4 (19.0)
8 13.50 (342.9) 11.75 (298.4) 0.88 (22.4) 8 3⁄ 4 (19.0)
10 16.00 (406.4) 14.25 (361.9) 1.00 (25.4) 12 7⁄ 8 (22.2)
12 19.00 (482.6) 17.00 (431.8) 1.00 (25.4) 12 7⁄ 8 (22.2)

14 21.00 (533.4) 18.75 (476.2) 1.12 (28.4) 12 1 (25.4)


16 23.50 (596.9) 21.25 (539.8) 1.12 (28.4) 16 1 (25.4)
18 25.00 (635.0) 22.75 (577.8) 1.25 (31.7) 16 11⁄8 (28.6)
20 27.50 (698.5) 25.00 (635.0) 1.25 (31.7) 20 11⁄8 (28.6)
24 32.00 (812.8) 29.50 (749.3) 1.38 (35.1) 20 11⁄4 (31.7)
A
Dimensions conform to ANSI B16.5 for Class 150 steel flanges.
B
For larger sizes, see 8.1.1.

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TABLE 3 B Flange Dimensions, in. (mm)A (continued)

Diameter of Bolt Circle Diameter of Bolt Holes Number Diameter of


Nominal Pipe Size Outside Diameter of Flange
of Bolts
Bolts

12 3.75 (95.3) 2.62 (66.5) 0.62 (15.75) 4 12⁄ (12)

34 4.62 (117.3) 3.25 (82.6) 0.75 (19.0) 4 58⁄ (16)
1 4.88 (124.0) 3.50 (88.9) 0.75 (19.0) 4 5 ⁄8 (16)
1 1⁄ 4 5.25 (133.4) 3.88 (98.6) 0.75 (19.0) 4 5 ⁄8 (16)
1 1⁄ 2 6.12 (155.4) 4.50 (114.3) 0.88 (22.4) 4 3 ⁄4 (18)

2 6.50 (165.1) 5.00 (127.0) 0.75 (19.0) 8 ⁄ (16)


58

2 1⁄ 2 7.50 (190.5) 5.88 (149.4) 0.88 (22.4) 8 ⁄ (18)


34

3 8.25 (209.6) 6.62 (168.1) 0.88 (22.4) 8 ⁄ (18)


34

3 1⁄ 2 9.00 (228.6) 7.25 (184.2) 0.88 (22.4) 8 3⁄4 (18)

4 10.00 (254.0) 7.88 (200.2) 0.88 (22.4) 8 3⁄4 (18)

5 11.00 (279.4) 9.25 (235.0) 0.88 (22.4) 8 3⁄4 (18)

6 12.50 (317.5) 10.62 (269.7) 0.88 (22.4) 12 3⁄4 (18)

8 15.00 (381.0) 13.00 (330.2) 1.00 (25.4) 12 7⁄8 (22)

10 17.50 (444.5) 15.25 (387.4) 1.12 (28.4) 16 1 (24)


12 20.50 (520.7) 17.75 (450.9) 1.25 (31.7) 16 11⁄8 (24)

14 23.00 (584.2) 20.25 (514.4) 1.25 (31.7) 20 11⁄8 (24)


16 25.50 (647.7) 22.50 (571.5) 1.38 (35.1) 20 11⁄4 (30)
18 28.00 (711.2) 24.75 (628.7) 1.38 (35.1) 24 11⁄4 (30)
20 30.50 (774.7) 27.00 (685.8) 1.38 (35.1) 24 11⁄4 (30)
24 36.00 (914.4) 32.00 (812.8) 1.62 (41.1) 24 11⁄2 (36)
A
Dimensions conform to ANSI B16.5 for Class 300 steel flanges.

9. Workmanship, Finish, and Appearance


9.1 Flanges shall be free as commercially practical of
defects, including indentations, delaminations, bubbles,
pinholes, foreign inclusions, and resin-starved areas.

10. Test Methods


10.1 Conditioning—When conditioning is required, and in
all cases of disagreement, condition the test specimens at 73.4
6 3.6°F (23 6 2°C) and 50 6 10 % relative humidity for not
less than 40 h prior to test, in accordance with Procedure A of
Practice D618.
10.2 Test Conditions—The tests may be conducted at ambi-
ent temperature and humidity conditions. When controlled
environment testing is specified, tests shall be conducted in the
FIG. 1 Test Assembly Configuration
Standard Laboratory Atmosphere of 73.4 6 3.6°F (23 6 2°C)
and 50 6 10 % relative humidity. When elevated temperature
testing is specified, the tests shall be conducted at the design free-end closure except as herein noted. The pressure in the
operating temperature 65.4°F (3°C). specimen shall be increased until failure of the flange occurs.
Pressure testing in an atmospheric environment is permissible.
10.3 Dimensions and Tolerances—Flange dimensions shall Minimum failure time shall be 60 s; no restriction shall be
be measured with a micrometer of vernier calipers, or other placed on maximum time-to-failure. Leaking past the gasket
suitable measuring devices accurate to within 60.001 in. interface is permissible during this test. Bolt torque may be
(60.02 mm). Diameters shall be determined by averaging a increased as necessary during the test in order to minimize
minimum of four measurements, equally spaced circumferen- gasket leaking and to achieve the pressure necessary to cause
tially. flange failure. The assembly used for the test in 10.4 may be
10.4 Sealing—Flanged components in general arrangement used for this test. (Warning—Do not test with any pressurized
with Fig. 1 shall be bolted together using the gasket and bolt gas.)
torque recommended for standard field installation by the 10.6 Maximum Bolt Torque—Using the gasket and hardware
flange manufacturer. The assembly shall then be pressure recommended by the flange manufacturer, bolt the flange
tested and be required to hold the test pressure for a period of against a flat face steel flange. Tighten the nuts by hand until
168 hours without leakage. Retorque to the manufacturer’s they are snug. Prior to fit-up, the nuts, bolts, and washers
specified level after initial pressurization is permitted. should be well lubricated, using a nonfluid thread lubricant.
10.5 Short-Term Rupture Strength—Flanged components Establish uniform pressure over the flange face by tightening
shall be tested in accordance with Test Method D1599 with bolts in 5 lbf·ft (7 N·m) increments according to the sequence

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D4024 − 15
shown in Fig. 2. For flanges with more than 20 bolts, similar 11.1.2 Identification of the flange in accordance with the
alternating bolt tightening sequences shall be used. Increase the designation code in 4.2,
bolt torque uniformly until flange failure occurs or until all 11.1.3 Nominal flange size, and
bolts have been torqued to five times the level recommended 11.1.4 Manufacturer’s name (or trademark) and product
by the manufacturer for field installation practice to establish designation.
the bolt torque cell classification of the flange. Any sign of 11.2 All required markings shall be legible and so applied as
flange damage (crumbling, flaking, cracking, or other break- to remain legible under normal handling and installation
ing) shall constitute failure. practices.
NOTE 4—The torque limits determined by 10.6 apply only to flanges 12. Precision and Bias
bolted up against a flat sealing surface. Significantly lower bolt torque
value will normally be obtained when RTR flanges are bolted up against 12.1 No precision and bias statement can be made for this
raised-faced flanges. When RTR flanges must be used against raised steel test method, since controlled round robin test programs have
flange face, the RTR flange manufacturer should be contacted for his not been run.
torque and installation recommendations.
NOTE 5—The wide variation in raw materials and constructions allowed
11. Product Marking in this specification make round robin testing difficult to apply.

11.1 Each flange shall be marked with the following infor- 13. Keywords
mation: 13.1 centrifugally-cast; compression-molded; filament-
11.1.1 The designation “ASTM D4024” indicating compli- wound; furan; machine-made; phenolic; polyester; resin-
ance with this specification, transfer; vinyl ester

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D4024 − 15

FIG. 2 Bolt Torquing Sequence

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4024 - 12)
that may impact the use of this standard. (May 1, 2015)

(1) Corrected bolt tightening sequence on 8-bolt flange dia-


gram (Fig. 2).

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4068 − 17 An American National Standard

Standard Specification for


Chlorinated Polyethylene (CPE) Sheeting for Concealed
Water-Containment Membrane1
This standard is issued under the fixed designation D4068; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* of this standard to establish appropriate safety and health


1.1 This specification covers flexible chlorinated polyethyl- practices and determine the applicability of regulatory limita-
ene (CPE) sheeting which is used without mastic, bedding, or tions prior to use.
coating for construction of concealed water-containment mem- 2. Referenced Documents
branes in applications where there is potential for costly
2.1 ASTM Standards:2
secondary damage from leakage, and where very long-term
D412 Test Methods for Vulcanized Rubber and Thermoplas-
reliable performance is essential. Examples are fountains,
tic Elastomers—Tension
pools, planters, shower and safe pans, tile tubs, and similar
D543 Practices for Evaluating the Resistance of Plastics to
installations where the membrane is inaccessible once con-
Chemical Reagents
struction is complete. Included are requirements for
D618 Practice for Conditioning Plastics for Testing
composition, strength and toughness, test methods, workman-
D751 Test Methods for Coated Fabrics
ship criteria, and methods of marking.
D883 Terminology Relating to Plastics
1.2 Manufacturers have the option to use recycled materials D1004 Test Method for Tear Resistance (Graves Tear) of
in this product. Recycled materials must be in accordance with Plastic Film and Sheeting
the requirements in Section 4. D1203 Test Methods for Volatile Loss From Plastics Using
1.3 The test methods used to characterize the sheeting are Activated Carbon Methods
intended to ensure quality and performance and are not D1204 Test Method for Linear Dimensional Changes of
necessarily adequate for design purposes. Test methods have Nonrigid Thermoplastic Sheeting or Film at Elevated
been selected to be conducted primarily with liquids that Temperature
simulate the environments to which the membrane will be D1876 Test Method for Peel Resistance of Adhesives (T-
subjected during actual installation and use. Peel Test)
D2136 Test Method for Coated Fabrics—Low-Temperature
1.4 This specification does not cover water-containment Bend Test
membranes exposed in use to ultraviolet light or direct sun- D2240 Test Method for Rubber Property—Durometer Hard-
light. ness
1.5 The values stated in inch-pound units are to be regarded D4968 Practice for Annual Review of Test Methods and
as standard. The values given in parentheses are mathematical Specifications for Plastics
conversions to SI units that are provided for information only D5947 Test Methods for Physical Dimensions of Solid
and are not considered standard. Plastics Specimens
D6988 Guide for Determination of Thickness of Plastic Film
NOTE 1—There is no known ISO equivalent to this standard.
Test Specimens
1.6 The following safety hazards caveat pertains only to the D7209 Guide for Waste Reduction, Resource Recovery, and
test method portion, Section 14, of this specification: This Use of Recycled Polymeric Materials and Products (With-
standard does not purport to address all of the safety concerns, drawn 2015)3
if any, associated with its use. It is the responsibility of the user E96/E96M Test Methods for Water Vapor Transmission of
Materials

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.24 on Plastic Building contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Products. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved March 1, 2017. Published March 2017. Originally the ASTM website.
3
approved in 1981. Last previous edition approved in 2015 as D4068 – 15. DOI: The last approved version of this historical standard is referenced on
10.1520/D4068-17. www.astm.org.

*A Summary of Changes section appears at the end of this standard


Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D4068 − 17
2.2 ANSI Document: 5.1.2.1 A specimen composed of plied sheets is permitted if
Safety Code for Safety Glazing Materials for Glazing Motor it has been shown the results are equivalent to a solid
Vehicles Operating on Land Highways4 specimen.

3. Terminology NOTE 2—Plied specimens may not agree with those made on solid
specimens, as the surfaces of the plied specimens may not be in complete
3.1 Definitions: contact.
3.1.1 General—Definitions are in accordance with Termi- 5.1.3 The lateral dimensions of the specimen shall be
nology D883 unless otherwise indicated. sufficient to permit measurements at least 0.48 in. (12.0 mm)
3.1.2 The abbreviation for chlorinated polyethylene is CPE. from any edge.
3.2 Definitions of Terms Specific to This Standard: 5.1.3.1 Measurements are permitted at a lesser distance
3.2.1 homogeneous sheeting—sheeting that is of homoge- from an edge if identical results are obtained as 5.1.3.
neous composition throughout its thickness. (Note that it is not
of a sandwich construction with a continuous or semi- 6. Mechanical Properties
continuous layer of one or more materials of different compo- 6.1 The sheeting shall conform to the mechanical property
sition enclosed between two or more layers of CPE.) requirements in Table 1.
3.2.2 monolithic sheeting—sheeting manufactured as one
7. Performance Requirements
piece. (Note that it is not several thicknesses laminated
together, nor is it two or more widths lapped and joined with 7.1 The sheeting shall conform to the performance require-
heat or chemicals.) ments in Table 2.
3.2.3 water containment membrane—a nonporous mem- 8. Other Requirements
brane impervious to water and resistant to permeation by water
vapor to an extent that provides a high degree of certainty that 8.1 The sheeting shall be capable of being bonded to itself
secondary damage from leakage shall not occur. in a manner suitable for making seams and repairs in the field.
The manufacturer shall recommend or furnish methods,
4. Materials and Manufacture materials, or equipment necessary and suitable for this purpose.
4.1 The sheeting shall be made from a compound that 8.2 Bonds between sheets of material used in fabrication of
contains more than 50 % chlorinated polyethylene resin by a water-containment membrane shall conform to the require-
weight of total resin content, and the CPE resin shall: (a) ments in Table 3 and shall not reduce the overall resistance of
contain 38 to 46 % chlorine; (b) be made from a linear the membrane to permeation or leakage.
polyethylene having a density of not less than 0.95 g/cm2; (c)
be substantially amorphous, having a heat of fusion of less than 9. Dimensions and Permissible Variations
0.4 cal/g (1.7 kJ/kg), and (d) have a melt viscosity of 1700 6 9.1 The actual width and length of the sheeting shall be as
500 Pa·s when measured in a capillary rheometer at a melt agreed upon between the purchaser and the seller.
temperature of 190 6 2 °C, and a shear rate of 150 6 10 s−. 9.1.1 Sheeting width tolerance shall be +0.5, −0 in. (+12.7,
4.2 When recycled materials, as defined in Guide D7209, −0 mm).
are used in this product, the material must meet the require- 9.1.2 The length of the sheeting after unrolling and relaxing
ments in Sections 3, 4, 5, 6, 7, and 8. for 10 min at 73.4 6 3.6°F (23 6 2.0 °C) shall be no less than
that specified in the purchase order or contract.
4.3 The use of water-soluble compounding ingredients shall
be prohibited. 9.2 The sheeting shall be divided by grade based on
thickness, as follows:
4.4 The sheeting shall be homogeneous and monolithic. 9.2.1 Grade 1—40 mil (1.02 mm) shall be a minimum of
0.040 in. (1.02 mm) in thickness.
5. Physical Requirements
5.1 The sheeting shall have an average Shore-A hardness of
84 6 6 points when ten specimens taken equidistantly across TABLE 1 Mechanical Properties
the width of the sheet are tested in accordance with Test Specification
Property Unit
Method D2240, using a Type A durometer and reading durom- Grade 1 Grade 2
eter hardness after 5 s of presser foot contact with the
Thickness in. (mm) 0.040 (1.02), 0.030 (0.0765),
specimen. min min
5.1.1 The thickness of the test specimens shall be 0.24 in. Tensile strength psi (MPa) 1200 (8.28), 800 (5.5), min
(6.0 mm) minimum unless it is known that results equivalent to min
Tensile stress at psi (MPa) 400 (2.76), 300 (2.07),
the 0.24 in. (6.0 mm) values are obtained with a thinner 100 % elongation min min
specimen. (modulus) 1200 (8.28), 1200 (8.28),
5.1.2 The test specimen shall be of solid construction max max

Elongation, at break % 350, min 300, min


Tear resistance lbf/in. (kN/m) 175 (30.6), min 120 (20.9), min
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., of width
4th Floor, New York, NY 10036, http://www.ansi.org.

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D4068 − 17
TABLE 2 Performance Requirements tests in this specification. In no case shall a sample be less than
Specification 16 ft2 (1.49 m2), nor shall either width or length be less than 3
Property Unit
Grade 1 Grade 2 ft (0.91 m).
11.1.4 Sample using a statistically acceptable procedure.
Volatile Loss at 158°F (70°C): 11.1.5 From this population, select samples randomly to
Weight change percent loss ±1.5, max ±1.5, max
Microorganism Resistance: provide specimens for each test.
Weight change percent ±5, max ±5, max
Chemical Resistance:
11.2 Sampling for In-Plant Quality Control Evaluation:
Sodium Hydroxide: 11.2.1 Samples for quality control evaluation shall be a
Weight change percent ±5, max ±5, max minimum of 25 ft2 (2.5 m2), and completely span the width of
Soapy Water, 1 % solution:
Weight change percent ±3, max ±3, max
the finished sheet.
Distilled Water: 11.2.2 Select randomly one or more samples from each
Weight change percent ±2, max ±2, max 10 000 ft2 (1 000 m2) for the quality assurance tests specified
in Section 18 and Table 4.
TABLE 3 Bonded Seam Requirements 12. Number of Tests and Retests
Specification 12.1 One set of test units is sufficient to determine confor-
Property Unit
Grade 1 Grade 2 mance. The average result of all samples tested shall conform
to the requirements of this specification.
Bonded seam shear percent of tensile 75, min 75, min
strength 12.2 Retesting to determine conformance shall be required
Bonded seam peel lbf/in. (kN/m) of 10 (2.75) min 6 (1.65) min
strength (T-peel) seam width
after any significant change in compound or method of
manufacture.
12.2.1 Significant changes in compound include addition,
elimination, or substitution of any ingredient, changes in ratios
between ingredients, change in type or grade of CPE resin,
9.2.2 Grade 2—30 mil (0.765 mm) shall be a minimum of change in supplier or manufacturer, or both, of CPE resin, and
0.030 in. (0.765 mm) in thickness. change in manufacturer or supplier, or both, of CPE compound
or sheet.
10. Workmanship, Finish, and Appearance 12.2.2 Changes in compound that are not significant include
substitution of one material for another (except CPE resin)
10.1 The sheeting shall be free of pin holes, particles of where the two are essentially identical and changes in material
foreign matter, undispersed raw materials, or other manufac- which do not remain a part of the sheet after manufacture.
turing defects that might affect serviceability.
NOTE 3—Material substitutions include changes in supplier, grade or
10.2 The sheeting shall be free of blisters, craters, pimples, type.
pits, crazing, and thin spots. Sheet edges shall be straight,
12.2.3 Significant changes in manufacture include blending
parallel, and free of trim material.
process (dry blend, wet blend, Banbury mix, or separate
10.3 Printing and markings on the sheet shall be legible and compounding line) or method of fabricating sheet (calender,
not easily removed from the sheet during normal handling, extrusion, or casting).
transportation, and installation. 12.2.4 Changes in manufacture that are not significant
10.4 The sheeting shall be colored as agreed upon between include changes in brands of processing equipment, age of
the purchaser and the seller. equipment, location of manufacture, personnel, take-off equip-
ment and processes, packaging, and ambient or atmospheric
11. Sampling conditions.
11.1 Sampling for Evaluating Conformance to Physical, 12.3 Retesting to determine conformance shall occur at least
Mechanical, and Performance Requirements: every five years whether or not significant changes have
11.1.1 One roll, or other equivalent packaged unit, with a occurred.
minimum continuous sheet of 100 ft2 (9.3 m2) shall be suffi- NOTE 4—This requirement is included to monitor cumulative effects of
cient for completing all tests and evaluations in this specifica- relatively insignificant changes in compound or manufacture over time.
tion.
11.1.2 Select randomly each roll or unit submitted for TABLE 4 Quality Assurance Requirements
evaluation from an inventory of regular production stock not
Specification
older than one year. Selecting more than one roll or unit or Property Unit
Grade 1 Grade 2
selecting from multiple inventory stocks or locations will
increase the likelihood of obtaining a representative sample of Thickness in. (mm) 0.040 (1.02) 0.030 (0.765)
contemporary production. The age of stocks from which Pinholes ... none none
selections are made is required to be documented. Shrinkage percent 5, max 5, max
Width tolerance in. (mm) +0.5 (−0.0) +0.5 (−0.0)
11.1.3 Divide all submitted sheet into smaller samples of Length tolerance in. (mm) −0.0 −0.0
sufficient size to provide a set of specimens for any one of the

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D4068 − 17
12.4 If the results of any test do not conform to the material passed or failed at that temperature. Failure of one
requirements of this specification, retesting to determine con- specimen (as defined in Method D2136) constitutes rejection of
formity is performed only after the purchaser and supplier the sample.
agree to the retesting. However, this provision shall not be used
NOTE 5—This test procedure may require testing an additional set of
to lower a minimum requirement, omit, substitute, or modify a three specimens. For greater efficiency, six specimens may be prepared,
test or requirement, or alter specification limits. conditioned, cooled, and tested at one time. If done in this manner the
three specimens comprising each testing group must be identified prior to
13. Specimen Preparation the start of the test.
13.1 Conditioning: NOTE 6—Requirement for Water-Vapor Transmission of Materials in
Sheet Form (Procedure E of Test Methods E96/E96M has been deleted
13.1.1 Condition all physical, mechanical, and performance until the test method is improved to the extent that it can be reproducibly
test specimens at 73.4 6 3.6°F (23.0 6 2.0 °C) and 50 6 10 % run by commercial laboratories).
relative humidity for not less than 40 h in accordance with
14.6 Chemical Resistance—Determine weight changes in
Procedure A of Methods D618 prior to testing or starting
accordance with Procedures I and II of Test Method D543.
environmental and chemical exposures.
14.6.1 Reagents:
13.1.2 Recondition all environmental and chemical expo-
sure samples at 73.4 6 3.6°F (23.0 6 2.0 °C) and 50 6 10 % 14.6.1.1 Sodium Hydroxide (10 % solution)—Immerse
relative humidity for not less than 40 h in accordance with specimens for 72 h at 120°F (49 °C).
Procedure A of Methods D618 following removal from expo- 14.6.1.2 Soap Solution (1 %)—Immerse specimens for 24 h
sure and prior to physical or mechanical property testing. at 120°F (49 °C). Rinse specimens in clean water after removal
13.1.3 Condition in-plant quality assurance specimens at and dry in forced-air oven at 125°F (52 °C) for 24 h prior to
73.4 6 3.6°F (23.0 6 2.0 °C) for 2 h in air prior to testing. weight measurement and testing.
14.6.1.3 Distilled Water—Immerse specimens for 24 h at
13.2 Bonded Seam Samples:
120°F (49 °C). Dry specimens in forced-air oven at 125°F
13.2.1 Bonded seam samples from which specimens are to
(52 °C) for 24 h prior to weight measurement and testing.
be taken for testing shall be prepared using sheet samples
14.6.2 Testing—Immerse adequate specimens in each re-
supplied by the manufacturer. The manufacturer shall include
agent to test for all properties specified.
detailed instructions as well as recommend or supply all
materials needed to fabricate the bonded seam samples. The 14.6.3 Weight Change—For each reagent, test a minimum of
manufacturer has the option to entirely prepare the bonded three weight-change specimens. Weigh each specimen after
seam samples used for the test specimens. conditioning prior to immersion and record the average weight
13.2.2 Finished bonded seam samples from which test (W1). Weigh each specimen again after conditioning following
specimens are to be cut shall be conditioned at 73.4 6 3.6°F immersion, recording the average weight (W2). Calculate
(23.0 6 2.0 °C) and 50 6 10 % relative humidity for no less weight change as:
than 40 h after being made and prior to cutting test specimens. Weight Change, % 5 ~ W2 2 W1 ! /W1 3 100 %.
13.2.3 After cutting, prepared specimens shall be condi-
Report this value as the average weight change.
tioned at 73.4 6 3.6°F (23.0 6 2.0 °C) and 50 6 10 % relative
humidity for not less than 168 h, in accordance with Procedure 14.7 Hydrostatic Pressure Resistance—Test three speci-
A of Methods D618 prior to testing or starting environmental mens in accordance with Annex A2. Rejection (failure) of one
exposures. specimen shall constitute failure of the entire sample. Report
results as pass or fail.
14. Test Methods
14.8 Puncture Resistance—Test six specimens in accor-
14.1 Stress-Strain Properties—Tensile strength, tensile dance with Annex A3. Report results as pass or fail.
stress at 100 % elongation (modulus), and ultimate elongation
shall be determined in accordance with Method A of Test 14.9 Bonded Seam Strength—Sufficient samples for speci-
Methods D412 using dumbbell cut specimens (Die C). Report men selection shall be prepared or provided as directed in 13.2
the average of six specimens. for each seaming method as specified by the manufacturer.
Possible seaming methods include solvent bonding, bodied
14.2 Tear Resistance—Determine average value from ten
cements, adhesives, and thermal, dielectric, or RF welding
acceptable specimens tested in accordance with Test Methods
techniques. Other methods or techniques are also acceptable.
D1004.
NOTE 7—There is no requirement as to which type of seaming must be
14.3 Volatile Loss—Determine volatile loss in accordance
tested, or that more than one type needs evaluation. It is only required that
with Test Methods D1203, Method A, at 158°F (70 °C) with at least one type be available and tested.
Grade AC (6⁄14 mesh) activated carbon. Test specimens shall be
nominal thickness sheeting. 14.9.1 Shear Bond:
14.9.1.1 Sample pieces shall be made from minimum 8- in.
14.4 Microorganism Resistance—Test in accordance with (203-mm) square pieces of sheet, with a seam overlap of 1 6
the method described in Annex A1. 1⁄8 in. (25.4 6 3.2 mm). When making the seam, align sheets

14.5 Low-Temperature Flexibility—Test three specimens in so that orientation is transverse. After conditioning (see 13.2),
accordance with Test Method D2136 at a temperature of −22°F cut the sample into 1-in. (25-mm) strips and discard the two
(−30 °C) or less. Report temperature used in test and whether outside edge pieces. Cut one specimen from each strip using

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D4068 − 17
the dumbbell-shaped Die C for Test Methods D412, taking care 14.12 Shrinkage—Test one specimen for 1 h at 158°F
to place the bonded seam portion in the center of the specimen. (70 °C) in accordance with Test Method D1204. Percent
14.9.1.2 Test a minimum of six specimens in accordance shrinkage is the average change in both lineal dimensions.
with Method A of Test Methods D412, measuring tensile
strength as shear bond. Report the average of the shear values 15. Certification
as a percentage of the average tensile strength.
15.1 When specified in the purchase order or contract, the
14.9.2 Peel Test (T-Peel):
manufacturer’s or supplier’s certification shall be furnished to
14.9.2.1 For each sample piece, cut two 8 by 12-in. (203 by
the purchaser that states that samples representing each lot
305-mm) pieces of sheeting, and bond these two pieces
have been manufactured, tested, and inspected in accordance
completely together except for 3 in. (76 mm) of the 8-in.
with this specification, and that the requirements have been
(203-mm) dimension (see Fig. 1). After allowing the sample to
met. When specified in the purchase order or contract, a test
cure, cut the sample into 2 by 8-in. (50 by 203-mm) strips.
report shall be furnished.
Discard the outside strips.
14.9.2.2 Test a minimum of six specimens in accordance
16. Product Marking
with Method E of Test Method D1876. Peel strength is the
average load per unit width of bond line required to produce 16.1 Material complying with this specification shall be
progressive separation of the samples when pulled apart at a continuously marked and shall include the following, spaced
rate of 10 in./min (254 mm/min). Report the average peel out at intervals of not more than 2 ft (0.61 m):
strength of all samples tested. 16.1.1 Manufacturer’s name (or brand name or trademark),
14.10 Thickness—Measure a minimum of five specimens 16.1.2 Material designation CPE,
obtained from locations equidistant across the width of the 16.1.3 Sheeting thickness,
sheet in accordance with Test Methods D5947 or Guide D6988. 16.1.4 Designation “ASTM D4068” with which the sheet
Report thickness as an average of all specimens measured. complies, and
14.11 Pinholes—The test specimen shall be a section of 16.1.5 A production code.
sheeting 16 in. (406 mm) or more in length by the full sheeting
width. Examine 12 in. (304 mm) of this specimen across the 17. Packaging and Package Marking
width by viewing the surface of the sheeting while held under
17.1 The sheeting shall be rolled on a substantial core and
slight hand tension. Position a bright light source behind the
packaged in standard commercial containers, so constructed as
sheet so as to clearly illuminate the surface without producing
to ensure acceptance by common or other carriers for safe
glare. A pinhole is defined as any opening observed under the
transportation at the lowest applicable rate to the point of
conditions specified. One or more pinholes will be considered
delivery, unless otherwise specified in the contract or order.
as failure of the sheeting. Report the number and locations of
Use containers and pallets designed for forklift truck handling.
any pinholes, and any other observed deformations of the
sheet. Separately report any other observed deformations of the 17.2 Shipping containers shall be marked as agreed upon
sheet. between the purchaser and the seller.

FIG. 1 Bonded-Seam T-Peel Sample After Bonding and Prior to Specimen Cutting and Selection

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D4068 − 17
18. Quality Assurance 18.3 The manufacturer shall maintain quality control
18.1 The sheeting shall conform to the quality assurance records, including production codes so that defects discovered
requirements in Table 4. later may be checked against quality control inspections and
18.1.1 The sheeting shall be regularly monitored by the traced to a specific production lot.
manufacturer for compliance to these requirements at intervals
that best ensure that all materials shipped are in compliance. 19. Keywords
18.2 The sheeting shall be continuously monitored at manu- 19.1 chlorinated polyethylene; plastic sheeting; recycle us-
facture for appearance, pinholes, voids, undispersed materials, age water-containment membrane
surface blemishes, and other defects which may impair ser-
viceability.

ANNEXES

(Mandatory Information)

A1. MICROORGANISM RESISTANCE (SOIL BURIAL) TEST

A1.1 Materials A1.3.3 Post-condition specimens removed from soil burial


A1.1.1 Prepare a compost soil for specimen burial accord- prior to physical properties testing as follows:
ing to usual greenhouse practice and having a pH of 6.5 to 7.5. A1.3.3.1 Wash specimens under fresh, clean, warm water to
Further enrich the soil with a cow manure slurry. remove soil and foreign materials from specimens. Take
A1.1.2 Maintain the moisture content of the soil between 30 particular care to remove materials from the inside of the
and 50 % throughout the duration of the test. T-peel specimens without starting peel action. Pat dry with soft
A1.1.3 Maintain the temperature of the soil between 15 and absorbent cloth.
30°C. A1.3.3.2 Desiccate specimens for one week or until speci-
A1.1.4 Microbiological Activity: men weights stabilize.
A1.1.4.1 Cut and condition 18 to 24 ten-ounce (540 to A1.3.3.3 Condition specimens at 73.4 6 3.6°F (23.0 6
720-mL) cotton duck tensile specimens in accordance with 2.0 °C) and 50 6 10 % relative humidity for at least 24 h
13.1.1. Test a minimum of three specimens in accordance with following desiccation and prior to testing.
Test Method A of Test Methods D412 to obtain an average
benchmark tensile strength value for the cotton duck. A1.4 Procedure
A1.1.4.2 Bury twelve cotton duck specimens in the enriched A1.4.1 Weigh all weight-change specimens and record the
soil with the test specimens. Remove three cotton duck average weight. Bury two sets of specimens vertically and
specimens after one, two, three, and four weeks and test for separately in the enriched soil for 30 days with a minimum of
tensile strength. 1 in. (25.4 mm) between each specimen.
A1.1.4.3 Adequate microbiological activity is assumed if
the cotton duck loses at least 70 % of its initial tensile strength A1.4.2 Weigh all weight-change specimens following post
in one week and at least 90 % in two weeks. A loss of 90 % or conditioning and compare average with pre-burial average
more for three- and four-week specimens is recommended. weight.
A1.1.4.4 After four weeks, test the three remaining unbur-
ied cotton duck specimens. A1.5 Calculation and Interpretation

A1.2 Specimen Preparation A1.5.1 For each set of samples calculate average weight
change.
A1.2.1 Prepare four sets of six 2-in. (50.8-mm) diameter
weight-change disk specimens. A1.5.2 Determine average change from original average
values for weight change using the formula:
A1.3 Conditioning
Change, % 5 @ ~ X2 2 X1 ! / X 1 # 3 100 %
A1.3.1 Precondition bonded seam samples at least 168 h at
73.4 6 3.6°F (23.0 6 2.0 °C) and 50 6 10 % relative humidity where:
after cutting and selecting bond seam test specimens. X1 = original average property value, and
A1.3.2 Condition all specimens at 73.4 6 3.6°F (23.0 6 X2 = average property value after test exposure.
2.0 °C) and 50 6 10 % relative humidity for not less than 40 h A1.6 Report
in accordance with Procedure A of Test Methods D618 prior to
burial. A1.6.1 Report the percent change in weight.

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D4068 − 17

A2. HYDROSTATIC PRESSURE TEST

A2.1 Materials A2.3 Procedure


A2.1.1 The apparatus for the hydrostatic pressure test, a A2.3.1 Clamp the test specimen in the holder that has been
puncture resistance apparatus, is essentially a pressure tube previously filled with water.
connected to a specimen holder. The inner diameter of the A2.3.1.1 Take care to avoid trapped air between the speci-
pressure tube shall be 2 in. (51 mm) and the outer diameter men and the water. This is done by filling the holder with water
shall be 3 in. (76 mm) with a means for introducing water from and sliding the specimen onto the holder in direct contact with
below the specimen. the water after having used a piece of transparent material for
practice and for becoming familiar with the technique.
NOTE A2.1—A drawing of such an apparatus is published in Test A2.3.2 Fill the tube to achieve a 2-ft (0.61-m) hydrostatic
Methods D751 as Fig. 3: Machine for Measuring Hydrostatic Resistance
of a Coated Fabric by Using the Pressure of a Rising Column of Water. head.
A2.3.3 Observe the specimen at 10-min intervals for the
A2.1.1.1 Connect an extension tube to permit a water head
first hour, and at hourly intervals for the succeeding 7 h, after
of 2 ft (0.61 m) with a cutoff valve or other suitable device at
which the specimen shall be left under hydrostatic pressure for
the water inlet to the pressure tube for isolating the specimen
40 h and again examined.
until the desired head is reached.
A2.4 Interpretation and Report
A2.2 Specimens
A2.4.1 Any evidence of wetness on top of the specimen or
A2.2.1 Each test unit shall consist of three specimens of the formation of a droplet shall cause the sheeting sample to be
sheeting 3 by 3 in. (76 by 76 mm). rejected.
A2.2.2 Condition all specimens in accordance with 13.1.1. A2.4.2 Report results as pass or fail.

A3. PUNCTURE RESISTANCE TEST

A3.1 Apparatus A3.3.2 Place a single specimen between the holding frame
A3.1.1 The specimen holder (Fig. A3.1) shall consist of two halves and clamp securely by tightening the thumb screws.
10 by 10-in. (254 by 254-mm) pieces of 3⁄4-in. (19-mm) Suspend the impact dart vertically above the center of the
smooth-surface hardwood. One of these pieces shall contain a specimen with a vertical distance of 3 ft (0.91 m) between the
symmetrically located 6 by 6-in. (152 by 152-mm) opening in nose of the dart and the surface of the specimen.
the center.
A3.3.3 Release the dart for one free fall on each specimen.
A3.1.1.1 Sandwich the specimen between these two speci-
men holders placing the holder with the opening on top. Use A3.3.4 All specimens completing this test without visible
the three thumb screws or bolts located in the center of each rupture shall be further hydrostatically tested in accordance
side to securely clamp the specimen within the holder. with 14.8, completely following all procedures in Annex A2.
A3.1.2 Impact Dart, a 7.0 6 0.1-oz (198.45 6 2.835-g) steel A3.3.4.1 Place the point of dart impact in the center of the
dart as shown in Fig. A3.2. This drawing is published in the hydrostatic testing apparatus.
American National Standard Safety Code for Safety Glazing
Materials for Glazing Motor Vehicles Operating on Land A3.4 Interpretation and Report
Highways. A3.4.1 Visible rupture of any specimen shall constitute
A3.2 Specimens failure of the sheeting sample to meet this test.
A3.2.1 Each test unit shall consist of six specimens of 10 by A3.4.2 Any wetness or leakage from any specimen during
10-in. (254 by 254-mm) sheeting. hydrostatic testing shall constitute failure of the sheeting
A3.2.2 Condition all specimens in accordance with 13.1.1. sample to pass this test.

A3.3 Procedure A3.4.3 Report results as pass or fail.


A3.3.1 Test three specimens with one side up and three with
the opposite side up.

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D4068 − 17

FIG. A3.1 Wood Holding Fixture for Drop Test

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D4068 − 17

FIG. A3.2 Dart for Safety Glass Tests

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D4068 − 17
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4068–15)
that may impact the use of this standard. (March 1, 2017)

(1) Changed average Shore-A hardness from 76 6 6 to 84 6 6 (4) Removed “in transverse direction” from 14.1, 14.2, and
in 5.1. 14.9.1.2.
(2) Removed “transverse direction” from Table 1. (5) Reworded 16.1.5.
(3) Removed “transverse direction” from Table 3.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4097 − 19

Standard Specification for


Contact-Molded Glass-Fiber-Reinforced Thermoset Resin
Corrosion-Resistant Tanks1
This standard is issued under the fixed designation D4097; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope mendations issued by the World Trade Organization Technical


1.1 This specification covers cylindrical tanks fabricated by Barriers to Trade (TBT) Committee.
contact molding for above-ground vertical installation, to
contain aggressive chemicals at atmospheric pressure, and 2. Referenced Documents
made of a commercial-grade polyester or vinyl ester, resin. 2.1 ASTM Standards:2
Included are requirements for materials, properties, design, C581 Practice for Determining Chemical Resistance of
construction, dimensions, tolerances, workmanship, and ap- Thermosetting Resins Used in Glass-Fiber-Reinforced
pearance. Structures Intended for Liquid Service
1.2 This specification does not cover the design of vessels C582 Specification for Contact-Molded Reinforced Thermo-
intended for pressure above atmospheric or under vacuum setting Plastic (RTP) Laminates for Corrosion-Resistant
conditions, except as classified herein, or vessels intended for Equipment
use with liquids heated above their flash points. D618 Practice for Conditioning Plastics for Testing
1.3 The values stated in inch-pound units are to be regarded D638 Test Method for Tensile Properties of Plastics
as standard. The values given in parentheses are provided for D790 Test Methods for Flexural Properties of Unreinforced
information purposes only. and Reinforced Plastics and Electrical Insulating Materi-
als
1.4 Special design consideration shall be given to tanks
D883 Terminology Relating to Plastics
subject to environmental and/or mechanical forces such
D2150 Specification for Woven Roving Glass Fabric for
seismic, wind, ice, agitation, or fluid dynamic forces, to
operational service temperatures greater than 180°F (82°C) and Polyester-Glass Laminates (Withdrawn 1987)3
to tanks with unsupported bottoms. D2583 Test Method for Indentation Hardness of Rigid Plas-
tics by Means of a Barcol Impressor
1.5 The following safety hazards caveat pertains only to the D2584 Test Method for Ignition Loss of Cured Reinforced
test method portion, Section 11, of this specification: This Resins
standard does not purport to address all of the safety concerns,
D2996 Specification for Filament-Wound “Fiberglass”
if any, associated with its use. It is the responsibility of the user
(Glass-Fiber-Reinforced Thermosetting-Resin) Pipe
of this standard to establish appropriate safety, health, and
D2997 Specification for Centrifugally Cast “Fiberglass”
environmental practices and determine the applicability of
(Glass-Fiber-Reinforced Thermosetting-Resin) Pipe
regulatory limitations prior to use.
D3892 Practice for Packaging/Packing of Plastics
NOTE 1—There is no known ISO equivalent to this standard. D4024 Specification for Machine Made “Fiberglass” (Glass-
1.6 This international standard was developed in accor- Fiber-Reinforced Thermosetting Resin) Flanges
dance with internationally recognized principles on standard- D5421 Specification for Contact Molded “Fiberglass”
ization established in the Decision on Principles for the (Glass-Fiber-Reinforced Thermosetting Resin) Flanges
Development of International Standards, Guides and Recom- F412 Terminology Relating to Plastic Piping Systems

1 2
This specification is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Plastic Piping Systems and Chemical Equipment. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Aug. 1, 2019. Published August 2019. Originally the ASTM website.
3
approved in 1982. Last previous edition approved in 2018 as D4097 - 18. DOI: The last approved version of this historical standard is referenced on
10.1520/D4097-19. www.astm.org.

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2.2 ANSI Standards: NOTE 3—The addition of a thixotropic agent may reduce the resistance
B 16.1 Cast Iron Pipe Flanges and Flanged Fittings, Class of many resin systems to certain corrosive chemical environments. It is the
responsibility of the fabricator, using a thixotropic agent in the resin
25, 125, 250, and 8004 required for 7.1.1 and 7.1.2, to ascertain its compatibility with the
B 16.5 Steel Pipe Flanges, Flanged Valves and Fittings4 corrosive environment when this has been reported by the purchaser.

3. Terminology 5.1.1.2 Resin pastes used to fill crevices before overlay shall
not be subject to the limitation of 5.1.1.
3.1 Definitions—Definitions are in accordance with Termi- 5.1.1.3 Resin may contain pigment, dyes, or colorants when
nologies D883 and F412, unless otherwise indicated. agreed upon between fabricator and purchaser.
3.2 Definitions of Terms Specific to This Standard: NOTE 4—The addition of pigment, dyes, or colorants may interfere with
3.2.1 contact molding—includes the “hand lay-up” or a visual inspection of laminate quality.
combination of the “hand lay-up” and the “spray-up” manu-
5.1.1.4 Ultraviolet absorbers may be added for improved
facturing processes.
weather resistance if agreed upon between the fabricator and
4. Classification the purchaser.
5.1.1.5 Antimony compounds or other fire-retardant agents
4.1 Tanks meeting this specification are classified according may be added to halogenated resins for improved fire
to type. It is the responsibility of the purchaser to specify the resistance, if agreed upon between the fabricator and the
requirement for Type II tanks, the operating pressure or purchaser.
vacuum levels, and the safety factor required for external
pressure. Absence of a designation of type required shall imply NOTE 5—Because the addition of fire-retardant agents may interfere
with visual inspection of laminate quality, they should not be used in the
that Type I is adequate. inner surface (7.1.1) or interior layer (7.1.2), unless their functional
4.1.1 Type I—Atmospheric pressure tanks vented directly to advantages would outweigh the loss of visual inspection.
the atmosphere, designed for pressure no greater or lower than
5.2 Reinforcement:
atmospheric.
5.2.1 Chopped-Strand Mat—Chopped-strand mat shall be
4.1.2 Type II—Atmospheric pressure tanks vented directly
constructed from chopped commercial-grade E-type glass
into a fume conservation system, and designed to withstand,
strands bonded together using a binder. The strands should be
the specified positive and negative pressure not to exceed 14 in.
treated with a sizing that is chemically compatible with the
of water (355.6 mm) when all tie-down lugs are properly
resin system used.
secured, in accordance with the fabricator’s recommendations
for flat-bottom tanks. NOTE 6—The selection of the particular chopped-strand mat is depen-
dent upon the performance characteristics required of the finished product
4.2 Tanks meeting this specification are classified according and upon the processing techniques to be used.
to type as follows:
5.2.2 Nonwoven Biaxial or Unidirectal Fabric—These
4.2.1 Grade 1—Tanks manufactured with a single generic
products shall be a commercial grade of E-type glass fiber with
type of thermoset resin throughout.
a sizing that is chemically compatible with the resin system
4.2.2 Grade 2—Tanks manufactured with different generic
used.
types of thermoset resin in the barrier and the structural
5.2.3 Woven Roving—Woven roving shall be in accordance
portion.
with Specification D2150.
NOTE 2—The external corrosive environment due to spillage or 5.2.4 Surface Mat—The reinforcement used for the inner
corrosive vapors should be considered when specifying Grade 2 tanks (see surface (7.1.1) shall be either a commercial-grade chemical
7.1.3.3). resistant glass surface mat or an organic-fiber surface mat. In
5. Materials and Manufacture environments that attack glass, the use of an organic-fiber
surface mat is required.
5.1 Resin—The resin used shall be a commercial grade,
corrosion-resistant thermoset that has either been evaluated in 6. Design Requirements
a laminate by test in accordance with 11.3, or that has been 6.1 Straight Shell—The minimum required wall thickness of
determined by previous documented service to be acceptable the cylindrical straight shell at any fluid level shall be deter-
for the service conditions. Where service conditions have not mined by the following equation, but shall not be less than 3⁄16
been evaluated, a suitable resin may also be selected by in.:
agreement between fabricator and purchaser.
5.1.1 The resin shall contain no pigment, dyes, colorants, or t 5 PD/2S H 5 0.036 γ HD/2S H or ~ 0.2489 γ HD/2S H !
filler, except as follows: where:
5.1.1.1 A thixotropic agent that does not interfere with
t = wall thickness, in. (mm),
visual inspection of laminate quality, or with the required SH = allowable hoop tensile stress (not to exceed 1⁄10 of the
corrosion resistance of the laminate, may be added for viscos- ultimate hoop strength), psi (kPa) (see 11.8),
ity control. P = pressure, psi (kPa),
H = fluid head, in. (mm),
4
γ = specific gravity of fluid, and
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
D = inside diameter of tank, in. (mm).
4th Floor, New York, NY 10036, http://www.ansi.org.

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NOTE 7—The use of an accepted analytical technique, such as laminated
plate theory (LPT), for design and analysis of composite vessels may
predict stresses, strains, and strength on a ply-by-ply basis, given some
basic lamina properties.
NOTE 8—The calculation is suitable for the shell design of elevated
dished-bottom tanks that are mounted or supported below the tangent of
the dished-bottom head. Special consideration must be given to the
loading on the straight shell at the support when tank has mounting
supports located above the tangent line.
NOTE 9—Table X2.1, Appendix X2, illustrates minimum straight-shell
wall thicknesses.
6.2 Design for External Pressure:
6.2.1 Cylindrical Shells—For cylindrical shells, compute
the value 1.73 (Do/t)0.5. If the result is less than L/Do of the
cylinder, compute Pa as follows:
P a 5 2.6~ E/F ! ~ D o /L ! ~ t/D o ! 2.5

If the result is greater than L/Do of the cylinder, compute Pa


as follows:
FIG. 1 Jointed Head Detail
2.6~ E/F !~ D o /L !~ t/D o ! 2.5 (Sketch A)
Pa 5
~ L/D o ! 2 0.45~ t/D o ! 0.5
where:
Do = outside diameter, in., I s 5 PLs D 3 F/24E h
Et = hoop tensile modulus of the filament wound structural
laminate, psi (kPa), where:
F = design factor = 5, Do = shell outside diameter, in. (mm),
L = design length, in. (mm), of a vessel section, taken as Eh = hoop tensile modulus, psi (kPa),
the largest of the following: (a) the distance between F = design factor = 5,
head tangent lines plus one-third the depth of each Is = moment of inertia, in.4(mm4), of stiffener for the
formed head, if there are no stiffening rings (excluding effective length of shell, Ls,
conical heads and sections); (b) the distance between Ls = one-half of the distance from the centerline of the
cone-to-cylinder junctions for vessels with a cone or stiffening ring to the next line of support on one side,
conical heads if there are no stiffening rings; (c) the plus one-half of the centerline distance to the next line
greatest center-to-center distance between any two of support on the other side of the stiffening ring, both
adjacent stiffening rings; (d) the distance from the measured parallel to the axis of the cylinder, in. A line
center of the first stiffening ring to the formed head of support is the following: (a) a stiffening ring that
tangent line plus one-third the depth of the formed head meets the requirements of this paragraph; (b) a circum-
(excluding conical heads and sections), all measured ferential line on a head at one-third the depth of the
parallel to the axis of the vessel; (e) the distance from head from the head tangent line; (c) a cone-to-cylinder
the first stiffening ring in the cylinder to the cone-to- junction,
cylinder junction, P = actual external pressure, psi (kPa).
Pa = allowable external pressure, psi (kPa), and Typical half-round stiffener sizes and dimensions for differ-
t = wall thickness, in. (mm) (nominal). ent values of Is are shown in Fig. 4. Other stiffener profiles
6.2.2 Torispherical Heads—For torispherical heads, com- meeting the required moment of inertia may be used.
pute the allowable external pressure, Pa, as follows: 6.3 Top Head—The top head, regardless of shape, shall be
P a 5 0.36~ E/F ! ~ t/R ! 2 able to support a 250-lb (113.4 kg) load on a 4 by 4-in. (100 by
o
100 mm) area without damage and with a maximum deflection
where: of 1⁄2 % of the tank diameter.
Ro = outside crown radius of head, in. (mm). 6.3.1 The minimum thickness of the top head shall be 3⁄16 in.
For toruspherical heads subject to internal loading, the (4.8 mm).
knuckle radius shall be externally reinforced in accordance NOTE 10—Support of auxiliary equipment, snow load, or operating
with Fig. 1. The reinforcement thickness shall be equal to the personnel, may require additional reinforcement or the use of stiffening
thickness of the head as calculated above. The thickness of a ribs, or both, sandwich construction, or other stiffening systems.
joint overlay near the knuckle radius tangent line of dished 6.4 Bottom Head:
head contributes to the knuckle reinforcement. 6.4.1 The minimum thickness for a fully supported flat-
6.2.3 Stiffening Rings—The required moment of inertia, Is, bottom head shall be as follows:
of a circumferential stiffening ring for cylindrical shells under 3⁄16 in. (4.8 mm) for 2 to 6-ft (0.6 to 1.8-m) diameter,

external pressure or internal vacuum shall not be less than that 1⁄4 in. (6.4 mm) for over 6 to 12-ft (1.8 to 3.7-m) diameter, and

determined by the following: 3⁄8 in. (9.5 mm) for over 12-ft (3.7-m) diameter.

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D4097 − 19
6.4.2 Bottom heads may be molded integrally with the laminate projections that would prevent uniform contact with a
straight-shell, or may be molded separately with a straight properly prepared flat support surface when the tank is filled
flange length for subsequent joining to shell. with liquid.
6.4.3 The radius of the bottom knuckle of a flat-bottom tank
shall be not less than 1 in. (25 mm) on tanks 4 ft or smaller in NOTE 11—This requirement is not intended to exclude the use of drain
nozzles, which are commonly used at the bottom of the side shell.
diameter and 1.5 in. (38 mm) on tanks larger than 4 ft in However, foundation cut-outs are required of the appropriate dimensions
diameter. The minimum thickness of the radiused section shall for nozzle type and size.
be equal to the combined thickness of the shell wall and the
bottom. The reinforcement of the knuckle-radius area shall 6.4.5 The thickness of an elevated torispherical dished
taper so that it is tangent to the flat bottom, and shall not extend bottom, suitable for supporting the weight of the fluid head,
beyond the tangent line onto the tank bottom, unless methods shall be determined by the following equation, but shall not be
of manufacture are used that maintain flat-bottom less than 3⁄16 in. (4.8 mm):
configuration, and shall extend up the vertical tank wall a t 5 0.885 PR/S 5 0.885 ~ 0.036 γ HR! /Sor ~ 0.885 ~ 0.2489 γ HR! /S !
minimum of length “L” of 8 in. (203 mm) on tanks up to 4 ft
(1219 mm) in diameter, and 12 in. (304 mm) on tanks over 4 where:
ft (1219 mm) in diameter. The reinforcement shall then taper t = thickness, in. (mm),
into the side wall over an additional length “ M” of 4 in. (102 S = allowable stress (not to exceed 1⁄10 of ultimate strength),
mm) (see Fig. 2). Methods of manufacture that incorporate psi (kPa) (see 11.8),
stiffening bands as a means of knuckle stabilization, are γ = specific gravity of fluid,
permissible alternatives by agreement between purchaser and P = pressure, psi (kPa),
fabricator, provided that the fabricator can document the R = inside radius of dished head, in. (mm), and
H = distance from the top of the fluid to the deepest portion
validity of design.
of the bottom, in. (mm).
6.4.4 The tank bottom shall not have variations from a
nominally flat plane that would prevent uniform contact of the NOTE 12— An alternate method for design of an elevated toruspherical
dished bottom is shown in Appendix X3.
entire bottom surface with a properly prepared support surface
when the tank is filled with liquid. The bottom laminate surface 6.4.5.1 Minimum thickness of ellipsodial heads, (2:1) shall
shall be a hand-work finish and shall have no excessive be calculated as follows:

FIG. 2 Flat-Bottom Tank Corner Detail

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D4097 − 19
PD TABLE 2 Standard Tank Inside Diameters
t5
2S in. (mm) in. (mm) in. (mm)
24 (610) 54 (1372) 96 (2438)
6.4.5.2 Minimum thickness of conical heads shall be calcu- 30 (762) 60 (1524) 108 (2743)
lated as follows: 36 (914) 66 (1676) 120 (3048)
42 (1067) 72 (1829) 132 (3353)
PD 48 (1219) 84 (2134) 144 (3658)
t5
2S· cos ~ } !

where:
} = 1⁄2 of APEX angle of the cone at the centerline of the
head (not to exceed 30°). the nozzle shall be at least equivalent to the inner surface and
6.4.6 The torispherical dished-bottom head shall have a interior layer (7.1.1 and 7.1.2) and shall be fabricated from the
radius of curvature that is equal to or less than the inside same resin as the tank head or shell to which it is attached.
diameter of the tank straight shell, and a minimum knuckle 6.7.2 Acceptable alternative methods are the use of contact-
radius of at least 6 % of the diameter of the head. molded pipe, filament-wound pipe in accordance with Speci-
6.4.7 Deflection of the flat bottom when the tank is empty, fication D2996, or centrifugally cast pipe in accordance with
commonly known as “oil canning,” is permissible as long as Specification D2997, joined to a suitable contact-molded
the requirements of 6.4.4 are met. (Specification D5421), compression-molded, or filament-
6.5 Open-Top Tanks—The top edge of open-top tanks shall wound flange (Specification D4024). The corrosion-resistant
have a horizontal reinforcing flange or other means of rein- barrier of the contact molded portions of such nozzles shall be
forcement sufficiently rigid to maintain the shape of the tank equivalent to the inner surface and interior layer (7.1.1 and
after installation. The flange shall be in accordance with Table 7.1.2) and shall be fabricated from the same resin as the tank
1. See Table 2. head or shell to which it is attached.
6.7.3 Nozzles 4 in. (102 mm) and smaller shall be supported
6.6 Joints: by a suitable gusseting technique using plate gussets or conical
6.6.1 The cured resin surfaces to be overlayed shall be gussets, as shown in Fig. 3 and Fig. 4. Plate gussets, where
roughened using 36 or coarser grit abrasive media. The needed, shall be evenly spaced around the nozzle and are to be
roughened area shall extend beyond the lay-up area so that no added after complete assembly of nozzle on shell. Larger
reinforcement is applied to an unroughened surface. Surfaces nozzles, subject to superimposed mechanical forces, require
shall be clean and dry before lay-up. The entire roughened area special consideration.
shall be coated with paraffinated resin after the joint lay-up is 6.7.4 Manways installed in top heads may be of the flanged
made. design or of a nonflanged design, as agreed upon between the
6.6.2 The secondary laminate joints are used to join hoop fabricator and purchaser.
segments of the straight shell, or to join the bottom or top head 6.7.4.1 Side-shell manways shall be in accordance with
to the shell. The thickness of the structural joint overlay shall 7.3.2 and 7.3.3.
be equal to the shell thickness as determined in 6.1. 6.7.4.2 Typical manway dimensions are shown in Table 5.
6.6.3 The minimum width of the structural joint overlay for
bottom supported tanks is shown in Table 3. NOTE 13—Tanks over 6 ft (1.8 m) straight-shell may need both top- and
side-shell opening manways for safety and maintenance considerations.
6.6.4 The corrosion-resistant barrier component of the joint
shall be formed in the same manner as the inner surface and the 6.7.5 Vents:
interior layer (7.1.1 and 7.1.2) and shall not be considered a 6.7.5.1 Vents that discharge freely into the atmosphere shall
structural element in determining joint thickness. The mini- be provided in all Type I closed-top tanks. Minimum vent size
mum overlay width shall be 4 in. (100 mm). shall be sufficient to handle the flow displacement of all
6.6.5 The thickness of a joint near the bottom tangent line combined inlet or outlet nozzles without creating any pressure
shall not be considered to contribute to the knuckle reinforce- above atmospheric pressure, or any vacuum condition.
ment of 6.4.3, but shall be additive thereto. NOTE 14—Special vent sizing consideration should be given to the
6.7 Fittings: numerous operating situations that could otherwise cause a positive or a
negative pressure in a closed tank. Since overfilling a closed tank with a
6.7.1 The more common method of fabricating nozzles is by top vent can cause it to be overpressurized, a suitably sized overflow or
contact molding both the nozzle neck and flange to the other appropriate protection may be required to prevent overpressuring the
dimensions shown in Table 4. The corrosion-resistant barrier of tank.

TABLE 1 Minimum Acceptable Contact Molded Laminate Physical Properties


Property Thickness, in. (mm)
⁄ to 3⁄16 (3.2 to 4.8)
18 ⁄ (6.4)
14 ⁄
5 16 (7.9) ⁄ and up (9.5 and up)
38

Ultimate tensile strength, min, psi (kPa) 9 000 (620.5) 12 000 (827.4) 13 000 (930.8) 15 000 (1 034)
Flexural strength, min, psi (kPa) 16 000 (1 103) 19 000 (1 310) 20 000 (1 399) 22 000 (1 517)
Flexural modulus for elasticity (tangent), psi (kPa) 700 000 (48 263) 800 000 (55 158) 900 000 (62 053) 1 000 000 (68 948)

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TABLE 3 Minimum Widths of Joint Overlay for Circumferential Joints

H × D = minimum 60 100 140 180 220 260 300 340 380 420 460 500
width of outside,A
in. 4 4 5 6 7 8 9 10 11 12 13 14
(mm) (102) (102) (127) (152) (178) (203) (229) (254) (279) (305) (330) (356)

where:
H = distance from the top of the liquid level to the joint, ft (m), and
D = inside diameter of the tank, ft (m).

A
Axial joint overlay widths shall be twice the width shown in the table.

TABLE 4 Reinforcing Flange for Open-Top TanksA,B


C
L Tank Diameter, ft (m) Flange Flange Dimensions
ft (m) 2 (0.610) 4 (1.219) 6 (1.829) 8 (2.438) 9 (2.743) 10 (3.048) 11 (3.353) 12 (3.658) Type Width, in. (mm) ThicknessD ,
in. (mm)

2 (0.610) A A A C D E F G A 2 (51) 14⁄ (6)


4 (1.219) A A A C D E F G B 2 (51) ⁄ (10)
38

6 (1.829) A A A C D E F G C 2 (51) 1⁄2 (13)

8 (2.438) A A A C D E F G D 21⁄2 (64) 3⁄8 (10)

10 (3.048) A A B C D E F G E 21⁄2 (64) 1⁄2 (13)

12 (3.658) A A B D D E F G F 3 (76) 3⁄8 (10)

14 (4.267) A A B D E F F G G 3 (76) 1⁄2 (13)

16 (4.877) A A C E E G G H H 3 (76) 5⁄8 (16)

18 (5.486) A A C E F G G H J 3 (76) 3⁄8 (19)

20 (6.096) A A D E F G H J K 3 (76) 1 (25)


24 (7.315) A B D F G H J K
30 (9.144) A B E G H H K K
36 (10.973) A B E H J K K
40 (12.192) A B E H J K
A
This table is based on handling considerations only. Significant superimposed loads, such as from wind or seismic conditions, should be considered independently.
B
Reinforcement configurations other than flanges may be used if equal or greater stiffness is provided.
C
L = maximum distance from flange to tank bottom or to the shell stiffener when used.
D
Flange thickness shall be at least equal to adjacent vessel wall thickness.

6.7.6 Type II tanks shall be designed to withstand the and top and bottom knuckle requirements. Fluid level in the
specified positive or negative pressures not to exceed 14 in. of tank is an important consideration in the analysis.
water (355.6 mm). Special design consideration shall be given 6.7.6.1 Flat-bottom tanks shall have all hold-down lugs
to buckling of tank wall and heads, the hold-down lug system, properly secured to the foundation, in accordance with the tank

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FIG. 3 Plate-Type Gussets

NOTE 1—This design does not require lay-up of nozzle neck to exterior tank wall.
FIG. 4 Conical-Type Gussets

TABLE 5 Typical Dimensions of Manways

NOTE 1—Bolt size equals bolt hole diameter minus 1⁄8 in. (3 mm).
NOTE 2— Gaskets shall be 1⁄8 in. thick full-face elastomeric material having a hardness of Shore A80 ± 5.
Minimum Diameter of Minimum Thickness of Minimum Manway Wall
Minimum Flange and Cover, Flange and Cover, Thickness, Diameter of Bolt Circle, Number of Bolt Hole Diameter,
Size, in. in. (mm) in. (mm) in. (mm) in. (mm)A,B,C Bolts in. (mm)

Pressurized Manway—up to 15 psig


20 271⁄2 (699) 1 (25.4) 3⁄8 (9.5) 25 (635) 20 ⁄ (19)
34

22 30 (762) 1 (25.4) 3⁄8 (9.5) 27 (686) 20 ⁄ (19)


34

24 32 (813) 11⁄4 (31.8) 3⁄8 (9.5) 291⁄2 (749) 20 3⁄4 (19)

Manway—Atmospheric Pressure up to 0.5 psig


20 271⁄2 (699) 3⁄8 (9.5) 1⁄4 (6.4) 25 (635) 20 ⁄ (12.7)
12

22 30 (762) 3⁄8 (9.5) 1⁄4 (6.4) 27 (686) 20 ⁄ (12.7)


12

24 32 (813) 3⁄8 (9.5) 1⁄4 (6.4) 291⁄2 (748) 20 1⁄2 (12.7)

A
± 0.06 in. (1.5 mm) (ASME/ANSI B 16.5).
B
± 0.03 in. (0.76 mm) center to center of adjacent bolt holes (ASME/ANSI B 16.5).
C
± 0.06 in. (1.5 mm) eccentricity between bolt circle and center of nozzle.

fabricator’s recommendation for the design of the lugs used 6.8.1 Hold-down lugs shall be placed on the tank in such a
and for the tank installation and operation. way that they do not protrude below the bottom surface of the
6.8 Hold-Down Lugs—Hold-down lugs shall be a require- tank.
ment on all tanks for outdoor service, on all Type II tanks, and 6.9 Lifting Lugs—Lifting lugs or other provisions for lifting
on tanks subject to seismic loads or vibrations. The design tanks (see Appendix X1) shall be provided for tanks over 500
number and attachment of such lugs is the responsibility of the
lb (227 kg) in weight.
fabricator, based on the wind, seismic, and other loads speci-
fied by the purchaser.

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7. Laminate Construction Requirements fabric, surfacing mat shall be overlapped. Laps in subsequent
7.1 Structural Tank—The laminate comprising the structural layers shall be staggered at least 2.25 in. (60 mm) from laps in
tank (bottom, cylindrical shell, top head) shall consist of a the preceding layer.
corrosion-resistant barrier comprised of an inner surface, 7.1.3.1 When the outer surface of this structural layer is to
interior layer, and a structural layer. be subject to spillage or a corrosive environment, a resin-rich
7.1.1 Inner Surface—The inner surface exposed to the layer in accordance with 7.1.1 shall be applied over the final
chemical environment shall be a resin-rich layer 0.010 and layer of reinforcement.
0.020 in. (0.254 to 0.508 mm) thick, reinforced with a suitable 7.1.3.2 Where air-inhibited resin is exposed to air, full
chemical-resistant glass-fiber surfacing mat or with an organic- surface cure shall be obtained by coating such surface with a
fiber surfacing mat, in accordance with 5.2.4. coat of resin containing 0.2 to 0.6 % paraffin with a melt point
of 122 to 126°F (50 to 52°C). Other techniques such as
NOTE 15—This resin-rich inner surface will usually contain less than sprayed, wrapped, or overlaid films are also acceptable meth-
20 % by weight of reinforcing material.
ods to attain surface cure. The acetone sensitivity test may be
7.1.2 Interior Layer—The inner surface layer exposed to the used to check surface cure (see Note 19).
corrosive environment shall be followed with a layer composed 7.1.3.3 Tanks used for outdoor service or subject to ultra-
of resin, reinforced only with noncontinuous glass-fiber strands violet exposure shall incorporate provisions to minimize ultra-
applied in a minimum of two plies of chopped-strand mat violet degradation. Suitable methods include use of ultraviolet
equivalent to a total of 3 oz/ft2 (0.92 kg/m2). As an alternative, absorbers, incorporation of pigment of sufficient opacity in the
a minimum of two passes of chopped roving of minimum outer surface of the resin rich layer, or use of resins inherently
length 0.5 in. (13 mm) to a maximum length of 2.0 in. (50.8 resistant to ultraviolet degradation. Since pigmentation makes
mm), shall be applied uniformly to an equivalent weight. Each inspection difficult, it shall be added after inspection or
ply of mat or pass of chopped roving shall be well rolled prior otherwise by agreement between the purchaser and fabricator.
to the application of additional reinforcement. The combined 7.1.4 All woven roving, nonwoven biaxial fabric, and sur-
thickness of the inner surface and interior layer shall not be less facing mat shall be overlapped. Laps in subsequent layers shall
than 0.10 in. (2.5 mm). be staggered at least 2.25 in. (67 mm) from laps in the
7.1.2.1 Glass content of the inner liner and the interior layer preceding layer.
combined shall be 27 6 5 % by weight, when tested in 7.1.5 Where woven roving or nonwoven biaxial fabric is
accordance with 11.4. used, chopped-strand glass reinforcement shall be used as
7.1.2.2 The degree of cure of the laminate shall be such as alternating and final layers.
to exhibit a Barcol hardness on the inner surface of at least
90 % of the resin manufacturer’s minimum specified hardness 7.2 Joints:
for the cured resin, when tested in accordance with 11.7 and 7.2.1 The width of the first layer of joint overlay shall be 3
Note 18, Note 19, and Note 20. in. (76 mm) minimum. Successive layers shall uniformly
7.1.3 Contact Molded Structural Layer in Top and Bottom increase in width to that specified in Table 6 to form a smooth
Heads—Subsequent reinforcement shall be comprised of 1.5 contour laminate centered on the joint.
oz/ft2 (0.46 kg/m2) chopped strand mat or equivalent weight of 7.2.2 A highly filled resin paste shall be placed in the
chopped roving or shall be comprised of chopped strand mat or crevices between joined pieces, leaving a smooth surface for
chopped roving and such additional number of alternating plies lay-up.
of 24 oz/yd2 (0.81 kg/m2) woven roving or 18 oz/yd2 (0.61 7.2.3 The cured resin surfaces to be joined shall be rough-
kg/m2) nonwoven biaxial fabric to a thickness as required to ened using 36 or coarser abrasive grit media to expose glass
meet the physical properties that are used for the design. The fibers. This roughened area shall extend beyond the lay-up
use of woven roving is optional. The designations of these areas so that no reinforcement is applied to an unprepared
specific weights of glass reinforcement are for reference only surface. The entire roughened area shall be coated with
and may be comprised of other weight combinations of paraffinated resin after joint overlay is made.
reinforcement materials, when agreed to between the fabricator 7.2.4 The interior overlay of a joint shall consist of a
and purchaser. Each successive ply or pass of reinforcement minimum of two plies of 1.5 oz/ft2 (0.46 kg/m2) chopped
shall be well rolled prior to the application of additional strand mat reinforcement, followed by a resin-rich layer
reinforcement. Where woven roving or nonwoven fabric is reinforced with surfacing mat. This overlay shall be the
used, chopped strand glass reinforcement shall be used as equivalent of 7.1.1 and 7.1.2 combined, and shall be centered
alternating and final layers. All woven roving and nonwoven on the joint. It shall be finished in accordance with 7.1.3.2.

TABLE 6 Shear Bond Length (Fig. 5 and Fig. 6)


NOTE 1—When internal overlay serves only as a corrosion barrier, the total shear length must be placed on the exterior overlay.
Overlay Thickness, in. ⁄ (6.4)
14 ⁄
5 16 (8) ⁄ (9.5)
38 ⁄
7 16 (11) ⁄ (13)
12 ⁄
9 16 (14) ⁄ (16)
58 ⁄
11 16 (17.5) ⁄ (19)
34 ⁄ (22)
78 1 (25.4)
(mm)
h (shear length), in. 3 (76) 3 (76) 3 (76) 3 ⁄ (90)
12 4 (100) 4 ⁄ (114)
12 5 (127) 5 ⁄ (140)
12 6 (152) 7 (178) 8 (203)
(mm)

where: h = total shear length (ho + hi) (Fig. 5 and Fig. 6).

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7.2.5 The outer structural overlay of a joint shall be centered 7.3.2.1 Nozzle Projection—The installed nozzle shall main-
on the joint, fabricated in accordance with 6.6.1, and shall be tain a minimum clearance of 3 in. (76 mm) between the back
finished in accordance with 7.1.2. face of the flange and the exterior of the cutout opening
7.3 Fittings and Accessories: reinforcement. In addition, this clearance shall not be less than
7.3.1 The surface of fittings, tank accessories, and the the shear distance required for proper installation of the nozzle
laminates required for their installation, that are exposed to the (see 7.3.3).
corrosive media, shall be constructed in accordance with 7.1.1 7.3.2.2 Cutout Reinforcement Laminate—When a vessel
and 7.1.2, except for those fitting surfaces which are made by shell or head is cut in an area bearing hydrostatic pressure, P,
manufacturing processes other than contact molding. the cutout shall be reinforced on a circular area concentric with
7.3.1.1 The cut edges of all laminates exposed to the the cutout as shown in Fig. 5 and Fig. 6. Acceptable patterns of
chemical environment shall be sealed with a laminate conform- reinforcement placement are shown in Fig. 7.
ing to 7.1.1 and 7.1.2. Where shape, thickness, or other 7.3.2.3 Cutout Reinforcement Diameter—The outer diam-
restrictions preclude covering the edges with the preceding eter of the cutout reinforcing laminate, dr, shall not be less than
laminate, such cut edges and any machined flange faces shall two times the nominal nozzle diameter. For nozzles less than 6
be at least coated with resin. In either case, the resin used shall in. (152 mm) in diameter, the minimum cutout reinforcement
be that used in the equipment laminate and finished in diameter, dr, shall be the nominal nozzle size plus 6 in. (152
accordance with 7.1.3.2. mm).
7.3.2 Nozzle and Manway Installation—Flanged nozzles 7.3.2.4 Cutout Reinforcement Thickness—The thickness, tr,
may be installed with the pipe stub flush with the inside of the of the cutout reinforcement laminate for nozzles installed in
tank shell (Flush Type, Fig. 5) or projecting inside the tank cylindrical shells or dished heads shall be determined as
(Penetrating Type, Fig. 6). follows:

FIG. 5 Flush Nozzle Installation

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FIG. 6 Penetrating Nozzle Installation

t r 5 PDK/2S r reinforcing layers should be staggered to avoid overlapping


where: and (on cylindrical shell installations) shall not be placed so
they parallel the axis of the tank. The intent of this requirement
K = 1.0 for nozzles 6-in. (152-mm) diameter and larger,
is to avoid orienting joints in reinforcing layers perpendicular
K = d/(dr − d) for nozzles less than 6-in. (152-mm)
to the maximum load-bearing direction (circumferential).
diameter,
P = hydrostatic pressure at the point of nozzle installation, 7.3.3 Nozzle Installation Laminates—Nozzle installation
psi (kPa), laminate dimensions are shown in Fig. 5 and Fig. 6. Installation
D = inside diameter of tank, in. (mm), laminate placements are shown in Fig. 7. The all interior
Sr = allowable tensile stress (not to exceed 1⁄10 of the installation laminate placement is used only when the nozzle
ultimate strength of the cutout reinforcing laminate) being installed has an integral conical gusset preventing
(Table 6), application of an exterior laminate.
d = nominal nozzle diameter, in. (mm), and 7.3.3.1 Installation Laminate Thickness—The inside and
dr = cutout reinforcement diameter, in. (mm). outside installation thicknesses (tl and to) combined shall be at
This thickness, tr, may be applied to the outer or inner least as thick as the nozzle neck.
surfaces, or be divided between them as shown in Fig. 7. 7.3.3.2 Inside Installation Laminate Construction—The in-
NOTE 16—When tr is calculated to be 1⁄8 in. (3.2 mm) or less, it can be side installation laminate shall be constructed using only
disregarded, as the strength requirements will be met by to, the overlay noncontinuous glass reinforcement, except that when woven
thickness shown in Fig. 5 and Fig. 6. roving is included to strengthen the laminate, it shall be
7.3.2.5 When reinforcing materials are cut to facilitate preceded and followed by a layer of 11⁄2 oz mat and then
placement around an installed nozzle, joints in successive covered with a laminate equivalent to 7.1.1 and 7.1.2. When

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NOTE 1—This installation method is used only when the nozzle is being installed with an integral conical gusset which would prevent application of
an exterior laminate.
FIG. 7 Nozzle Installation and Cutout Reinforcement Location Alternate

the inside laminate consists only of a corrosion barrier, the conical type gussets are shown in Fig. 3 and Fig. 4. Other
length of the laminate, hr, shall be a minimum of 3 in. and gusseted nozzle installations may be used as agreed upon
hi shall be the lesser of 3 in. or the nominal radius of the nozzle. between fabricator and purchaser.
7.3.3.3 Installation Laminate Lengths—The length of the 7.3.5 Location of Cutouts on the Shell—For cutouts made
outside laminate, ho, and the inside laminate, hi, shall each be within 6 in. (152 mm) of the knuckle radius area of a head or
equal to the shear length, hs, given in Table 6, based on the within 6 in. (152 mm) of a shell-to-shell or shell-to-head joint,
thickness of the individual laminates. additional hole cutout reinforcement is required, unless the
7.3.3.4 In nozzle installations where the installation overlay area of installation is at a point within the vessel that is not
is installed before the cutout reinforcement has fully cured, that exposed to hydrostatic pressure.
portion of the overlay which extends onto the tank shell may be 7.3.6 All nozzles and manways shall be installed in accor-
considered to become a part of the cutout reinforcement dance with Fig. 5 and Fig. 6. The interior overlay shall present
laminate if the installation laminate length is extended to the the same corrosion resistance to the fluid as specified in 7.1.1
required cutout reinforcement diameter, dr. and 7.1.2.
7.3.3.5 Monolithic Installation—The total bond thickness,
tm, shall be the greater of either the cutout reinforcement
8. Requirements
thickness, tr, or the outside bond thickness, to.
7.3.4 Gussets—If gussets (either plate or conical) are used to 8.1 Physical Properties—The minimum physical properties
stiffen the installed nozzle, gusset installation laminates are in of the laminate constructions used to manufacture various
addition to the requirements of 7.3.3. Typical plate type and portions of a tank and its accessories shall be as shown in Table

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D4097 − 19
6 when tested in accordance with 11.5 and 11.6 or as agreed 9.3 Tolerance on overall tank height shall be 1⁄2 %, but shall
upon between the manufacturer and the purchaser. not exceed 61⁄2 in. (613 mm).
8.2 Degree of Cure—Degree of cure of the laminate shall be 9.4 Nozzle flange faces shall be perpendicular to the cen-
found by determining the Barcol hardness as indicated in 11.7. terline of the pipe within tolerances shown in Fig. 8, and shall
NOTE 17—The use of organic reinforcing materials may reduce the
be flat within 61⁄32 in. (60.8 mm) through 18-in. (457-mm)
Barcol hardness readings without necessarily indicating undercure. nozzle size and 61⁄16 in. (61.6 mm) for larger nozzles sizes.
NOTE 18—A test for the surface cure of polyester reins is as follows: Tolerances on installation are shown in Fig. 8.
Remove mold release or paraffin wax, if present, and wipe clean of dust.
Rub a small amount of acetone on the laminate surface until it evaporates.
9.5 The standard orientation of flanges shall provide bolt
If the surface becomes softened or tacky, it is an indication of undercure. holes straddling the normal centerlines of the tank. Bolt holes
of flanges located on the tank top or bottom shall straddle the
9. Dimensions and Tolerances principal X-Y centerlines of the vessel or lines parallel to it as
9.1 Standard tank diameters, based on internal measure- shown in Fig. 8.
ments with the tank in the vertical position, are listed in Table 9.6 The location of nozzles shall be held to the tolerances
7. Tolerance on the inside diameter, including out-of- shown in Fig. 8.
roundness, shall be 61 %.
9.2 Where employed, shell taper shall be additive to the 10. Workmanship, Finish, and Appearance
figure used for the tank diameter, unless otherwise specified by 10.1 The minimum acceptable level for workmanship and
the manufacturer and accepted by the purchaser. The shell taper finish of the finished laminate shall conform to the require-
shall not exceed 1⁄2 ° per side. ments specified in Section 9 of Specification C582.

TABLE 7 Dimensions for Contact Molded Nozzles (25 psi Rating)


Nozzle Inside Maximum Wall Minimum Flange Minimum Hub Minimum Hub
Diameter, (D), Thickness, (tn), Thickness, (tt), Thickness, (th), Length, (h),
in. (mm) in. (mm) in. (mm) in. (mm) in. (mm)

1 (25) ⁄ (5)
3 16 ⁄ (13)
12 ⁄ (6)
14 2 (51)
11⁄2 (38) ⁄ (5)
3 16 ⁄ (13)
12 ⁄ (6)
14 2 (51)
2 (51) 3⁄16 (5) 1⁄2 (13) ⁄ (6)
12 2 (51)
3 (76) 3⁄16 (5) 1⁄2 (13) 1⁄2 (6) 2 (51)
4 (102) 3⁄16 (5) 1⁄2 (13) 1⁄2 (6) 2 (51)
6 (152) 3⁄16 (5) 1⁄2 (13) 1⁄2 (6) 2 (51)
8 (203) 3⁄16 (5) 9⁄16 (14) 5⁄16 (8) 21⁄4 (57)
10 (254) 3⁄16 (5) 11⁄16 (17) 3⁄8 (10) 23⁄4 (70)
12 (305) 3⁄16 (5) 3⁄4 (19) 3⁄8 (10) 3 (76)
14 (356) 1⁄4 (6) 13⁄16 (21) 7⁄16 (11) 31⁄4 (83)
16 (406) 1⁄4 (6) 7⁄8 (22) 7⁄16 (11) 31⁄2 (89)
18 (457) 1⁄4 (6) 15⁄16 (24) 1⁄2 (13) 33⁄4 (95)
20 (508) 1⁄4 (6) 1 (25) 1⁄2 (13) 4 (102)
24 (610) 1⁄4 (6) 11⁄8 (29) 9⁄16 (14) 41⁄2 (114)

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Nozzle Inside Diameter, in. Permissible Angular Deviation, −0

Up to 10 1°
10 and larger ⁄ °
12

NOTE 1—Larger tolerances may be agreed upon between purchaser and fabricator for tanks over 12 ft in diameter.
FIG. 8 Nozzle Location and Orientation Tolerances

NOTE 19—A representative laminate sample may be used for determi- layer. The glass content of the separated sample shall be
nation of an acceptable surface finish and acceptable level of visual determined in accordance with Test Method D2584.
imperfections.
11.5 Tensile Strength—Tensile strength of the laminate shall
11. Test Methods be determined in accordance with Method D638.
11.1 Conditioning—Condition the specimens prior to test at 11.6 Flexural Properties—Determine the flexural strength
23 6 2°C (70 to 77°F) for not less than 40 h in accordance with and tangent modulus of elasticity of the laminate in accordance
Procedure A of Method D618, for those tests when condition- with Method D790.
ing is required and in all cases of disagreement.
11.7 Degree of Cure—Degree of cure of the laminate shall
11.2 Test Conditions—Conduct the test at a laboratory be found by determining the Barcol hardness in accordance
temperature of 70 to 77°F (23 6 2°C) unless otherwise with Test Method D2583.
specified.
11.8 Physical Properties—Where required, physical proper-
11.3 Chemical Resistance of Resin—Determine the chemi- ties shall be determined in accordance with the test methods
cal resistance of the resin in accordance with Practice C581. listed in Specification C582.
11.4 Glass Content—Determine the glass content of the NOTE 20—A useful technique to check for cure of a non-molded surface
inner liner and interior layer combined. Obtain a test sample by of a polyester laminate is as follows: Rub a few drops of acetone on the
carefully splitting these combined areas from the structural laminate surface until it evaporates. If the surface becomes softened or

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D4097 − 19
tacky, it is an indication of under cure. vertical position. The cradles or skid shall be padded and
NOTE 21—Barcol hardness values may vary when tests are conducted at secured to the bed of the vehicle in such a manner that will
temperatures that differ from those shown in 11.7.
prevent damage to the tank with normal handling. The tank
12. Product Marking shall be secured to the cradles or skid so that there can be no
12.1 The tank shall be marked to identify the producer, date movement of the tank in a relation to the skid or cradle under
of manufacture, the capacity, all resins used, inner surface normal handling.
reinforcements, specific gravity, design temperature, and the 14.3 A suitable stiffening member shall be provided at the
words “Pressure-Atmospheric,” or the operating pressure and open end of open-top tanks.
vacuum, shall be imprinted on the tank.
14.4 Tanks shall be loaded to provide at least 2-in. (50.8-
12.2 Additional marking requirements may be needed for
mm) clearance between the tank (including fittings) and the
compliance with local codes. It is the responsibility of the
bulkheads or bed of the vehicle.
purchaser or the user, or both, to specify additional labelling
requirements for the vessel, such as liquid content, operating 14.5 When two or more tanks are shipped on the same
and safety instructions, NFPA symbols, and any other warnings vehicle, sufficient clearance or padding shall be provided
necessitated by local codes. between tanks to prevent contact in transit.
13. Packaging and Package Marking 14.6 Upon arrival at the destination, the purchaser shall be
13.1 All packing, packaging, and marking provisions of responsible for inspection for damage in transit. If damage has
Practice D3892 shall apply to this specification. occurred, a claim should be filed with the carrier by the
purchaser and the supplier should be notified. If the damage is
14. Shipping not first repaired by the fabricator prior to the tank being put
14.1 Since there are variations in the design of support into service, the purchaser accepts all future responsibility for
cradles, lifting and hold-down lugs, and methods of shipping, the effects of tank failure resulting from such damage.
the manufacturer’s special instructions shall be followed in all
cases. 15. Keywords
14.2 Tanks shall be mounted on cradles if shipping 15.1 above ground; atmosphere; contact-molded; polyester;
horizontally, or on a suitable skid of pallet if shipping in the vinylester

APPENDIXES

(Nonmandatory Information)

X1. HANDLING AND INSTALLATION

X1.1 Handling shackle of the crane and the tank should be at least equal to the
X1.1.1 The following normal precautions should be taken in span between the lugs used for lifting. If this is not possible, a
handling the tank at the destination: spreader bar must be used to approximate the same angle in
X1.1.1.1 Proper rigging practices should be observed at all lifting.
times. Hoisting equipment operators should attach a guide line X1.1.1.6 Where tanks are not equipped with lifting lugs, it
to prevent the tank from swinging out of control. is recommended that such tanks be lifted with rope slings (over
X1.1.1.2 The tank should not be dropped or allowed to 1 in. in diameter) or fabric straps positioned near each end of
strike any other object. Damage caused by such action may the tank. Tanks can be moved by positioning fork lift trucks on
result in cracking the inner corrosion-resistant liner, as well as either side of the tank with forks padded.
the structural portion of the tank. X1.1.1.7 Under no conditions should chains or cables be
X1.1.1.3 The tank should not be rolled or slid on rough allowed to contact a tank. Full protection must be provided
ground. Never set a tank upon a fitting or other protrusion that when using chains or cables. Do not attach lifting devices to
may be attached to the shell. any fitting other than lifting lugs.
X1.1.1.4 In working around the tank, care should be exer- X1.1.1.8 When storing the tank on the ground prior to
cised to prevent tools, scaffolding, or other objects from installation, it should be placed on the shipping cradles and tied
striking the tank or being dropped on, or inside the tank. down so that it cannot roll due to wind or sloping ground.
Soft-soled shoes should be worn by workman entering the
tank. Where ladders are used (inside and outside), all points of
X1.2 Installation
contact with the tank should be cushioned to protect the surface
from scratching or point loading. X1.2.1 Vertical flat bottom tanks should be installed on a
X1.1.1.5 The use of a crane is recommended, both in lifting base providing continuous support and having sufficient
and positioning the tank. The clearance between the head strength to support the weight of the tank full of liquid with

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D4097 − 19
negligible deflection. Full support of the bottom should be attaching to other fittings. Prior to hoisting the top end, a
obtained by one of the following: suitable protection pad of material should be placed under the
X1.2.1.1 If the surface of the pad and the bottom of the tank bottom pivot point of the tank so that as the tank rises, the
are flat and have no projections from the plane surface, the tank strain is taken on the pad. The hoist wire should be connected
may be set on such a surface. to the top lifting lugs, and tank should be raised carefully using
X1.2.1.2 If the conditions of X1.2.1.1 cannot be met, guide ropes to prevent sudden swinging.
methods of support recommended by the manufacturer should X1.2.3.2 All hold-down lugs supplied should be utilized to
be used. secure the tank to its pad. Hold-down lugs should be grouted or
X1.2.2 If the tank has a bottom drain, a hole should be shimmed to prevent excessive loads being trans-ferred to the
provided in the pad with sufficient clearance so that the drain tank shell.
and its flange will not contact the base at any point. X1.2.3.3 Valves, controllers, or other heavy items connected
X1.2.3 Erection of Vertical Tank: to the tank nozzle should be independently supported.
X1.2.3.1 Tanks should be handled with a crane, utilizing the X1.2.3.4 When agitators, mixers, or cooling/heating coils
lifting lugs provided. Do not attempt to lift the tank by are to be installed, special design considerations are to be used.

X2. WALL THICKNESSES

X2.1 The wall thicknesses shown in Table X2.1 can be used


as a guide for tanks designed in accordance with the equation
in 6.1, using the minimum laminate physical properties given
in Table 6.
TABLE X2.1 Wall ThicknessesA
Distance from Tank Diameter, ft (Inch-Pound Units)
top, ft 2 21⁄2 3 31⁄ 2 4 41⁄ 2 5 5 1⁄ 2 6 7 8 9 10 11 12
Wall Thickness, in.

2 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16

4 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16 ⁄
3 16

6 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 14 ⁄ 14 ⁄ 14 ⁄
8 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 1⁄4 1 ⁄4 1⁄4 14 ⁄ 14 ⁄ 14 ⁄
10 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 1⁄4 1 ⁄4 1⁄4 1 ⁄4 1⁄5 ⁄
5 16 ⁄
5 16 ⁄
5 16

12 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 3⁄16 1 ⁄4 1 ⁄4 1 ⁄4 1⁄4 1 ⁄4 5⁄16 ⁄


5 16 ⁄
5 16 38 ⁄
14 3⁄16 3⁄16 3⁄16 3⁄16 1 ⁄4 1 ⁄4 1 ⁄4 1 ⁄4 1 ⁄4 5⁄16 5⁄16 5⁄16 5⁄16 ⁄
38 38 ⁄
16 3⁄16 3⁄16 3⁄16 1 ⁄4 1 ⁄4 1 ⁄4 1 ⁄4 1 ⁄4 1 ⁄4 5⁄16 5⁄16 3⁄8 3⁄8 3 ⁄8 ⁄
7 16

18 3⁄16 3⁄16 3⁄16 1 ⁄4 1 ⁄4 1 ⁄4 1 ⁄4 5⁄16 5⁄16 5⁄16 3⁄8 3⁄8 3⁄8 7⁄16 12 ⁄
20 3⁄16 3⁄16 1⁄4 1 ⁄4 1 ⁄4 1 ⁄4 5⁄16 5⁄16 5⁄16 3⁄8 3 ⁄8 3⁄8 7⁄16 1⁄2 12 ⁄
22 3⁄16 1 ⁄4 1 ⁄4 1 ⁄4 1 ⁄4 5⁄16 5⁄16 5⁄16 5⁄16 3⁄8 3 ⁄8 7⁄16 1⁄2 1 ⁄2 ⁄
9 16

24 3⁄16 1 ⁄4 1 ⁄4 1 ⁄4 1 ⁄4 5⁄16 5⁄16 5⁄16 3⁄8 3⁄8 7⁄16 1⁄2 1⁄2 9⁄16 58 ⁄
Distance from Tank Diameter, m (SI Units)
top, m 0.61 0.76 0.914 1.07 1.22 1.37 1.524 1.68 1.88 2.134 2.44 2.743 3.048 3.35 3.55
Wall Thickness, mmA

0.61 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76
1.22 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76
1.33 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 6.35 6.35 6.35
2.44 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 4.76 6.35 6.35 6.35 6.35 6.35 6.35
3.05 4.76 4.76 4.76 4.76 4.76 4.76 4.76 6.35 6.35 6.35 6.35 6.35 7.94 7.94 7.94
3.66 4.76 4.76 4.76 4.76 4.76 4.76 6.35 6.35 6.35 6.35 6.35 7.94 7.94 7.94 9.53
4.27 4.76 4.76 4.76 4.76 6.35 6.35 6.35 6.35 6.35 7.94 7.94 7.94 7.94 9.53 9.53
4.38 4.76 4.76 4.76 6.35 6.35 6.35 6.35 6.35 6.35 7.94 7.94 9.53 9.53 9.53 11.11
5.49 4.76 4.76 4.76 6.35 6.35 6.35 6.35 7.94 7.94 7.94 9.53 9.53 9.53 11.11 12.70
6.10 4.76 4.76 6.35 6.35 6.35 6.35 7.94 7.94 7.94 9.53 9.53 9.53 11.11 12.70 12.70
6.72 4.76 6.35 6.35 6.35 6.35 7.94 7.94 7.94 7.94 9.53 9.53 11.11 12.70 12.70 14.29
7.32 4.76 6.35 6.35 6.35 6.35 7.94 7.94 7.94 9.53 9.53 11.11 12.70 12.70 14.29 15.88
A
This table is based on a design factor of 10 to 1 and a liquid specific gravity of 1.2 using the laminate construction detailed in 7.1.1, 7.1.2, and 7.1.3 and the minimum
laminate physical properties in Specification C582, Table 7.

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X3. DISHED BOTTOM

X3.1 An alternative method for calculating the thickness of


an elevated torispherical dished bottom head is as follows:
(refer to Fig. X3.1):
t c 5 PR c /2S 5 0.036 γ HRc /2S or ~ 0.2489 γ HRc W/2S !
t i 5 PR c W/2S 5 0.036 γ HRc W/2S or ~ 0.2489 γ HRc W/2S !

where:
tc = head thickness in area of the crown radius, in. (mm),
ti = head thickness in area of the knuckle radius, in. (mm),
S = allowable stress, psi (kPa),
γ = specific gravity of fluid
P = pressure, psi (kPa),
Rc = crown radius of dished head, in. (mm),
H = fluid head, in. (mm), FIG. X3.1 Thickness of Dished-Bottom Head
W = stress intersification factor = (1⁄4) (3 + square root Rc/ri),
and
ri = knuckle radius of the dished head, in. (mm).

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4161 − 14 (Reapproved 2019)

Standard Specification for


“Fiberglass” (Glass-Fiber-Reinforced Thermosetting-Resin)
Pipe Joints Using Flexible Elastomeric Seals1
This standard is issued under the fixed designation D4161; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D1600 Terminology for Abbreviated Terms Relating to Plas-


1.1 This specification covers axially unrestrained bell-and- tics
spigot gasket joints including couplings required for machine- F412 Terminology Relating to Plastic Piping Systems
made “fiberglass” (glass-fiber-reinforced thermosetting-resin) F477 Specification for Elastomeric Seals (Gaskets) for Join-
pipe systems, 8 in. (200 mm) through 156 in. (4000 mm), using ing Plastic Pipe
flexible elastomeric seals to obtain soundness. The pipe sys- 3. Terminology
tems may be pressure (typically up to 250 psi) or nonpressure
systems for water or for chemicals or gases that are not 3.1 Definitions:
deleterious to the materials specified in this specification. This 3.1.1 General—Definitions and abbreviations are in accor-
specification covers materials, dimensions, test requirements, dance with Terminology D883 or Terminology F412, and
and methods of test. Terminology D1600 unless otherwise indicated.
1.2 The values stated in inch-pound units are to be regarded 4. Types of Joints
as the standard. The values given in parentheses are provided 4.1 This specification covers two types of axially unre-
for information purposes only. strained joints based on effecting soundness of the joint
NOTE 1—There is a similar but technically different ISO Standard (ISO through compression of an elastomeric seal or ring:
8639). 4.1.1 Bell-and-spigot or coupling joint with the gasket
1.3 This standard does not purport to address all of the placed in the bell in circumferential compression. An elasto-
safety concerns, if any, associated with its use. It is the meric gasket joint design featuring a continuous elastomeric
responsibility of the user of this standard to establish appro- ring gasket placed in an annular space provided in the bell or
priate safety, health, and environmental practices and deter- socket of the pipe or fitting. The spigot end of the pipe or fitting
mine the applicability of regulatory limitations prior to use. is forced into the bell, thereby compressing the gasket radially
1.4 This international standard was developed in accor- to form a positive seal.
dance with internationally recognized principles on standard- 4.1.2 Bell-and-spigot or coupling joint with the gasket
ization established in the Decision on Principles for the placed on the spigot in circumferential tension: A push on joint
Development of International Standards, Guides and Recom- design featuring a continuous elastomeric ring gasket placed in
mendations issued by the World Trade Organization Technical an annular space provided on the spigot end of the pipe or
Barriers to Trade (TBT) Committee. fitting. The spigot is forced into the bell of the pipe or fitting,
thereby compressing the gasket radially to form a positive seal.
2. Referenced Documents NOTE 2—A coupling joint of these types is a loose double-bell sleeve
2.1 ASTM Standards:2 used to connect pipes which have spigots at both ends (see Fig. 1). All
D883 Terminology Relating to Plastics references to bells in this specification are applicable to the sleeve
coupling as well as to the integral bell of a bell-and-spigot gasket joint.

5. Materials and Manufacture


1
This specification is under the jurisdiction of ASTM Committee D20 on 5.1 The gasket shall be a continuous elastomeric ring of
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced circular or other geometric cross section and shall meet the
Plastic Piping Systems and Chemical Equipment.
Current edition approved April 1, 2019. Published May 2019. Originally requirements of Specification F477, unless otherwise specified
approved in 1982. Last previous edition approved in 2014 as D4161 – 14. DOI: in this specification. When a splice is used in the manufacture
10.1520/D4161-14R19.
2
of the gasket, no more than two splices shall be made in any
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
one gasket.
Standards volume information, refer to the standard’s Document Summary page on 5.1.1 The chemical composition of the gasket shall be
the ASTM website. compatible with the type of environment to which it will be

*A Summary of Changes section appears at the end of this standard


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6.3.1 Joints Using Circular Gasket Cross Sections:
6.3.1.1 The volume of the annular space provided for the
gasket, with the engaged joint at normal joint closure in
concentric position, and neglecting ellipticity of the bell and
spigot, shall not be less than the design volume of the gasket
furnished. For a rectangular gasket groove, the cross-sectional
area of annular space shall be calculated for minimum bell
inside diameter, maximum spigot outside diameter, minimum
width of groove at surface of spigot, and minimum depth of
groove. The volume of the annular space shall be calculated at
the centerline of the groove and considering the centroid of the
cross-sectional area to be at the midpoint between the surface
of the groove on which the gasket is seated and the surface of
the bell, if the groove is on the spigot, or the surface of the
spigot, if the groove is in the bell.
6.3.1.2 When the design volume of the gasket is less than
FIG. 1 Typical Coupling Joint Detail 75 % of the volume of the annular space in which the gasket is
confined, the dimensions and tolerances of the gasket, bell, and
subjected. Selection of the gasket composition shall be in spigot shall be such that, when the outer surface of the spigot
accordance with a purchaser and seller agreement. and the inner surface of the bell come into contact at some
point in their periphery, the deformation in the gasket shall not
NOTE 3—Consult the gasket manufacturer for advice as to the suitabil-
ity of specific rubber compounds for the intended service and joint exceed 40 % at the point of contact nor be less than 15 % at any
configurations. Items such as cold set when the joint is deflected under point. If the design volume of the gasket is 75 % or more of the
low-temperature conditions and maximum and minimum stretch in the volume of the annular space, the deformation of the gasket, as
gasket may be dependent upon the specific chemical compounds used. prescribed above, shall not exceed 50 % nor be less than 15 %.
5.2 Materials in the bell and spigot of the joint shall meet The cross-sectional area of annular space shall be calculated
the requirements of the applicable ASTM specification for the for average bell diameter, average spigot diameter, average
pipe or fitting of which the joint is a part. width of groove at surface of spigot, and average depth of
groove. The volume of the annular space shall be calculated at
6. Requirements the centerline of the groove and considering the centroid of the
6.1 Joint Surfaces—All surfaces of the joint upon or against cross-sectional area to be at the midpoint between the surface
which the gasket may bear shall be smooth and free of cracks, of the groove on which the gasket is seated and the surface of
fractures, or other imperfections that would adversely affect the the bell, if the groove is on the spigot, or the surface of the
performance of the joint. spigot, if the groove is in the bell.
6.2 Joint Geometry—The design of the joint shall include a NOTE 4—It is recognized that a relationship exists between the
means to retain the gasket and prevent it from being uninten- water-tightness of a joint, the gasket deformation, and the ratio of gasket
tionally displaced, either during assembly of the joint or during volume to space volume. For high-pressure applications, it may be
necessary to provide a very high-volume ratio to obtain a sound joint.
operation of the completed pipe system. Some manufacturers also have developed satisfactory joints with very
6.3 Dimensions and Tolerances—The provisions of 6.3.1.1 little gasket deformation, but meet the requirements of Section 6 by
apply only to a joining system utilizing a gasket of circular utilizing a very high-volume ratio.
cross section retained in a rectangular groove. Manufacturers 6.3.1.3 When determining the maximum percent deforma-
may submit to the purchaser detailed designs for joints utilizing tion of the gasket, the minimum depth of groove and the
gaskets or grooves, or both, of other geometric shape or for stretched gasket diameter shall be used and calculations made
joints not meeting the criteria of 6.3.1. Joints not meeting the at the centerline of the groove. When determining the mini-
requirements of this section shall meet the test requirements of mum percent deformation of the gasket, the maximum bell
Section 7; such joints shall be acceptable, provided the design diameter, the minimum spigot diameter, the maximum depth of
is approved by the purchaser prior to manufacture and provided groove, and the stretched gasket diameter shall be used and
the test pipe complies with the specified test requirements. Test calculations made at the centerline of the groove. For gasket
results may be extended to other diameters with the same joint deformation calculations, if the gasket is placed on the spigot
configuration, gasket shape and gasket composition provided in circumferential tension, the stretched gasket diameter shall
substantially similar gasket compressions and gasket hardness be determined as being the design diameter of the gasket
are maintained. Gasket dimensions may be increased or de- divided by the square root of (1 + x) where x equals the design
creased provided joint geometry is also appropriately propor- percent of gasket stretch divided by 100. If the gasket is placed
tioned so that critical relationships like gasket confinement are in the bell in circumferential compression, the design diameter
equal or superior to the tested joint. Design submissions shall of the gasket shall be used.
include joint geometry, tolerances, gasket characteristics, pro- 6.3.1.4 The taper on all sealing surfaces of the bell and
posed plant tests, and such other information as required by the spigot on which the elastomeric gasket may bear after closure
purchaser to evaluate the joint design for field performance. of the joint and at any degree of partial closure, except within

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D4161 − 14 (2019)
the gasket groove, shall form an angle of not more than 2° with
the longitudinal axis of the pipe. If the joint design does not
incorporate a mechanical locking feature, the joint shall be
designed and manufactured in such a way that at the position
of normal joint closure, the parallel surfaces upon which the
gasket may bear after closure will extend not less than 0.75 in.
(20 mm) away from the edges of the gasket groove.
6.3.1.5 Circular Gaskets:
(1) In a joint in which the gasket is placed in the bell in
circumferential compression, the circumferential length of the
gasket shall be such that, when inserted into the gasket groove,
the amount of circumferential compression will be less than
4 %. In larger pipe diameters, an adhesive may be required to Pipe Size Joint Angle
hold the gasket in place prior to installation. # 20 in. 3°
(2) In an elastomeric joint in which the gasket is placed on >20 in. # 33 in. 2°
>33 in. # 60 in. 1°
the spigot in circumferential tension, the circumferential length > 60 in. 1⁄ 2 °

of the gasket shall be such that, when installed in the gasket


groove, the amount of stretch shall not exceed 30 %. NOTE 1—Joint opening shall not exceed the maximum unstressed limit
(3) Compute the amount of compression or stretch by permitted by dimensional clearance between spigot and bell.
comparing the circumferential length of the centroid of the FIG. 2 Typical Bell-and-Spigot Gasket Joint Detail
relaxed gasket with the circumferential length of the centroid
of the compressed or stretched gasket after installation in the
out leakage. The angle defined by the joint openings given in
bell or on the spigot.
Fig. 2 is the angle between the axis of the two joined pipes.
(4) Each gasket shall be manufactured to provide the
7.2.1 Joints intended for use of pressures greater than 250
volume of elastomer required by the pipe manufacturer’s joint
psi may have lower allowable angular deflections than those
design, with a tolerance of 61 % for gaskets of 1.0-in.
given in Fig. 2 by manufacturer purchaser agreement. The
(25-mm) diameter and larger. The allowable percentage toler-
joints shall be tested at the manufacturers maximum allowed
ance shall vary linearly between 63 % and 61 % for gasket
angular deflection.
diameters between 0.5 and 1.0 in. (13 and 25 mm).
7.2.2 Determine the joint opening by scribing a circumfer-
6.3.2 The tolerances permitted in the construction of the
ential index mark on the outside of the pipe a sufficient distance
joint shall be those stated in the pipe manufacturer’s design as
from the spigot end to be visible when the pipe is joined.
approved.
Measure the maximum and minimum distance from the end of
6.3.3 Drawings—The manufacturer shall furnish drawings
the bell to the mark. The difference equals the joint opening.
of the joint and gasket, including dimensions and tolerances, if
Fig. 2 illustrates a typical joint in closed and deflected positions
requested by the purchaser.
and the index mark.
7. Laboratory Performance Requirements NOTE 5—This test is a laboratory performance test of joint integrity and
is not indicative of allowable angular deflections in field installations. In
7.1 General: actual installations, deflections greater than the manufacturer’s recom-
7.1.1 The gasket shall be the sole element depended upon to mended maximum should be avoided, and elbows, bends, or special
make the joint leakproof. The assembled joints shall pass the fittings should be used in such cases.
performance tests listed in this section. The tests shall be 7.3 Pipes in Laterally Offset Position (Shear Loading)—
performed with components selected to provide minimum Using a pipe and joint system as described in 7.1.2, the test
compression in the gasket. The internal hydrostatic pressures sections shall be deflected while the pipe units are in a
required in 7.2 and 7.3 shall be two times the rated pressure, if horizontal position, as shown in Fig. 3, by applying a perpen-
the pipe is manufactured for pressure service, or 29 psi (200 dicular load. The load shall be 100 lb/in. (17.5 kN/m) in
kPa), if the pipe is manufactured for nonpressure service. diameter. The load shall be uniformly applied over an arc of not
7.1.2 Laboratory hydrostatic pressure tests on joints shall be more than 120° along a longitudinal distance equal to one pipe
made on an assembly of two sections of pipe properly diameter or 12 in. (300 mm), whichever is the smaller, at the
connected in accordance with the joint design. Suitable bulk- unsupported spigot end of the pipe immediately adjacent to the
heads may be provided within the pipe adjacent to and on bell of the assembled joint. The pipe in the test shall be
either side of the joint, or the outer ends of the two jointed pipe supported on adequate blocks placed immediately behind or on
sections may be bulkheaded. Restraints may be provided at the the bells, as indicated in Fig. 3. Bands may be required to
joint to resist transverse thrust. No coatings, fillings, or secure the pipe to the blocks. There shall be no leakage when
packings shall be placed prior to the hydrostatic tests. the appropriate internal hydrostatic test pressure is applied for
7.2 Pipes in Angularly Deflected Position—Using a pipe 10 min after application of the load.
and joint system as described in 7.1.2, the test sections shall be 7.4 Vacuum or External Pressure Test—The assembled joint
deflected angularly, as shown in Fig. 2, and subjected to the shall withstand an external pressure of 11.6-psi (80-kPa) gage
appropriate internal hydrostatic test pressure for 10 min with- or an internal vacuum of −11.6-psi (−80-kPa) gage while in the

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D4161 − 14 (2019)

NOTE 1—The load shall be applied perpendicular to the axis of the pipe. It may be applied vertically, as shown in this figure, or at any other
circumferential orientation.
FIG. 3 Shear Loading-Test Setup

angularly deflected position, as in 7.2, and in the laterally offset 8. Retesting


position, as in 7.3. Allow the pressure to stabilize for 30 min, 8.1 If any failure occurs during performance of the tests
then seal off for a minimum of 10 min. The maximum specified in Section 7, the joint may be retested to establish
permissible pressure increase inside of the pipe during the conformity in accordance with agreement between the pur-
seal-off period shall be 0.1 psi (0.7 kPa). Some grades of pipe chaser and the manufacturer.
may not have the capability in the pipe wall of withstanding the
above vacuum or external pressure. In such cases, the joint 9. Keywords
design may be considered as meeting these criteria if a pipe and 9.1 angular deflection; bell and spigot; coupling; elasto-
joint system, incorporating a geometrically identical joint and meric seals; flexible gasket; glass-fiber-reinforced; pipe joints;
heavier-walled pipe, meets the criteria satisfactorily. specification; thermosetting resin

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standards since the last issue
(D4161–14) that may impact the use of this standard.

(1) Reapproved without changes.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

Copyright by ASTM Int'l (all rights reserved); Sat Jun 20 15:18:01 EDT 2020
4
Downloaded/printed by
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4167 − 15

Standard Specification for


Fiber-Reinforced Plastic Fans and Blowers1
This standard is issued under the fixed designation D4167; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This specification covers centrifugal and axial fans and 2.1 ASTM Standards:2
blowers with airstream components fabricated of fiber- C582 Specification for Contact-Molded Reinforced Thermo-
reinforced thermoset plastics (FRP) for corrosion resistance. It setting Plastic (RTP) Laminates for Corrosion-Resistant
is acceptable for internal structures to include encapsulated Equipment
metal fastening devices, hubs, and shafts. D883 Terminology Relating to Plastics
D2563 Practice for Classifying Visual Defects in Glass-
1.2 Reinforcing materials other than fibrous glass are ac- Reinforced Plastic Laminate Parts
ceptable for use in the fabrication, provided the fans and 2.2 Other Standards:
blowers produced meet all the requirements of this specifica- AMCA 99 Standards Handbook3
tion. AMCA Fan and Air System Applications Handbook
1.3 The term “fans” as used in this specification includes (AMCA 200, 201, 202, 203)3
fans and blowers, both centrifugal and axial. AMCA Bulletin 210 Laboratory Methods of Testing Fans for
Certified Aerodynamic Performance Rating3
1.4 The purpose of this specification is to provide users, AMCA 300 Reverberant Room Method for Sound Testing of
system designers, specifiers, and manufacturers of FRP fans Fans3
with minimum standards for fan construction and a common AMCA 301 Methods for Calculating Fan Sound Ratings
basis for determining safe operating speeds. from Laboratory Test Data3
1.5 The values stated in inch-pound units are to be regarded ACGIH Industrial Ventilation: A Manual of Recommended
as the standard. The values given in parentheses are provided Practice4
for information only. NFPA 91 Standard for Exhaust Systems for Air Conveying
of Vapors, Gases, Mists, and Particulate Solids5
NOTE 1—There is no known ISO equivalent to this standard.
NOTE 2—Appendix X2 contains a list of documents potentially of 3. Terminology
interest to designers of fan systems.
3.1 Definitions—The definitions of terms used in this speci-
1.6 This standard does not purport to address all of the fication are the same as those found in Terminology D883.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4. Construction of Fan Housings
priate safety, health, and environmental practices and deter- 4.1 Laminate Construction shall conform to Specification
mine the applicability of regulatory limitations prior to use. C582. The same resin shall be used throughout a housing
1.7 This international standard was developed in accor- unless the user and manufacturer agree to use a different resin
dance with internationally recognized principles on standard- for the inner surface and interior layer than for the structural
ization established in the Decision on Principles for the layer.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
1 3
This specification is under the jurisdiction of ASTM Committee D20 on Available from Air Movement and Control Association International, 30 West
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced University Dr., Arlington Heights, IL 60004, http://www.amca.org.
4
Plastic Piping Systems and Chemical Equipment. Available from American Conference of Governmental Industrial Hygienists
Current edition approved Dec. 1, 2015. Published January 2016. Originally (ACGIH), 1330 Kemper Meadow Dr., Cincinnati, OH 45240, http://www.acgih.org.
5
approved in 1982. Last previous edition approved in 2007 as D4167 –97(2007). Available from National Fire Protection Association (NFPA), 1 Batterymarch
DOI: 10.1520/D4167-15. Park, Quincy, MA 02269, http://www.nfpa.org.

*A Summary of Changes section appears at the end of this standard


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D4167 − 15
4.1.1 The inner surface exposed to the chemical environ- 5.3 Metal hubs, fasteners, and shafts shall be made of
ment shall be a resin-rich layer 0.010 to 0.020 in. (0.25 to 0.5 material at least as corrosion-resistant to the specified corrosive
mm) thick reinforced with a suitable chemical-resistant glass- environment as is the laminate construction, or be encapsulated
fiber surface mat or with an organic-fiber surface mat. with a laminate reinforced with at least two layers of 11⁄2 oz/ft2
4.1.2 The inner surface layer shall be followed with an (45.7 g/m2) chopped-strand mat with the same surface finish
interior layer composed of resin reinforced only with non- that is used in the laminate.
continuous glass-fiber strands applied in a minimum of two
5.4 Shafts not made of corrosion-resistant alloy shall be
plies of chopped-strand mat equivalent to a total of 3 oz/ft2
protected by a sleeve of FRP extending out through the fan
(0.92 kg/m2). As an alternative, a minimum of two passes of
housing a minimum of 0.4 in. (10 mm) (see Section 7).
chopped roving of minimum length of 0.5 in. (13 mm) to a
maximum length of 2.0 in. (50.8 mm) shall be applied 5.5 Additives that obscure visual inspection shall be used
uniformly to an equivalent weight of 3 oz/ft2 (0.92 kg/m2). only in the final surface coat(s) for the purpose of enhancing
Each ply of mat or pass of chopped roving shall be well rolled corrosion resistance or preventing the buildup of static
prior to the application of additional reinforcement. The electricity, or both.
combined thickness of the inner surface and interior layer shall
5.6 Acceptable surface treatments include the following:
not be less than 0.10 in. (2.5 mm).
resin coating without reinforcement; resin coating with
4.1.3 The structural layer comprises the balance of the
reinforcement, such as glass flakes, graphite, or surface veil; or
housing laminate.
resin coating reinforced with other materials agreed upon by
NOTE 3—Although fan housings are subject to vibrational stresses, the the fabricator and user. Resins that exhibit air inhibition shall
design considerations regarding construction of the laminate are similar to be paraffinated for use in the final coat.
those used for static FRP process system components.
4.2 Fastening Devices, such as bolts, shall be made of 6. Spark-Resistant Construction
material the user and manufacturer agree is at least as
corrosion-resistant to the specified corrosive environment as is 6.1 Fans built in accordance with this specification will be
the laminate construction, or shall be embedded in a laminate spark-resistant, providing the outer surface of the wheel and
in such a way that the laminate covering the device is the inner surface of the housing are rendered electrostatically
reinforced with at least two layers of 11⁄2 oz/ft2 (4.57 g/m2) conductive (6.1.1). To be considered acceptably conductive,
chopped-strand glass mat and with the same surface finish used the surface resistivity between all points of the airstream
in the housing laminate. surface and ground shall be no more than 1 MΩ when tested
with an insulation resistance tester.6
4.3 Gasketing, used where housings are constructed so that 6.1.1 The user shall electrically ground all fan parts in order
sections or inspection panels are removable, shall be of to maintain spark resistance.
elastomeric material sufficiently resilient to seal the sections.
The gasketing shall be of material the user and manufacturer 7. Shaft-Hole Closures
agree is suitable for the corrosive environment.
7.1 It is possible that gas will flow either into or out of the
4.4 Housings, shall have minimum inside corner radii of 0.6
shaft holes of the fan housing, depending on pressure distribu-
in. (15 mm).
tion in the system and type of fan wheel. The shaft-hole closure
4.5 Suitable housing construction design shall be deter- shall be one of the following types, as specified by the user:
mined by running the fan at maximum-rated speed with the
inlet blocked tight and with an open outlet. The design will be NOTE 4—The user needs to determine the importance of restricting gas
flow through the shaft holes before selecting the type of closure required.
deemed acceptable if the test does not cause any part of the
housing to move more than a distance equal to 1⁄2 of 1 % of the 7.1.1 Shaft encapsulated with an FRP sleeve to at least 0.4
wheel diameter from the position with the fan not running. in. (10 mm) outside the fan housing, with the shaft hole no
4.6 Where the user determines that system design is such larger than the sleeve diameter plus 0.08 in. (2 mm). (An
that it is possible that liquid will collect in housings, the fan acceptable alternative is to mount a membrane onto the
housings shall be specified with drains. housing to maintain the 0.08-in. maximum space).
7.1.2 Lubricated lip seals or stuffing boxes must ride on
5. Construction of Fan Wheels smooth metal shafts or shaft sleeves, necessitating the use of
shafts or shaft sleeves made of material selected to withstand
5.1 Where a history of service acceptable to the manufac- the corrosive environment.
turer and the user shows that resin systems and joint designs
selected for use in the construction of fan wheels are
acceptable, destruction tests need not be run. Where acceptable
6
history does not exist, destruction tests shall be performed in The sole source of supply of the apparatus known to the committee at this time
is the Danaher Corporation, 2200 Pennsylvania Avenue, NW, Suite 800W,
accordance with Section 10. Washington, DC 20037, to Everett, Washington. Their testers are sold by many
companies and can be located on their web site: www.danaher.com. If you are aware
5.2 Defects visible in fan wheels shall be limited to those
of alternative suppliers, please provide this information to ASTM International
shown in Table 1 (taken from Practice D2563 and modified for Headquarters. Your comments will receive careful consideration at a meeting of the
specific use with fan wheels). responsible technical committee,1 which you may attend.

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TABLE 1 Allowable Defects in the Construction of FRP Fan Wheels (adapted from Practice D2563)
Type of Defect Definition Degree Allowed

Chip A small piece broken off an edge or surface None permitted


Crack An actual separation of the laminate, visible on opposite surfaces, and extending through the None permitted
thickness
Crack, surface Crack existing only on the surface of the laminate None permitted
Crazing Fine cracks at or under the surface of a laminate None permitted
Delamination, edge Separation of the layers of material at the edge of a laminate None permitted
Delamination, internal Separation of the layers of material in a laminate None permitted
Dry spot Area of incomplete surface film where the reinforcement has not been wetted with resin 0.4-in. (10-mm) diameter and
1/ft2 (12/m2)
Foreign inclusion Metallic particles included in a laminate that are foreign to its composition 0.04-in. (1-mm) diameter and
(metallic) 1/ft2 (12/m2)
Foreign inclusion Nonmetallic particles of substance included in a laminate that seem foreign to its composition 0.04-in. (1-mm) diameter and
(nonmetallic) 1/ft2 (12/m2)
Fracture Rupture of laminate surface without complete penetration None permitted
Air bubble (void) Air entrapment within and between the plies of reinforcement, usually spherical in shape 0.04-in. (1-mm) diameter and
200/ft2 (2000/m2)
Blister Rounded elevation of the surface of a laminate, with boundaries more or less None permitted
sharply defined, somewhat resembling in shape a blister on the human skin
Burned Showing evidence of thermal decomposition through some discoloration, distortion, or destruc- None permitted
tion of the surface of the laminate
Fish-eye Small globular mass that has not blended completely into the surrounding material and is par- None permitted
ticularly evident in a transparent or translucent material
Lack of fillout An area, occurring usually at the edge of a laminated plastic, where the reinforcement has not None permitted
been wetted with resin
Orange peel Uneven surface somewhat resembling an orange peel None permitted
Pimple Small, sharp, or conical elevation on the surface of a laminate None permitted
Pit (pinhole) Small crater in the surface of a laminate, with its width approximately of the same order of mag- 0.02 in. (0.5 mm) and 200/ft2
nitude as its depth (2000/m2)
Porosity (pinhole) Presence of numerous visible pits (pinholes) None permitted
Pre-gel An unintentional extra layer of cured resin on part of the surface of the laminate. (This condition None permitted
does not cover gel coats.)
Resin pocket An apparent accumulation of excess resin in a small localized area within the laminate 0.125 by 0.250-in. (3 by 6
mm) and 1/ft2 (12/m2)
Resin-rich edge Insufficient reinforcing material at the edge of molded laminate None permitted
Shrink mark (sink) Depression in the surface of a molded laminate where it has retracted from the mold None permitted
Wash Area where the reinforcement of molded plastic has moved inadvertently during closure of the None permitted
mold resulting in resin-rich areas
Wormhole Elongated air entrapment that is either on or near the surface of a laminate and potentially cov- None permitted
ered by a thin film of cured resin
Wrinkles In a laminate, an imperfection that has the appearance of a wave molded into one or more plies None permitted
of fabric or other reinforcement material
Scratch Shallow mark groove, furrow, or channel caused by improper handling or storage None permitted
Short In a laminate, an incompletely filled out condition None permitted
Note—It is possible that this will be evident either through an absence of surface film in some
areas, or as lighter unfused particles of material showing through a covering surface film, possi-
bly accompanied by thin-skinned blisters.

8. Balancing and Test Running 8.2 Balance correction shall be accomplished by one or
8.1 The fan manufacturer shall perform one of the following more of the following methods:
methods of checking balance of wheel/shaft assemblies and 8.2.1 Removal of FRP built onto the wheel for this purpose.
complete fans: 8.2.2 Addition of FRP so that it becomes homogeneous with
8.1.1 Dynamically balance the wheel/shaft assembly as a the wheel by proper surface preparation (normally by grinding
unit in accordance with ANSI S2.19, Grade 6.3. For example: away the surface to expose structural fibers) and laminating the
At 1000 rpm the maximum total residual unbalance of both necessary weight on so that it blends into the wheel without
planes is not to exceed 0.002 lb·in./lb (0.05 g·mm/g) of the total abrupt changes of contour.
assembly weight. 8.2.3 Application of metal weights, where the weights and
8.1.2 Run the assembled fan and balance in such a way that necessary fasteners are compatible with the corrosive environ-
the peak-to-peak vibration measured horizontally at the pillow ment.
blocks perpendicular to the axis of the shaft will not exceed the
8.2.4 Application of metal weights and fasteners covered by
following:
at least two layers of 11⁄2 oz/ft2 (45.7 g/m2) chopped-strand
8.1.2.1 2.5 mils (0.06 mm) up to 600 rpm,
glass mat with the same surface finish that is used in the
8.1.2.2 2.0 mils (0.05 mm) up to 900 rpm,
laminate.
8.1.2.3 1.5 mils (0.04 mm) up to 1200 rpm,
8.1.2.4 1.0 mils (0.025 mm) up to 1800 rpm, 8.3 In all cases, FRP exposed as in 8.2.1 or applied as in
8.1.2.5 0.6 mils (0.015 mm) up to 3000 rpm, and 8.2.2 and 8.2.4, shall be given the same surface treatment as
8.1.2.6 0.5 mils (0.013 mm) above 3000 rpm. was used in constructing the wheel.

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9. Fan Aerodynamic Rating and Testing 10.1.2 Destruction speed is defined as the speed at which the
9.1 Fans shall be tested and rated in accordance with AMCA test is discontinued because of complete or imminent failure.
210, ANSI/ASHRAE 51, Laboratory Methods of Testing Fans 10.1.3 The failure speed so determined is established in
for Certified Aerodynamic Performance Rating. reference to the specific size, construction, and resin system
used in the test wheel at 68°F (20°C).
10.1.4 The safe 68°F (20°C) operating speed is a maximum
10. Safe Operating Speed
of 58 % of the failure speed. (This is one-third failure stress, or
10.1 The variables of cross sections, reinforcement content, a safety factor of 3:1 on stress.)
resin characteristics, and bonding strength limit the applicabil- 10.1.5 The safe operating speed at other temperatures is the
ity of methods such as the use of strain gages, the use of brittle speed at 68°F (20°C) multiplied by the square root of the ratio
lacquer, and the calculation of wheel stresses. Where a history of the flexural modulus at the elevated temperature to the
of service, acceptable to the manufacturer and user, shows that flexural modulus at 68°F (20°C).
resin systems and joint designs selected for use in the construc-
tion of fan wheels are acceptable, destruction tests need not be 11. Nameplates
run. Where a history of service, acceptable to the manufacturer 11.1 Nameplates shall be permanently fastened to the fans
and user, is not available, representative wheels shall be tested and shall carry the following information:
to destruction to determine actual failure speeds (see 5.1). 11.1.1 Identification of the fan manufacturer,
Application of a safety factor defines safe operating speed (see 11.1.2 Serial or other identifying number, and
10.1.4). 11.1.3 Fan size and model.
10.1.1 The test method is performed by running the wheel at
slowly increasing speed until failure occurs. Because the major 12. Keywords
destructive stresses are centrifugal, and not related to fan 12.1 axial blowers; centrifugal blowers; fan balancing; fan
horsepower, tests can be run in a vacuum for the sake of housing; fan wheel; fiber-reinforced plastic fans (FRP fans);
convenience. FRP; safe operating speed

APPENDIXES

(Nonmandatory Information)

X1. NFPA REQUIREMENTS

X1.1 Some fans are required to conform with NFPA 91, nature of the fan system. This standard should be studied prior
Standard for Exhaust Systems for Air Conveying of Vapors, to the design of reinforced-plastic duct systems.
Gases, Mists, and Particulate Solids, depending upon the

X2. DOCUMENTS OF POSSIBLE INTEREST TO DESIGNERS OF FAN SYSTEMS

X2.1 Air Movement and Control Association (AMCA):3 X2.1.4 Bulletin 99, Standards Handbook.
X2.1.1 Bulletin 300, Reverberant Room Method for Sound X2.1.4.1 Includes definitions of, and standard terminology
Testing of Fans for, rotation and discharge, drive arrangements, and motor
X2.1.2 Bulletin 301, Methods for Calculating Fan Sound position.
Ratings from Laboratory Test Data
X2.2 ACGIH Publicastions. American Conference of Gov-
X2.1.3 Fan and Air System Applications Handbook (AMCA
ernment Industrial Hygienists
200, 201, 202, 203)
X2.1.3.1 Section One defines the usually unmeasurable X2.2.1 Industrial Ventilation—A Manual of Recommended
adverse effects of fan inlet and outlet connections that are other Practice
than those used for rating purposes and which should be
included in the system designer’s calculations of fan pressure.

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D4167 − 15

X3. GAS DENSITY AT FAN INLET

X3.1 The system designer should note that fans are rated necessary to make density corrections for fan selection pur-
according to fan inlet density. (See AMCA 210 and AMCA poses. Gas-stream density may vary because of temperature or
201). When actual fan inlet density varies from that used for system resistance on the inlet side of the fan (the normal
standard ratings [usually 0.075 lb/ft3 (1.20 kg/m3)], it is situation for FRP fans) and because of chemical composition.

X4. RESIN SELECTION FOR CORROSION RESISTANCE

X4.1 The selection of resin for corrosion resistance is scrubbed by fumes (perhaps with entrapped or condensed
similar to that for other corrosion-resistant devices, but it liquid droplets).
should be recognized that the gas-stream surfaces of fans are

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D4167 – 97(2007)) that may impact the use of this standard. (December 1, 2015)

(1) Updated standards and other referenced documents. (4) Eliminated mandatory Note 4 and made it into actual
(2) Eliminated obsolete documents. standard text language.
(3) Eliminated non-mandatory language.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4226 − 19 An American National Standard

Standard Test Methods for


Impact Resistance of Rigid Poly(Vinyl Chloride) (PVC)
Building Products1
This standard is issued under the fixed designation D4226; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 These test methods cover the determination of the 2.1 ASTM Standards:2
energy required to crack or break rigid poly(vinyl chloride) D618 Practice for Conditioning Plastics for Testing
(PVC) plastic sheeting and profile flat sections used in building D883 Terminology Relating to Plastics
products, as well as extruded or molded test samples, under D5947 Test Methods for Physical Dimensions of Solid
specified conditions of impact from a freefalling standard Plastics Specimens
weight striking an impactor with either of two configurations in E178 Practice for Dealing With Outlying Observations
contact with the specimen. E456 Terminology Relating to Quality and Statistics
1.2 Two test procedures are included: E691 Practice for Conducting an Interlaboratory Study to
1.2.1 Procedure A, used to determine minimum impact Determine the Precision of a Test Method
energy required to cause failure (hole, crack, split, shatter, or E2935 Practice for Conducting Equivalence Testing in
tear). Laboratory Applications
1.2.2 Procedure B, used to determine minimum impact
3. Terminology
energy required to cause brittle failure.
3.1 Definitions—Definitions are in accordance with Termi-
1.3 The values stated in inch-pound units are to be regarded
nology D883, unless otherwise specified. For terms relating to
as standard. The values given in parentheses are mathematical
precision and bias and associated issues, the terms used in this
conversions to SI units that are provided for information only
standard are defined in accordance with E456.
and are not considered standard.
3.2 Definitions of Terms Specific to This Standard:
NOTE 1—There is no known ISO equivalent to this standard.
3.2.1 failure (of test specimen, as related to impact
1.4 The text of this standard references notes and footnotes resistance)—signified by the presence of a punched hole,
which provide explanatory material. These notes and footnotes crack, split, shatter, or tear that was created in the target area by
(excluding, those in tables in figures) shall not be considered as the impact of the falling weight (see Fig. 1).
requirements of this standard.
3.2.2 ductile failure (ductile break, as related to impact
1.5 This standard does not purport to address all of the resistance)—a tear or split having an angle greater than 0° at
safety concerns, if any, associated with its use. It is the the tip and extending through the entire thickness of the
responsibility of the user of this standard to establish appro- specimen such that light is directly visible through the tear or
priate safety, health, and environmental practices and deter- split (see Fig. 1).
mine the applicability of regulatory limitations prior to use.
3.2.3 brittle failure (brittle break, as related to impact
Specific precautionary statements are given in Section 8.
resistance)—a punched hole, split, or shatter where a piece of
1.6 This international standard was developed in accor-
the specimen separates from the main part of the specimen or
dance with internationally recognized principles on standard-
a crack that has a 0° angle at the tip as viewed by the naked eye
ization established in the Decision on Principles for the
(see Fig. 1).
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical 3.2.4 mean failure height (Procedure A)—the height from
Barriers to Trade (TBT) Committee. which the falling weight will cause 50 % of the specimens to
fail.
1
These test methods are under the jurisdiction of ASTM Committee D20 on
Plastics and are the direct responsibility of Subcommittee D20.24 on Plastic
2
Building Products. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2019. Published December 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1983. Last previous edition approved in 2016 as D4226 - 16. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4226-19. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D4226 − 19

FIG. 1 Types of Failures of the Specimen

3.2.5 mean failure energy (mean impact resistance), ( Pro- 3.2.10 outlier—an observation that appears to deviate mark-
cedure A)—energy required to produce 50 % failures; the edly from other members of the sample in which it occurs.
product of the weight and mean failure height.
4. Summary of Test Method
3.2.6 normalized mean failure energy (normalized mean
impact resistance)—the mean failure energy per unit (average) 4.1 Flat sections of a PVC building profile are tested by
specimen thickness (Procedure A). means of an impactor driven by a falling weight to determine
impact resistance of the profile. If necessary, cut the profile into
3.2.7 mean brittle failure height—the height from which the
smaller sections or coupons in order to properly position the
falling weight will cause 50 % brittle failures in specimens
profile on the tester support plate.
(Procedure B).
3.2.8 mean brittle failure energy (mean energy of ductile- 4.2 Procedure A establishes the height from which a stan-
to-brittle transition), (Procedure B)—energy required to pro- dard falling 8-lb (3.6-kg) weight will cause 50 % of the
duce 50 % brittle failures; the product of the weight and mean specimens to fail.
brittle failure height. 4.3 Procedure B establishes the height from which a stan-
3.2.9 normalized mean brittle failure energy (normalized dard falling 8-lb (3.6-kg) weight will cause 50 % of the
mean energy of ductile-to-brittle transition), (Procedure B)— specimens to fail in a brittle mode.
the mean brittle failure energy per unit (average) specimen 4.4 Both procedures employ either of two configurations of
thickness. impactor heads resting on the specimen. The specimen lays flat

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D4226 − 19

FIG. 2 Impact Tester

on a stand that has a 0.64-in. (16.3-mm) hole. The falling thickness and product toughness as well as abstract factors,
weight impacts on the impactor head tending to drive it through such as the anticipated mode of failure in a specific application.
the specimen into the hole of the stand. The geometric uniqueness of the impactor head configurations
4.5 The technique used to find 50 % failure level in both prevents any comparison or correlation of testing results on
procedures is commonly called the Bruceton Staircase Method samples tested with differing impactor head configurations. In
or Up-and-Down Method. Testing is concentrated near the general, the conical impactor, C.125, is useful to ensure failure
mean, reducing the number of specimens required to obtain a of thicker specimens where the H.25 impactor caused no
reasonably precise estimate. failure.
NOTE 2—Equivalent surface conditions are more likely to occur when
specimens are prepared by compression molding or extrusion than by
5. Significance and Use
injection molding.
5.1 The impact strength values obtained on the flat sections 5.5 When comparing different samples tested with the same
of a building product profile are relevant only to the flat section impactor head configuration, impact resistance shall be permit-
that has been tested and these values do not necessarily indicate ted to be normalized for average specimen thickness over a
the impact resistance of the whole product, which is affected by reasonably broad range (for example, 1 to 3 mm).3 However,
the configuration of the profile (that is, corners, ribs, etc). this should only be done when the surface conditions listed in
5.2 Constant weight and variable height, employed in these 6.1 are essentially equivalent.
test methods, allow the velocity of impact to vary and,
therefore, by Procedure B, can determine the energy of 6. Interferences
ductile-to-brittle transition, which cannot be determined if a 6.1 The results obtained are greatly influenced by the
variable weight is dropped from a constant height. quality of the test specimens. Cracks usually start at the surface
5.3 These test procedures have been found to be useful in tension; the surface opposite the one that is struck by the
elements in rigid poly(vinyl chloride) (PVC) building product impactor head. The composition of this surface layer and the
characterization. Compound qualification, finished product degree of orientation introduced during the formation of the
quality control, environmental and weatherability research and specimen are very important variables. Flaws in this surface
development studies, and fabrication tolerance prediction con-
stitute useful applications.
3
O.R. Weaver, “Using Attributes to Measure a Continuous Variable in Impact
5.4 Choice of the specific impactor head configuration used Testing Plastic Bottles,” Materials Research & Standards, MR & S, Vol. 6, No. 6,
is related to a variety of product attributes, such as specimen June, 1996, pp. 285-291.

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D4226 − 19

FIG. 3 Impactor Head Configuration H.25 Specimen Support Detail

will also affect results. Because of these factors, sometimes 7.1.2.2 Impactor H.25 shall be constructed, as is shown in
additional information about the sample is achieved by testing Fig. 3, of tough, hardened (Rockwell C50-55) scratch resistant
the sample from a variety of locations in a product or testing steel. It should have a 0.25-in. (6.35-mm) radius hemispherical
from both sides of a flat section. tip (see Fig. 3 and Fig. 4).
6.2 Samples must not collapse into the hole in the specimen 7.1.2.3 The surface of the impactor head shall be polished
support plate when driven by the impactor. Sample collapse free of nicks, scratches, or other surface irregularities.
into the hole during the impact test affects impact results. 7.2 Supporting Base—In order to minimize the energy
6.3 When resting on the support plate and in contact with absorption, compression, and deflection of the support the
the impactor the specimen must lie flat. Bowed samples will tester shall be firmly fixed to a dense, solid, block or base.
affect test results. 7.2.1 The main body of said block or base shall have
maximum dimensions of 16 in. (40 cm) (h) × 30 in. (75 cm)
7. Apparatus (w) × 30 in. (75 cm) (d) and shall have a minimum weight of
375 lb (171 kg). This block shall be placed at a height that
7.1 Testing Machine—The apparatus shall be constructed facilitates equipment usage. It is not necessary to bolt blocks or
essentially as shown in Fig. 2 and Fig. 3 and shall consist of the bases of this weight to the floor.
following: suitable base to withstand the impact shock; steel-
rod impact weight weighing 8 6 0.2 lb (3.6 6 0.1 kg); NOTE 3—The required block weight and dimensions conform to
commercially available butcher block type tables.
hardened steel impactors as specified in 7.1.2; a slotted guide
tube 40 in. (1.0 m) in length in which the impact weights slide, 7.2.2 Alternative supporting bases or those lighter than 375
having an internal diameter sufficient so that friction does not lb (171 kg) should be bolted to a concrete floor. Mean failure
reduce the weight velocity, and having graduations in inch- energy comparisons shall be made between these alternative
pound (newton-meter) increments, or multiples thereof. A supports and one where the tester is bolted directly to the
bracket is used to hold the tube in a vertical position by concrete floor. If mean failure energy differences between the
attaching it to the base and also to hold the hand knob, which concrete floor and the alternative support are found statistically
is a pivot-arm alignment for the impactor, about 2 in. (50 mm) nonsignificant, use of the lighter support shall be allowed.
under the tube. The top edge of the opening in the specimen 7.2.3 If the weight of the butcher block that was originally
support plate should be rounded to a 0.031-in. (0.8-mm) radius. 375 lb (171 kg) or greater decreases with time to less than 375
Fig. 3 shows the specimen support configuration for this test. lb (171 kg), increase the block weight to a minimum of 375 lb
7.1.1 The tester shall be mounted so that the axis of the tube (171 kg) by adding a suitable amount of weight to the bottom
is plumb when measured with a spirit level at least 1 ft (300 of the table. The weight shall be tightly affixed and in direct
mm) in length. contact with the bottom of the table and not cause any
7.1.2 Impactor Configurations: vibrations during the impact test.
7.1.2.1 Impactor C.125 shall be constructed, as is shown in NOTE 4—The weight of the butcher block can decrease over time, for
Fig. 4, of tough, hardened (Rockwell C50-55), scratch resistant instance, due to drying.
steel. It should have a conical (40°) configuration and 0.125-in. 7.2.4 Use of rubber mats either under the tester or the
(3.18-mm) radius hemispherical tip. supporting base is prohibited.

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D4226 − 19

FIG. 4 Impactor Head Configuration C.125

7.3 Micrometer, for measurement of specimen thickness. It plate is related to sample thickness and for thicker samples it’s possible to
should be accurate to 1 % of the average thickness of use smaller samples.
specimens used. See Test Method D5947 for suitable microm- 10.2 When the approximate mean failure height for a given
eters. sample is known, 20 specimens usually yield sufficiently
precise results. If the mean failure height cannot be
8. Safety Precautions approximated, six or more specimens shall be used to deter-
8.1 Shield devices to protect personnel. mine the appropriate starting point of the test.
8.2 A tube can contain the impactor head if it rebounds after NOTE 6—Specimen quantity, as small as five, often yields sufficiently
striking a specimen, or the impactor head may be drilled for a reliable estimates of the mean failure height. However, the estimated
cotterpin to prevent rebound. The cotterpin must be located standard deviation will be relatively large.4
well above the penetration depth of the impactor head. 11. Conditioning
9. Sampling 11.1 Unless otherwise specified, condition the test speci-
9.1 Sample in a statistically acceptable manner. The samples mens at 73.4 6 3.6°F (23 6 2°C) and 50 6 10 % relative
shall be representative of the lot under study. humidity for not less than 40 h prior to test in accordance with
Procedure A of Methods D618. In cases of disagreement, the
10. Test Specimen tolerance shall be 61.8°F (61°C) and 65 % relative humidity.
10.1 Test specimens must lay flat on the specimen support 11.2 Quality Control Tests—Condition the test specimens at
plate during testing, cover the hole in the support plate, and be 73.4 6 3.6°F (23 6 2°C) for 4 h in air.
of sufficient size to prevent their collapse into the hole of the
specimen support plate during the impact test. The specimens 12. Procedure
shall be free of obvious imperfections unless they constitute 12.1 Procedure A:
variables under study.
NOTE 5—When individual coupons are used, a size of 1.5 in. by 1.5 in. 4
Brownless, K. A., Hodges J. L., Jr., and Rosenblatt, Murray, “The Up-and-
(38 mm by 38 mm) was found sufficient to avoid collapse of most Down Method with Small Samples,” American Statistical Association Journal,
specimens. Collapse of the sample into the hole of the specimen support JSTNA, Vol. 48, 1953, pp. 262-277.

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D4226 − 19
12.1.1 When testing individual specimens or coupons, mea- improper starting height and affects final results. Re-estimate
sure and record the thickness of each specimen at the antici- approximate starting height and restart the test.
pated area of impact. Average all values to determine average 12.1.12 Keep a running plot of the data. Use one symbol,
thickness. When using a single large specimen such as a strip such as “X”, to indicate a failure and a different symbol, such
of PVC siding, measure the thickness at five points uniformly as “O”, to indicate a non-failure at each height level.
down the length of PVC siding under test. Use the average of 12.1.13 For any specimen that gives a break behavior that
these five values as the average thickness. The thickness of any appears to be an outlier, the conditions of that impact shall be
individual measurement shall not vary by more than 5 % from examined. The specimen may be discarded only if a unique
the average thickness. cause for the anomaly can be found, such as an internal flaw
12.1.2 When testing individual specimens or coupons, visible in the broken specimen. Note that break behavior may
choose randomly from the sample. Determine the order of vary widely within a set of specimens. Data from specimens
testing by using a set of random numbers. that show atypical behavior shall not be discarded simply on
12.1.3 Select the proper impactor-head configuration (C.125 the basis of such behavior. Refer to Practice E178 for detailed
or H.25) specified for the test and install on the apparatus. information on how outliers shall be handled.
Adjust the guide arm so that each impactor head is visually 12.2 Procedure B:
centered and achieves the proper depth of penetration. Depth of 12.2.1 Test the specimen in the same way as described in
penetration is the distance the impactor head protrudes into the Procedure A (12.1.1 – 12.1.9).
support plate when properly seated. For the H.25 impactor this 12.2.2 If brittle failure is observed (Fig. 1) at the mean
shall be 0.48 in 6 0.04 in. (1.22 cm 6 0.10 cm) (Fig. 3) and failure height, the mean brittle failure height and mean brittle
0.69 in. 6 0.04 in. (1.75 cm 6 0.10 cm) for the C.125 impactor failure energy are the same as mean failure height and mean
(Fig. 4). failure energy for the specimen.
NOTE 7—Periodic visual inspection during testing ensures tup is 12.2.3 If ductile breaks are observed (Fig. 1), continue the
centered. test by increasing the height by increments, as described in
12.1.4 After raising the weight and impactor foot, place the Procedure A, until a brittle failure occurs.
specimen between the impactor foot and the specimen support 12.2.4 Use one symbol, such as “D”, to indicate ductile
plate making sure that it covers the hole in the specimen break and a different symbol, such as “B”, to indicate brittle
support plate. The clamping force, when clamping is used, failure at each height level.
shall be sufficient to prevent motion of the specimen. 12.2.5 At the start of a test, a continuous run of seven or
12.1.5 Place the impactor foot so that it rests on the more identical results (brittle or ductile) is indicative of an
specimen. The specimen must lie flat at this point. improper starting height and affects final results. Re-estimate
12.1.6 Raise the weight in the tube to the approximate starting height and restart the test.
failure energy value for the specific sample and release it so
that the weight drops on the impactor. If the approximate 13. Calculation
failure energy value for the sample is unknown, run a minimum 13.1 Mean Failure Height (Procedure A)—Calculate the
of six impact tests at varying energy levels to bracket the mean failure height from the test data obtained as follows:
approximate failure energy level before initiating the test series h 5 h o 1d h ~ A/N60.5! (1)
of impacts.
12.1.7 Remove the specimen and examine it to determine where:
whether it has failed. See 3.2.1 for criteria of failure. h = mean failure height, in. (mm),
12.1.8 If the first impact of the specimen results in failure, dh = increment of weight height, in. (mm),
decrease the drop height one increment. If the first impact of N = total number of failures or non-failures, whichever is
the specimen does not cause failure, increase the drop height smaller. For ease of notation, call whichever is used
one increment. Then test a second specimen or target point on “events,”
the specimen. ho = lowest height at which an event occurred, in. (mm),
12.1.9 In this manner, select the impact height for each A = ∑ki=0 in i,
successive test from the results observed with the specimen just i = 0, 1, 2 . . . k (counting index, starts at ho),
previously tested. The same target point on a specimen shall ni = number of events that occurred at hi, and
hi = ho + idh.
not be tested more than once.
12.1.10 For best results, the height increment used should In calculating h, the negative sign is used when the events
be approximately equivalent to s, the estimated standard are failures. The positive sign is used when the events are
deviation of the test for that sample. An increment from 0.5 to non-failures. See the example in Fig. 5.
2 times s is satisfactory (see 13.6). 13.2 Mean Brittle Failure Height (Procedure B)—Calculate
NOTE 8—For unknown materials it’s recommended to start with a 1.0 the mean brittle failure height using the same formula as in
in. (25.4 mm) height increment to calculate an estimated standard Procedure A. Designations of h and N are different, as follows:
deviation utilizing Eq. 4 in 13.6. If necessary adjust height increments to
meet recommendations of 12.1.10. h = mean brittle failure height in. (cm), and
12.1.11 At the start of a test, a continuous run of seven or N = total number of brittle failures or ductile breaks, which-
more identical results (failure or non-failure) is indicative of an ever is smaller.

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D4226 − 19

FIG. 5 Sample Calculations

In calculating h, the negative sign is used within the 14.1.4 Average thickness of specimen tested.
parentheses when the events are brittle failures. The positive 14.1.5 Number of test specimens (target points) employed
sign is used when the events are ductile breaks. to determine the mean failure height.
13.3 Mean Failure Energy (Procedure A)—Compute the 14.1.6 Mean failure energy (Procedure A) or mean brittle
mean failure energy as follows: failure energy (Procedure B), or both.
14.1.7 Estimated standard deviation of either the mean
MFE 5 h 3 w (2) failure energy (Procedure A) or mean brittle failure energy
where: (Procedure B) or both, if required.
MFE = mean failure energy, in.•lbf (J), 14.1.8 Normalized mean energies, when required.
h = mean failure height, in. (cm), and 14.1.9 Any departures from the specified test procedures.
w = weight, 8 lb (3.6 kg).
15. Precision and Bias
13.4 Mean Brittle Failure Energy (Procedure B)—Compute
the mean brittle failure energy as follows: 15.1 Warning—The data contained in Table 1 shall not be
rigorously applied to acceptance or rejection of material, as
MBFE 5 h 3 w (3)
those data are specific to the interlaboratory study and are not
where: representative of other lots, conditions, materials, or laborato-
MBFE = mean brittle failure energy, in.•lbf (J), ries. Users of this test method shall apply the principles
h = mean brittle failure energy, in. (cm), and outlined in Practice E691 to generate data specific to their
w = weight, 8 lb (3.6 kg). laboratory and materials or between specific laboratories.
13.5 Normalized mean failure energy (Procedure A) and 15.2 Precision, extruded lineals—An interlaboratory study
normalized mean brittle failure energy (Procedure B) are with six laboratories was conducted in which thick flat sections
calculated by dividing the mean energy by the average thick- from various rigid poly(vinyl chloride) (PVC) extruded profiles
ness. were tested with impactor-head configuration C.125.
13.6 Estimated Standard Deviation—Calculate the esti- 15.2.1 The average within-laboratory and between-
mated standard deviation from the test data as follows: laboratory coefficients of variation for Procedure A and for
Procedure B were as follows:
s 5 1.620d @@ NB 2 A 2 ! /N 2 # 1 0.029 (4)
Average V
k
Procedure Within-laboratory Between-laboratory
A 7.5 18.2
B5 (i n
i50
2
i B 6.4 21.0

where:
14. Report
V (Procedure A) = ⁄
100 S MFEaverage
14.1 The report shall include the following: V (Procedure B) = ⁄
100 S MBFEaverage
14.1.1 Complete identification of the sample tested, manu-
facturer’s code, form, principle dimensions, and previous 15.2.2 Bias—No statement of bias can be provided because
history. of the lack of a referee method for impact behavior of plastic,
14.1.2 Procedure used, either A or B, or both. which can provide a “true” or reference value.
14.1.3 Impactor head configuration used, either C.125 or 15.3 Precision, extruded siding—An interlaboratory study
H.25, or both. with nine laboratories was conducted in which four vinyl

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D4226 − 19
TABLE 1 Within-Laboratory and Between-Laboratory Variations
Materials Average Sr SR r R
Emboss A 92.292 2.206 4.880 6.178 13.665
Emboss B 71.157 3.031 4.207 8.486 11.957
Emboss C 56.956 3.452 5.704 9.666 15.970
Emboss D 61.406 2.538 4.922 7.107 13.782

siding (PVC) panels of 0.040 in. thickness were tested using 15.4 Equivalence testing on numerical data from two
Procedure A with impactor-head configuration H.25. The four sources shall be conducted in accordance with E2935.
vinyl siding panels had a variety of emboss patterns typical for
the industry. 16. Keywords
15.3.1 The within-laboratory and between-laboratory varia-
16.1 brittle failure energy; building products; failure energy;
tion from this study is found in Table 1.
falling weight; impact test
15.3.2 Bias—No statement of bias can be provided because
of the lack of a referee method for impact behavior of plastic
which can provide a “true” or reference value.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D4226 – 16) that may impact the use of this standard. (November 1, 2019)

(1) Revised Referenced Documents, Terminology, and Preci- (5) Revised Fig. 5 to correct syntax in equations, added
sion and Bias sections consistent with D20 policy on statistical calculations for MFE and MBFE.
terminology (April 2019), revisions made to 2.1, 3.1, and (6) Corrected equation syntax in 13.6.
Section 15. Removed reference to D3679 as it is not used in (7) Clarified reporting requirements in 14.1.7.
standard. (8) Added warning statement in 15.1 as noted above in (1) of
(2) Changed size requirements for individual samples (4.1). the Summary of Changes.
(3) Added sample collapse into support table hole as potential (9) Added metric equivalences as needed.
interference (6.2).
(4) Added Note 7 recommending a starting height increment of
1 in.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
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Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4477 − 16 An American National Standard

Standard Specification for


Rigid (Unplasticized) Poly(Vinyl Chloride) (PVC) Soffit1
This standard is issued under the fixed designation D4477; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope D635 Test Method for Rate of Burning and/or Extent and
1.1 This specification establishes requirements and test Time of Burning of Plastics in a Horizontal Position
methods for the materials, dimensions, camber, impact D696 Test Method for Coefficient of Linear Thermal Expan-
strength, expansion, and appearance of extruded single-wall sion of Plastics Between −30°C and 30°C with a Vitreous
soffit manufactured from rigid (unplasticized) PVC compound. Silica Dilatometer
Methods of indicating compliance with this specification are D883 Terminology Relating to Plastics
also provided. D1600 Terminology for Abbreviated Terms Relating to Plas-
tics
1.2 The use of PVC recycled plastic in this product shall be D2244 Practice for Calculation of Color Tolerances and
in accordance with the requirements in Section 4. Color Differences from Instrumentally Measured Color
1.3 Rigid (unplasticized) poly(vinyl chloride) (PVC) siding Coordinates
is covered in Specification D3679. D2457 Test Method for Specular Gloss of Plastic Films and
1.4 Soffit produced to this specification shall be installed in Solid Plastics
accordance with Practice D4756. Reference shall also be made D3679 Specification for Rigid Poly(Vinyl Chloride) (PVC)
to the manufacturer’s installation instructions for the specific Siding
product to be installed. D3892 Practice for Packaging/Packing of Plastics
D4226 Test Methods for Impact Resistance of Rigid Poly-
NOTE 1—Information with regard to soffit maintenance shall be (Vinyl Chloride) (PVC) Building Products
obtained from the manufacturer. D4756 Practice for Installation of Rigid Poly(Vinyl Chlo-
1.5 The values stated in inch-pound units are to be regarded ride) (PVC) Siding and Soffit
as standard. The values given in parentheses are mathematical D5033 Guide for Development of ASTM Standards Relating
conversions to SI units that are provided for information only to Recycling and Use of Recycled Plastics (Withdrawn
and are not considered standard. 2007)3
1.6 The following precautionary caveat pertains to the test D5947 Test Methods for Physical Dimensions of Solid
method portion only, Section 6 of this specification. This Plastics Specimens
standard does not purport to address all of the safety concerns, E631 Terminology of Building Constructions
if any, associated with its use. It is the responsibility of the user E1753 Practice for Use of Qualitative Chemical Spot Test
of this standard to establish appropriate safety and health Kits for Detection of Lead in Dry Paint Films
practices and determine the applicability of regulatory limita-
tions prior to use. 3. Terminology
NOTE 2—There is no known ISO equivalent to this standard. 3.1 Definitions—Definitions are in accordance with Termi-
nologies D883, D1600, and E631, unless otherwise specified.
2. Referenced Documents
3.2 Definitions of Terms Specific to This Standard:
2.1 ASTM Standards:2
3.2.1 vinyl soffıt, n—a shaped material, made principally
D618 Practice for Conditioning Plastics for Testing
from rigid poly(vinyl chloride) (PVC) that is used to clad the
1
underside of a roof overhang.
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.24 on Plastic Building 3.2.2 Discussion—Any exception to a homogeneous rigid
Products. PVC compound is present in a coextruded or laminated
Current edition approved May 1, 2016. Published May 2016. Originally
approved in 1985. Last previous edition approved in 2009 as D4477 – 09. DOI: capstock.
10.1520/D4477-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.

*A Summary of Changes section appears at the end of this standard


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D4477 − 16
4. Materials and Manufacture 1, and each individual reading shall not vary more than 10
4.1 The soffit, shall be made of one or more layers of points from the average. Gloss shall be tested in accordance
poly(vinyl chloride) (PVC) compound. Any layers of materials with 6.9.
TABLE 1
other than poly (vinyl chloride) (PVC) compound shall be kept
to less than 20% by volume. Manufacturer’s Permitted difference
Specified Gloss Value from
4.2 Use rigid PVC recycled plastic, as defined in Guide Mfg. Spec. Gloss
Value
D5033 if all the requirements in the sections on Terminology Less than or equal to 35 ±8
(Section 3), on Materials and Manufacture (Section 4), and on Greater than 35 ±10
Physical Requirements (Section 5) are met by the soffit
5.7 Deflection of the soffit shall not exceed 61⁄8 in. (3.2
containing PVC recycled plastic.
mm) when installed flat in a horizontal position over a span of
4.3 The poly(vinyl chloride) soffit material, when tested in 24 in. (610 mm) without intermittent support when tested in
accordance with Test Method D635, shall not exceed an accordance with 6.11.
average extent of burn of 4 in. (100 mm), with an average time
of burn not to exceed 10 s. A minimum sample thickness of 5.8 Color—The color of the soffit shall be within the defined
0.030 in. (0.8 mm) is required. (Warning—The flammability color space parameters for the specific color agreed upon
testing data, conclusions, and recommendations of Test between the purchaser and the manufacturer. The color speci-
Method D635 relate solely to the measurement and description fied shall be uniform on the surface of the soffit panels, except
of properties for classification of the poly(vinyl chloride) soffit in the case of multi-colored wood grain panels.
material in response to flame under controlled laboratory 5.8.1 Uniformity of Color—When tested in accordance with
conditions and shall not be used for the description or appraisal 6.10, the total color change, E, between a production specimen
of the fire hazard of vinyl soffit under actual fire conditions.) and the appropriate reference specimen or agreed-upon color
coordinates shall not vary by more than 1.5, and the chromatic
4.4 The PVC compound when extruded into soffit shall
coordinates shall not change by more than 6∆a = 1.0 and6∆
maintain uniform color and be free of any visual surface or
b = 1.0.
structural changes, such as peeling, chipping, cracking, flaking,
or pitting.
6. Test Methods
4.5 PVC soffit shall not contain elemental lead (Pb) or
compounds of that material other than traces incidental to raw 6.1 General—The inspection and test procedures contained
materials or the manufacturing process. Compliance with this in this section are used to determine the conformance of
requirement shall be demonstrated by one of the methods in products to the requirements of this specification. Each pro-
6.12. ducer who represents its products as conforming to this
specification shall be permitted to use statistically based
5. Physical Requirements sampling plans that are appropriate for each manufacturing
process, but shall keep the essential records necessary to
5.1 Length and Width—The nominal length and width of the document, with a high degree of assurance, his claim that all of
soffit shall be as agreed upon between the purchaser and the the requirements of this specification have been met. Addi-
seller. The actual length shall not be less than 1⁄4 in. (6.4 mm) tional sampling and testing of the product, as agreed upon
of the nominal length and the actual width shall be within between the purchaser and manufacturer, are not precluded by
61⁄8 in. (3.2 mm) of the nominal width when measured in this section.
accordance with 6.3 and 6.4.
6.2 Conditioning and Test Conditions—Condition the test
5.2 Thickness—The minimum thickness of the soffit shall be specimen in accordance with Procedure A of Practice D618 and
0.030 in. (0.8 mm) when measured in accordance with 6.5. test under those conditions, unless otherwise specified herein.
5.3 Camber—A full length of soffit, typically 10 or 12 ft
6.3 Length—Lay the specimen on a flat surface and measure
(3.05 or 3.66 m), will not have a camber greater than 1⁄8 in. (3.2
with a steel tape. Measure the length of a soffit panel to the
mm) when measured in accordance with 6.6.
nearest 1⁄16 in. (1.6 mm) at the center, the butt edge, and the
5.4 Initial Impact Resistance—The soffit shall have a mini- bottom of the top lock. The average of the three measurements
mum impact strength of 45 in.·lbf (5.34 J) when tested in is the actual length.
accordance with 6.7.
6.4 Width—Interlock two long specimens, each at least 26
5.5 Coeffıcient of Linear Expansion—The soffit shall have a in. (660 mm) long in the normal mode for installation. Lay the
coefficient of linear expansion not greater than 4.5 by 10−5 two specimens on a flat surface. Measure to the nearest 1⁄16 in.
in./in./°F (8.1 by 10−5 mm/mm/°C) when tested in accordance (1.6 mm), the distance between the lowest butt edge of the top
with 6.8. specimen and the lowest butt edge of the bottom specimen.
5.6 Gloss—This requirement is not applicable to surface Commencing approximately 1 in. (25 mm) from one end of the
ventilated soffit. The gloss of soffit shall be uniform across the specimens, make 5 measurements at 6 in. (152 mm) intervals,
exposed face. The average of all readings for a panel deter- making sure that the measurement is made perpendicular to the
mined in 6.9.1.2 shall not differ from the manufacturer’s butt edge. Average the measurements. The average constitutes
specified gloss value more than the permitted variation in Table the exposed width of soffit.

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D4477 − 16
6.5 Thickness—Make a minimum of five equally spaced mm) apart, are set up with the provision of measuring height
measurements across the width of the soffit specimen perpen- distance at the center of the beams.
dicular to the exposed surface with a micrometer similar to that 6.11.3 Procedure—Interlock the three pieces of soffit panel
described in Test Method D5947, Method A or B, with the with ends being in line. Position the soffit unit across the
exception that the vernier reading shall be to 0.001 in. (0.0254 support beams so that the ends of the unit are equidistant from
mm). Average the measurements. The average constitutes the the outside edges of the beams. The panel center area is
thickness of the soffit. compared in height distance to the height of the support beams
6.6 Camber—Place a full length of soffit (typically 10 or 12 and any deviation is recorded.
ft (3.05 or 3.66 m), on a flat surface alongside a straightedge at 6.12 Lead Content:
least as long as the soffit specimen. Measure the maximum 6.12.1 Testing for lead content shall be conducted on
space between the edge of the soffit specimen and the straight- extruded soffit using a rhodizinate-type lead swab test kit
edge for each edge to the nearest 1⁄16 in. (1.6 mm). conforming to Practice E1753. Testing shall be performed in
6.7 Impact Resistance—Test impact resistance of soffit in accordance with the test kit manufacturer’s instructions. The
accordance with Test Methods D4226, Procedure A impactor soffit shall be deemed to comply with 4.5 if the test shows a
head configuration H.25. 4 in-lb increments (0.5 in height negative or not-detected result; that is, the test does not indicate
increments with 8 lb falling weight) shall be used. Minimum the presence of lead. The test shall be conducted separately on
sample dimensions shall be 1.5 in. by 1.5 in. Samples shall be the substrate and on any cap or film material.
tested with the normally exposed surface facing up. Condition- 6.12.2 As an alternative to the method in 6.12.1, and as a
ing time for quality control test shall be at least 1 hr. means of resolving any ambiguous results from that method, an
analytical method capable of detecting lead at least as low as
6.8 Coeffıcient of Linear Expansion—Conduct this test in 0.02 percent by sample weight shall be employed. Under this
accordance with Test Method D696. alternative, neither the substrate nor any cap or film shall
6.9 Gloss—Measure gloss using a 75° geometry glossmeter contain a concentration of lead in excess of 0.02 percent by
that meets the requirements of the Apparatus section of Test weight.
Method D2457.
6.9.1 Procedure: 7. Product Marking
6.9.1.1 Measure gloss on one piece of soffit on at least three 7.1 To aid identification of products conforming to all
widely separated points across the width of the exposed requirements of this specification, producers and distributors
surface. At least one reading shall be taken on each face of the shall include a statement of compliance in conjunction with
panel. The area to be tested must be flat. If a flat area on the their name and address on product labels, invoices, sales
exposed surface cannot be found due to the style or depth of literature, and the like. The following statement is suggested
embossing of the panel being tested, then a non-exposed area when sufficient space is available: “This product conforms to
of the panel shall be chosen in its place. Such locations shall be all the requirements established in ASTM Specification D4477,
representative of the gloss of the area that will be exposed after developed cooperatively with the industry and published by the
installation. ASTM. Full responsibility for the conformance of this product
6.9.1.2 Each reading shall be within the limits specified in to the specification is assumed by (name and address of
5.6. The average of all readings shall be used to represent the producer or distributor).”
gloss of the sample. 7.2 The following abbreviated statement is suggested when
6.9.1.3 This test method is not applicable to surface venti- available space on labels is insufficient for the full statement:
lated soffit. “Conforms to ASTM D4477, (name and address of producer or
6.10 Color Uniformity—Calculate the difference between distributor).”
the LH, aH, bH color coordinates for a production specimen to
those of either the appropriate reference specimen or the 8. Packing, Packaging, and Package Marking
agreed-upon color coordinates for that specific color product in 8.1 The soffit shall be packaged in such a manner as to
accordance with Test Method D2244. Calculate the total provide reasonable protection against damage in ordinary
difference, E, between the production specimen and the refer- handling, transportation, and storage.
ence specimen in accordance with Test Method D2244. 8.2 The provisions of Practice D3892 shall apply to this
6.11 Deflection: specification.
6.11.1 Specimen Preparation—Three pieces of soffit, 30 in.
(762 mm) long, are prepared and conditioned at room tempera- 9. Keywords
ture for 24 h. 9.1 plastic building products; plastic weatherability; re-
6.11.2 Apparatus—Two parallel supporting beams, 1⁄2 in. cycled plastics; rigid PVC soffit; weatherability color-hold
(12.7 mm) wide at the same level of elevation and 24 in. (610 guidelines

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D4477 − 16
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4495 − 16 An American National Standard

Standard Test Method for


Impact Resistance of Poly(Vinyl Chloride) (PVC) Rigid
Profiles by Means of a Falling Weight1
This standard is issued under the fixed designation D4495; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 3. Terminology
1.1 This test method covers the determination of the energy 3.1 Definitions—Definitions are in accordance with Termi-
required to crack or break rigid poly(vinyl chloride) (PVC) nology D883, unless otherwise indicated.
profile under specified conditions of impact by means of a 3.2 Definitions of Terms Specific to This Standard:
falling weight. 3.2.1 failure—the presence of a brittle failure readily visible
1.2 This test method is used either by itself or in conjunction by the naked eye, including a sharp crack, split, or shatter in
with other methods for measuring PVC product toughness. any part of the profile as a result of the impact of the falling
1.3 Because of the wide variety of profile sizes and shapes weight. Failure does not include ductile tears (where the
and the wide variety of manufacturing procedures and field surfaces at the tip of the crack have a greater than 0° angle), or
abuse, this test method does not correlate universally with all ductile breaks (hinged breaks where the cracked part remains
types of abuse. Therefore, correlations must be established as joined to the unbroken part throughout the length of the
needed. cracked part or section), (Fig. 1).
3.2.2 mean failure height—the height from which the
1.4 The text of this standard references notes and footnotes
falling weight will cause 50 % of the specimens to fail.
which provide explanatory material. These notes and footnotes
(excluding those in tables and figures) shall not be considered 3.2.3 mean failure energy—energy required to produce
as requirements of this standard. 50 % failures. The product of the weight and mean failure
height.
1.5 The values stated in inch-pound units are to be regarded
as the standard. 3.2.4 outlier—an observation that appears to deviate mark-
edly from other members of the sample in which it occurs.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 The profile is cut into lengths of at least 6 in. The test
priate safety and health practices and determine the applica-
method establishes the height from which a standard falling
bility of regulatory limitations prior to use.
weight will cause 50 % of the specimens to fail.
NOTE 1—There is no known ISO equivalent to this standard.
5. Significance and Use
2. Referenced Documents 5.1 The impact strength of PVC profiles relates to suitability
2.1 ASTM Standards:2 for service and to quality of processing. Impact tests are used
D618 Practice for Conditioning Plastics for Testing for quality-control purposes and as an indication that products
D883 Terminology Relating to Plastics can withstand handling during assembling, installation, or in
E178 Practice for Dealing With Outlying Observations service.
5.2 Results obtained by use of this test method are used in
two ways:
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics 5.2.1 As the basis for establishing impact-test requirements
and is the direct responsibility of Subcommittee D20.24 on Plastic Building in product standards, and
Products.
Current edition approved May 1, 2016. Published May 2016. Originally
5.2.2 To measure the effect of changes in materials or
approved in 1985. Last previous edition approved in 2012 as D4495 – 12. DOI: processing.
10.1520/D4495-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Apparatus
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 6.1 General—One type of impact tester is illustrated in Fig.
the ASTM website. 2.

*A Summary of Changes section appears at the end of this standard


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D4495 − 16

FIG. 1 Types of Breaks

6.2 Falling Weight, shall be cylindrical and 2 1⁄2 in. in necessary to provide a protective barrier around the specimen, particularly
diameter, with a flat-bottom surface that strikes the test for larger sizes of profile, to protect the operator from flying broken
pieces.
specimen. NOTE 4—The dropped weight may not fall freely if it is restrained by a
NOTE 2—It is suggested that the striking portion of the weight be made partial vacuum above the weight, such as can be caused by the hold and
of scratch-resistant steel to reduce damage to the striking surface. Badly release device.
scarred surfaces may affect test results. 6.3.2 Means shall be provided to hold the weight to be
6.2.1 The mass of the falling weight shall be 10 6 0.5 lb. dropped at steps of 2 in. (50 mm) for a distance of 2 to 10 ft
6.3 Drop Tube, shall be of sufficient length (approximately (600 mm to 3 m) above the flat-plate holder, to release the
12 ft (4 m)) to provide for a fall of at least 10 ft (3 m) and shall weight in a reproducible manner, and to allow the weight to fall
be mounted so that the lengthwise direction is vertical, as freely.
measured with a plumb bob or a spirit level at least 2 ft (600 6.4 Specimen Holder—The flat plate shall be used as a
mm) in length. specimen holder.
6.3.1 Care must be taken to ensure that the weight falls 6.4.1 The rigid steel flat-plate holder shall consist of a plate
freely; it must not “chatter” down the tube. approximately 8 by 12 by 1 in. (200 by 300 by 25 mm). The
NOTE 3—No particular material for the drop tube is specified. However, specimen holder shall be fastened to a concrete slab (floor).
a cold-drawn seamless steel tubing with an inside diameter of 2 5⁄8 to 2 3⁄4 Means shall be provided to center the specimens under the drop
in. (67 to 70 mm) has been found to be satisfactory. It may also be tube.

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D4495 − 16
for not less than 24 h prior to test in accordance with Procedure
A of Methods D618. In cases of disagreement, the tolerance
shall be 61.8°F (61°C) and 65 % relative humidity.
8.2 Quality-Control Tests—Condition the test specimens at
73.4 6 3.6°F (23 6 2°C) for 4 h in air.

9. Procedure
9.1 Cut the profile into samples 6 in. (152 mm) long.
9.2 Choose a specimen at random from the sample.
9.3 After raising the weight, place the specimen on the
specimen holder between two pair of snug-fitting right-angle-
slotted brackets in such a way that it rests in the most stable
position and is centered under the weight. The brackets are
used to prevent any lateral movement of the profile and any
sliding out during impact.
NOTE 6—During the round robin, it was found that choice of the side of
the profile impacted made no difference on impact resistance. Even then,
the position was defined so that it is likely that all would hit the same side.
9.4 Raise the weight in the tube to the approximate failure
height value for the specific sample and release it so that it
drops on the specimen. Height is determined as the distance
between the top surface of the profile under impact, and the
bottom surface of the falling weight.
9.5 Remove the specimen and examine it to determine
whether or not it has failed.
9.6 If the first impact of the specimen results in failure,
decrease the drop height one increment. If the first impact of
the specimen does not cause failure, increase the drop height
one increment. Then test a second specimen.
9.7 In this manner, select the impact height for each
successive test from the results observed with the specimen just
previously tested. Do not test the same target point on a
specimen more than once.
9.8 Keep a running plot of the data. See Appendix X1. Use
FIG. 2 Testing Apparatus
one symbol, such as “X” to indicate a failure and a different
symbol such as “O” to indicate a non-failure at each height
7. Test Specimens level.
7.1 The profile shall be not less than 6 in. (150 mm) in 9.9 For any specimen that gives a break behavior that
length. appears to be an outlier, the conditions of that impact shall be
7.2 When the approximate mean-failure height for a given examined. The specimen is discarded only if a unique cause for
sample is known, 20 specimens usually yield sufficiently the anomaly can be found, such as an internal flaw visible in
precise results. If the mean failure height is not able to be the broken specimen. Note that break behavior varies widely
approximated, six or more specimens shall be used to deter- within a set of specimens. Data from specimens that show
mine the appropriate starting point of the test. atypical behavior shall not be discarded simply on the basis of
such behavior. Refer to Practice E178 for detailed information
NOTE 5—As few as five specimens often yield sufficiently reliable on how outliers shall be handled.
estimates of the mean failure height. However, in such cases, the estimated
standard deviation will be relatively large.3
10. Calculation
8. Conditioning 10.1 Mean Failure Height (Procedure A)—Calculate the
8.1 Unless otherwise specified, condition the test specimens mean failure height from the test data obtained as follows:
at 73.4 6 3.6°F (23 6 2°C) and 50 6 10 % relative humidity h 5 h o 1d h ~ A/N60.5!

where:
3
Brownless, K. A., Hodges, J. L., Jr., and Rosenblatt, Murray, “The Up-and- h = mean failure height, in. (cm),
Down Method With Small Samples”, American Statistical Association Journal,
dh = increment of weight height, in. (cm),
JSTNA, Vol 48, 1953, pp. 262–277.

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D4495 − 16

N = total number of failures or non-failures, whichever is 11.1.1 Complete identification of the sample tested, manu-
smaller. For ease of notation, call whichever are used facturer’s code, form, and previous history.
“events”, 11.1.2 Weight being used.
ho = lowest height at which an event occurred, in. (cm), 11.1.3 Number of test specimens (target points) employed
A = k to determine the mean failure height.
( in ,
i50
i 11.1.4 Mean failure energy.
11.1.5 Estimated standard deviation.
i = 0, 1, 2 . . . k (counting index, starts at ho), 11.1.6 Any departures from the specified test procedures.
ni = number of events which occurred at hi, and
hi = ho + idh. 12. Precision and Bias
In calculating h, the negative sign is used when the events
are failures. The positive sign is used when the events are 12.1 Precision—An interlaboratory study with five labora-
non-failures. tories was conducted in which various rigid poly(vinyl chlo-
ride) (PVC) extruded profiles were tested by means of a falling
10.2 Mean Failure Energy (Procedure A)—Compute the weight.
mean failure energy as follows: 12.1.1 The average within-laboratory and between-
MFE 5 h 3 w laboratory coefficients of variation were as follows:
where: Average V

MFE = mean failure energy, in./lb (J), Within Laboratory Between Laboratory
h = mean failure height, in. (cm), and 13.6 23.5
w = weight. where:
10.3 Estimated Standard Deviation—Calculate the esti- V = 100 S
mated standard deviation from the test data as follows:
MFE average
s 5 1.620 d FF ~ NB 2 A 2 !
N2
10.029G G 12.2 Bias—No statement of bias is provided because of the
k
lack of a referee method for impact behavior of plastics which
B5 (i 2
ni can provide a “true” or reference value.
i50

11. Report 13. Keywords


11.1 The report shall include the following: 13.1 impact resistance; profile toughness; PVC rigid profiles

APPENDIX

(Nonmandatory Information)

X1. SAMPLE CALCULATIONS

Height in. Outcome of


X—Failure 0—Non-Failure
40
38
36
34
32
30 X X X X
28 X O X O O X O
26 O O O O
24 O
22 X O
20 O O

Height in. Nx No i Ni iNi i 2Ni


30 4 0 4 4 16 64
28 3 4 3 3 9 27
26 0 4 2 0 0 0
24 0 1 1 0 0 0
22 1 1 0 1 0 0
20 0 2
Totals 8 12 8 25 91
(Nx) (No) (N) (A) (B)

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D4495 − 16
h o 5 22, N 5 N x 5 7 d 5 2 in.
S 5 1.620 d S NB 2 A 2
10.029 D
h 5 h o 1d S A
2 0.5 D N2
N
S 5 1.620~ 2 ! S 728 2 625
10.29 D
h 5 2212 S 25
8
2 0.5 D S 5 5.3 in.
64

h 5 27.2 in.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D4495 – 12) that may impact the use of this standard. (May 1, 2016)

(1) Revised 5.2 and Note 4.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4551 − 17 An American National Standard

Standard Specification for


Poly(Vinyl Chloride) (PVC) Plastic Flexible Concealed Water-
Containment Membrane1
This standard is issued under the fixed designation D4551; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* ization established in the Decision on Principles for the


1.1 This specification covers poly(vinyl chloride) (PVC) Development of International Standards, Guides and Recom-
flexible sheeting which is used without mastic, bedding, or mendations issued by the World Trade Organization Technical
coating for construction of concealed water-containment- Barriers to Trade (TBT) Committee.
membranes in applications where there is potential for costly
secondary damage from water leakage and very long-term 2. Referenced Documents
reliable performance is essential. Examples are fountains, 2.1 ASTM Standards:2
pools, planters, shower and safe pans, tile tubs, or similar wet D374/D374M Test Methods for Thickness of Solid Electri-
installations where the membrane is inaccessible once the cal Insulation
construction is complete. Included are requirements for mate- D412 Test Methods for Vulcanized Rubber and Thermoplas-
rials and sheeting, test methods, workmanship criteria, and tic Elastomers—Tension
methods of marking. D543 Practices for Evaluating the Resistance of Plastics to
1.2 Recycled materials may be used in this product in Chemical Reagents
accordance with the requirements in Section 5. D618 Practice for Conditioning Plastics for Testing
D883 Terminology Relating to Plastics
1.3 The tests are intended to ensure quality and performance D1004 Test Method for Tear Resistance (Graves Tear) of
and are not intended for design purposes. Tests have been Plastic Film and Sheeting
selected to be conducted primarily with liquids that simulate D1203 Test Methods for Volatile Loss From Plastics Using
the environment to which the membrane will be subjected Activated Carbon Methods
during actual use. D1204 Test Method for Linear Dimensional Changes of
1.4 This specification does not cover water-containment Nonrigid Thermoplastic Sheeting or Film at Elevated
membranes exposed to ultraviolet light. Temperature
1.5 The values stated in inch-pound units are to be regarded D1243 Test Method for Dilute Solution Viscosity of Vinyl
as the standard. The values given in parentheses are for Chloride Polymers
information only. D3892 Practice for Packaging/Packing of Plastics
E96/E96M Test Methods for Water Vapor Transmission of
1.6 There is no known ISO equivalent to this standard. Materials
1.7 The following precautionary caveat pertains only to the
2.2 ANSI Standard:
test method portion, Section 11, of this specification: This
Z 26.1 Safety Code for Safety Glazing Materials for Glazing
standard does not purport to address all of the safety concerns,
Motor Vehicles Operating on Land Highways3
if any, associated with its use. It is the responsibility of the user
of this standard to establish appropriate safety, health, and 2.3 Military Standard:
environmental practices and determine the applicability of MIL-STD-105 Sampling Procedures and Tables for Inspec-
regulatory limitations prior to use. tion by Attributes4
1.8 This international standard was developed in accor-
dance with internationally recognized principles on standard-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
1
This specification is under the jurisdiction of ASTM Committee D20 on Standards volume information, refer to the standard’s Document Summary page on
Plastics and is the direct responsibility of Subcommittee D20.24 on Plastic Building the ASTM website.
3
Products. Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
Current edition approved Dec. 1, 2017. Published January 2018. Originally 4th Floor, New York, NY 10036, http://www.ansi.org.
4
approved in 1986. Last previous edition approved in 2012 as D4551 – 12. DOI: Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
10.1520/D4551-17. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.

*A Summary of Changes section appears at the end of this standard


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D4551 − 17
3. Terminology TABLE 2 Quality Assurance Requirements

3.1 Definitions: Property Unit Specification Specification


Grade 30 Grade 40
3.1.1 General—Definitions are in accordance with Termi-
nology D883 unless otherwise indicated. Thickness in. (mm) 0.030 (0.765), min 0.040 (1.02), min
3.2 Definitions of Terms Specific to This Standard: Pinholes number none none
Shrinkage at 158°F % of original 5 %, max 5 %, max
3.2.1 water-containment membrane—a non-porous mem- Width in. (cm) +0.5 (1.27), −0.0 +0.5 (1.27), −0.0
brane impervious to water and resistant to permeation by water
vapor to an extent that it provides a high degree of certainty
that secondary damage from leakage shall not occur.
3.2.2 homogeneous sheeting—sheeting that is of uniform
6.2 Sheeting shall be compounded so that bonds between
composition throughout its thickness.
sheets used in fabrication of large water-containment mem-
4. Classification branes can be accomplished in the field without reducing the
overall resistance of the membrane to permeation or leakage or
4.1 The sheeting will be subdivided by grades based on significantly reducing the sheeting’s physical strength. The
thickness: manufacturer shall specify recommended bonding procedures
4.1.1 Grade 30—0.03 in. (0.765 mm). in its product literature.
4.1.2 Grade 40—0.04 in. (1.02 mm).
6.3 The sheeting shall be monolithic and homogeneous.
5. Materials and Manufacture
7. Dimensions
5.1 This specification covers poly(vinyl chloride) (PVC)
water-containment membrane formulated from PVC materials 7.1 Minimum thickness of Grade 30 sheeting shall be 0.03
meeting the following requirements: in. (0.765 mm) and minimum thickness of Grade 40 sheeting
5.1.1 A PVC resin with an inherent viscosity (logarithmic shall be 0.04 in. (1.02 mm).
viscosity number) of not less than 0.92 as determined by Test
Method D1243. 8. Workmanship
5.1.2 A PVC compound density of 1.26/1.29 g/cm3 . 8.1 If not monitored continuously, a minimum of every hour
5.2 Recycle materials, used in this product shall meet all the production shall be sampled and inspected for appearance,
requirements in Sections 3, 5, 6, and 9. thickness, width, and workmanship. The material shall be free
of pin holes, foreign inclusions, undispersed materials, or other
5.3 The use of water-soluble compounding ingredients shall defects that could affect serviceability.
be prohibited.
5.4 Plasticizers that are resistant to migration, mildew, and 9. Qualification Tests
bacterial degradation shall be used. 9.1 The PVC sheeting shall pass all the qualification tests
prescribed in Section 11 and Table 1.
6. Physical Properties 9.1.1 Any modification of this compound shall require that
6.1 The sheeting shall conform to the physical requirements the sheeting be retested for conformance to this specification.
prescribed in Section 9 (Table 1) and Section 16 (Table 2). In addition, retesting shall be done every 3 years whether the

TABLE 1 Qualification Tests


Property Unit Specification
Grade 30 Grade 40

Thickness in. (mm) 0.030 (0.765), min 0.040 (1.02), min


Tensile strength lbf/in. (kN/m) of width 60 (10.45), min 80 (14.05), min
Tensile stress at 100 % elongation lbf/in. (kN/m) of width 30 (5.23), min 40 (7.03), min
Elongation at break % 300, min 300, min
Tear resistance lbf/in. (kN/m) of width 185 (32.5), min 250 (43.7), min
Pinholes number none none
Micro-organism resistance specimen, pass/fail 12 of 12 pass 12 of 12 pass
Puncture resistance specimen, pass/fail 6 of 6 pass 6 of 6 pass
Indentation resistance specimen, pass/fail 3 of 3 pass 3 of 3 pass
Folding resistance specimen, pass/fail 3 of 3 pass 3 of 3 pass
Chemical resistance
Distilled H2O % weight change +1 %, max +1 %, max
Soapy H2O % weight change +2 %, max +2 %, max
Alkali specimen, pass/fail 3 of 3 pass 3 of 3 pass
Hydrostatic pressure test specimen, pass/fail 3 of 3 pass 3 of 3 pass
Shrinkage % original 5 %, max 5 %, max
Volatile loss at 158°F % loss 1.5 max 1.5 max

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D4551 − 17
compound has been modified or not to assess cumulative during the installation of the water-containment membrane in
effects of switching suppliers, grades of raw materials, or accordance with the procedure described in Annex A2.
processing changes. 11.6.2 Indentational Resistance Test—Determine the ability
of the material to withstand nail-head indentation without
10. Sampling impairing waterproofness. Conduct the test in accordance with
10.1 Test specimens shall be selected at random from the procedure detailed in Annex A3.
production stock. In each roll selected, units comprising the 11.6.3 Folding Resistance Test—Determine the ability of the
required number of specimens shall be taken from a portion not material to withstand corner folding without impairing water-
including the first or last foot of the roll or portions within 6 in. proofness in accordance with the procedure outlined in Annex
of the edge of the roll. A4.
11. Test Methods 11.7 Shrinkage—Test for 1 h at 158°F (70°C) in accordance
with Test Method D1204.
11.1 Thickness—Test five specimens obtained from loca-
tions equidistant across the width of the sheet in accordance 11.8 Hydrostatic Pressure Test—Determine the ability of
with Method C of Test Methods D374/D374M. Report thick- plastic membrane material to withstand water pressure without
ness of each specimen and location in sheet. leaking in accordance with the test procedure in Annex A5.
11.2 Stress-Strain Properties—Determine tensile stress at 11.9 Tear Resistance—Determine the average value for six
100 % elongation (modulus), tensile strength, and ultimate specimens in accordance with Test Method D1004.
elongation in accordance with Method A of Test Methods 11.10 Volatile Loss—Determine volatile loss in accordance
D412, using a dumbbell specimen (Die C). Report physical with Test Methods D1203, Method A, at 158°F (70°C) with
properties as the average value from testing of 6 specimens. grade AC (6⁄14 mesh) activated carbon. Test specimens shall be
11.3 Pinholes—Examine sheeting for pinholes by viewing nominal thickness sheeting.
the surface of the sheeting while held under slight-hand
NOTE 1—Requirement for Water—Vapor Transmission of Materials in
tension. Position a bright light source behind the film so as to Sheet Form (Procedure E of Test Methods E96/E96M) has been deleted
clearly illuminate the surface without producing glare in the until the test method is improved to the extent that it can be reproducibly
observer’s eyes. A pinhole is defined as any opening observed run by commercial laboratories.
in the sheet under the conditions specified. Examine a 12-in.
(305-mm) strip from the entire width of the sheet and report the 12. Conditioning
presence or absence of pinholes. 12.1 Condition all qualification test specimens at 73 6 4°F
11.4 Resistance to Chemical Reagents—Conduct this test in (23 6 2°C) and 50 6 10 % relative humidity for not less than
accordance with Test Method D543, Procedure 1. 40 h prior to testing, in accordance with Method A of Methods
11.4.1 Weigh loss after immersion in distilled water at D618.
120°F (49°C) for 24 h.
12.2 In-plant quality control specimens shall be conditioned
11.4.2 Weigh loss after immersion in a 1 % soapy water
at 73 6 4°F (23 6 2°C) for 2 h in air.
solution at 120°F (49°C) for 24 h.
11.4.3 Alkali Resistance Test—This test indicates the effect
13. Certification
of hot alkali solutions on the plastic membrane materials.
11.4.3.1 Specimens—Each test unit shall consist of three 13.1 When specified in the purchase order or contract, the
specimens of flat material 3 by 3 in. (76 by 76 mm) selected in manufacturer’s or the supplier’s certification shall be furnished
accordance with 12.1. to the purchaser stating that samples representing each lot have
11.4.3.2 Procedure—Make a solution by dissolving 5.0 g of been manufactured, tested, and inspected in accordance with
reagent-grade sodium hydroxide and 5.0 g of reagent-grade this specification and the requirements have been met. When
potassium hydroxide in 1 L of distilled water in a beaker. The specified in the purchase order or contract, a report of the test
solution shall be maintained at a temperature of 150°F (66°C). results shall be furnished.
11.4.3.3 Immerse each specimen in its own individual
beaker of solution in accordance with 11.4.3.2. Immerse the 14. Product Marking
specimen for 72 h, and completely change the solution every 14.1 Material complying with this specification shall be
24 h. Before immersion of a specimen in the new solution, the continuously marked and shall include the following spaced
solution shall be at a temperature of 150°F (66°C). out at intervals of not more than 2 ft (610 mm).
11.4.3.4 Test each specimen for waterproofness in accor-
14.1.1 Manufacturer’s name (or brand name or trademark).
dance with 11.8 for hydrostatic pressure test.
14.1.2 Material designation.
11.5 Microorganism Resistance Test—Determine the resis- 14.1.3 Designation, Grade 30 or Grade 40, with which the
tance of PVC membrane to mold growth in accordance with sheet complies.
Annex A1. 14.1.4 Designation, “ASTM D4551”, with which the sheet
11.6 Strength and Toughness Tests: complies.
11.6.1 Puncture Resistance Test—Determine the resistance 14.1.5 The production code shall be included inside the core
of the material to mechanical damage which might occur of all shipping units.

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D4551 − 17
15. Packaging and Package Marking 16.1.1 In addition to the in-plant quality control inspections
15.1 The material shall be rolled on a substantial core and specified in Section 8, at least annually samples shall be tested
packaged in standard commercial containers, so constructed as and certified as complying with the requirements of Table 2.
to ensure acceptance by common or other carriers for safe 16.2 If the results of any tests do not conform to the
transportation to the point of delivery, unless otherwise speci- requirements of this specification, retesting to determine con-
fied in the contract or order. formity may be performed as agreed upon between the
15.2 Shipping containers shall be marked as agreed upon purchaser and the seller.
between the purchaser and the seller.
15.3 Packaging provisions for government/military procure- 17. Keywords
ment. 17.1 flexible sheeting; fountains; planters; pools; poly(vinyl
15.4 All packing, packaging, and marking provisions of chloride); PVC; recycle usage; shower and safe pans; tile tubs;
Practice D3892 shall apply to this specification. water containment membrane; water leakage resistance; water
permeation
16. Quality Assurance
16.1 Sheeting manufactured from compound qualified by
Section 9 shall pass the quality assurance and control require-
ments prescribed in Table 2.

SUPPLEMENTARY REQUIREMENTS

QUALITY ASSURANCE PROVISIONS FOR GOVERNMENT/MILITARY


PROCUREMENT

These requirements apply only Federal/Military procurement, not domestic sales or transfers.

S1. Selection of Acceptable Quality Level (AQL) and of IL AQL


Inspection Level (IL) shall be made with consideration of the Defects in material and workmanship II 2.5
Defects of preparation for delivery S-2 2.5
specific use requirements. This is discussed in Sections 7 and Testing (products) S-1 1.5
8 of the above document, with reference to MIL-STD-105. Testing (polymer, unfabricated) S-1 ...
S3. In the absence of contrary requirements the following
values shall apply:

ANNEXES

(Mandatory Information)

A1. MICROORGANISM RESISTANCE TEST

A1.1 Specimens—Each unit of specimens shall consist of A1.2.1.6 Petri Dishes (4 in.) 10 cm in diameter with covers
twelve samples of material each 11⁄2 by 11⁄2 in. (38 by 38 mm) capable of being sealed with cellophane tape. One petri dish is
square, selected in accordance with 11.1. required for each of the twelve samples comprising a test unit.
A1.2.1.7 Incubation Chamber, capable of maintaining a
A1.2 Apparatus, medium and test fungi. temperature of 84.5 6 1.8°F (296 1°C) and a relative humidity
A1.2.1 Apparatus shall consist of: of at least 50 %.
A1.2.1.1 Autoclave, capable of maintaining an interior tem- A1.2.1.8 Sterile Room, dust-free, using sterilamps, antisep-
perature of 251 6 4°F (122 6 2°C) at a pressure of 15.5 6 0.5 tic spray, or air filtration under pressure to maintain sterile
lb psig (107 6 3.5 kPa) for the purpose of sterilizing glassware conditions.
and the medium. A1.2.2 Test Fungi:
A1.2.1.2 Erlenmeyer Flask, 100-cm2 capacity. A1.2.2.1 Chaetomium globosum, ATCC 6205.
A1.2.1.3 Glass Beads, 1⁄4 in. (6 mm) in diameter, 5 pieces. A1.2.2.2 Aspergillus niger, ATCC 6275.
A1.2.1.4 Glass Pipettes, two required. A1.2.3 Medium—A culture medium of the following com-
A1.2.1.5 Wire Loop, of nichrome wire. position:

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NH4NO3 3.0 g A1.3.4 Inoculate six specimens of each test unit as defined
KH2PO4 2.5 g in A1.1 with each of the two varieties of fungi. Inoculate three
MgSO47H2O 2.0 g
K2HPO4 2.0 g
with the face side up and three with the back side up.
Agar 20.0 g A1.3.4.1 Preparation—Handle each specimen under aseptic
Distilled water to make 1000 mL conditions and sterilize by dipping in 70 % ethanol for a few
Adjust the pH to a range from 6.4 to 6.8 with HCl or NaOH, seconds followed by a thorough rinse in distilled water after
as required. This is the base medium for both fungus cultures. which place each firmly in the center of the solidified agar
However, the medium to be used for the Aspergillus niger shall medium in its respective petri dish. Test six of the specimens
be enriched by adding 30 g of brown sugar. with one fungi and six with the other. Of each subunit of six,
test three with one surface in contact with the medium and
A1.3 Procedure: three in contact with the opposite surface as stated under
A1.3.1 Prepare medium as specified in A1.2.3 and pour in A1.3.4.
the required number of petri dishes to a depth of 3⁄8 in. (9.5 A1.3.4.2 Place controls in each petri dish along with the
mm). specimen. Each control shall be a strip of sterile blotting paper
A1.3.2 Sterilize in the autoclave, all of the apparatus in or filter paper placed on the agar separated from the specimen.
A1.2.1 including the medium contained in the petri dishes by The purpose of the control is to provide a medium for the
retention in the autoclave at the temperature and pressure fungi, thus proving that the fungi is active.
prescribed in A1.2.1.1 for 60 min. After sterilization, remove to A1.3.4.3 Make inoculation with a particular fungus by using
sterile room of A1.2.1.8, taking care not to contaminate the a sterile pipette individual to the fungus. With the pipette,
sterilized equipment and medium. Use the sterile room for all distribute approximately 1.5 mL of inoculum over the
preparation procedures. specimen, the control, and the surrounding medium.
A1.3.3 Cultures, Stock and Substocks, and Inoculum: A1.3.5 Incubate the inoculated specimens for a period of 28
A1.3.3.1 Carefully maintain Chaetomium globosum fungus days at a temperature of 84.5 6 1.8°F (29 6 1°C) and a
stock cultures on strips or squares of sterile porous filter paper, relative humidity of 90 %. An appropriate incubation condition
or blotting paper, on a sterilized culture medium as specified in is obtained by placing the covered and sealed petri dishes in a
A1.2.3 and A1.3.2. If there is evidence of contamination, room or chamber maintained at 85°F (29.5°C) and 50 %
promptly renew the culture. The culture may be kept for not relative humidity.
more than four months in a refrigerator at approximately 37.5
to 50°F (3 to 10°C). A1.3.6 Results—Reject test dishes with controls that do not
(1) Prepare subcultures from a stock culture by transferring exhibit a substantial growth of fungi after 7 days of incubation
spores from the stock culture to a sterilized covered petri dish and start anew. Examine a unit test, the controls of which
containing sterilized medium. Incubate the subculture for a indicate a substantial fungus growth, after the required 28-day
period of 7 to 21 days at 84.5 6 1.8°F (29 6 1°C) in the incubation period. If after this period any one of the specimens
incubation chamber until in a ripe fruiting condition. show evidence of evenly distributed or intense localized fungus
(2) Prepare inoculum by transferring the spores with the growth under 16X magnification of either side of the sample
sterilized wire loop to a sterilized Erlenmeyer flask containing (excluding growth overlapping the edges), the test sample shall
five sterilized glass beads and 10 mL of distilled water. Shake be considered to have failed the test.
this mixture sufficiently to break up the spores, after which the A1.3.6.1 Photographs of the specimen taken at the end of
solution shall be diluted to 200 mL. the 28 day incubation period are required as a part of the test
A1.3.3.2 Carefully maintain Aspergillus niger fungus stock on fungus resistance. Take each photograph with a scale laid
cultures as specified in A1.3.3.1 (1) on a medium as specified beside the specimen to indicate its size, allowing the light
in A1.3.3.1. conditions of the photographs to reveal the nature and height of
(1) Prepare subcultures and incubate as in A1.3.3.1 (1) the fungus growth on the surface of the material. Enlarge the
using a medium as specified in A1.3.3.1. photographs so the specimen will be a 6 by 6 in. (152 by 152
(2) Prepare inoculum as specified in A1.3.3.1 (2). mm) size.

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A2. PUNCTURE-RESISTANCE TEST

A2.1 Specimens—Six 10 by 10 in. (254 by 254 mm) pieces A2.3 Procedure:


of material shall make up each test unit.
A2.3.1 Test three specimens with one side up and three with
A2.2 Apparatus:5 the opposite side up.
A2.2.1 Specimen Holder (Fig. A2.1), shall consist of two 10 A2.3.2 Place a single specimen between the holding frame
by 10 in. (254 by 254-mm) square pieces of 3⁄4 in. (19 mm) halves and clamp securely by tightening the thumb screws.
smooth surface hard maple. One of these pieces shall contain a Suspend the impact dart vertically above the center of the
symmetrically located 6 by 6-in. (152 by 152-mm) opening in specimen with a vertical distance of 3 ft (0.91 m) between the
the center. Sandwich the specimen between two specimen nose of the dart and the surface of the specimen.
holders, placing the holder with the opening on top. Three
thumb screws or bolts located in the center of each side are A2.3.3 Release the dart for one free fall on each specimen.
used to securely clamp the specimen within the holder. A2.4 Results:
A2.2.2 Impact Dart—A7 6 1-oz (196 to 201-g) steel dart as
A2.4.1 Visible rupture of any specimens shall require rejec-
described in Fig. A2.2.
tion of the materials in accordance with 17.2.

5
A2.4.2 All specimens passing this test for rupture shall be
Photographs of apparatus described are published in Federal Housing Admin-
istration Document 4900.1, Appendix D, available from the U.S. Department of
further hydrostatically tested in accordance with 11.8 with the
Housing and Urban Development, 451 7th St., SW, Washington, DC 20410. point of impact in the center of the test apparatus.

FIG. A2.1 Wood Holding Fixture for Drop Test

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FIG. A2.2 Dart for Safety Glass Tests

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D4551 − 17

A3. TEST FOR RESISTANCE TO INDENTATION

A3.1 Specimens—The specimens shall be in accordance A3.3 Procedure—Place the specimen on the supporting
with 11.1. plate of the apparatus with the bottom surface up, and lower the
indenter gently until its face contacts the surface of the
A3.2 Apparatus5—The apparatus shall consist of an in- specimen. Within 1 or 2 s, apply the total load of 120 lb (54.4
denter acting under a total weight of 120 lb (54.4 kg), a smooth
kg) to the specimen and maintain for a period of 60 min.
steel plate as a specimen support, and a rigid form for
supporting the indenter and the imposed weight. The indenting A3.4 Results—Test each specimen of the test unit
head shall be a 0.178-in. (4.5-mm) diameter steel bar with the hydrostatically, in accordance with 11.8, with the water con-
pressing face buffed smooth, but not rounded. The rigid tacting each of the specimens on the side opposite the
support shall hold the indenter vertically so that the indenting indentation and with the indentation centered in the hydrostatic
face shall contact the specimen in the plane of the contact test specimen holder.
surface of the specimen when the specimen is placed on the
horizontal steel plate. The shaft of the indenter shall be capable
of vertical motion along its axis without friction when the
weight causing indentation is imposed thereon.

A4. FOLDING RESISTANCE TEST

A4.1 Specimens—The specimens shall be in accordance s. Then, remove the specimen from the mandrel without
with 12.1. unfolding and place on a smooth, hard surface for support
while the weight is placed on the fold for 30 s. Place the weight
A4.2 Apparatus—The apparatus shall consist of a 10-lb so that its force is evenly distributed over the full length of the
(4.5-kg) weight having a smooth, flat surface, a 1⁄4-in. (6.3-mm) fold. Unfold each specimen and repeat the bending and
diameter mandrel, and a constant temperature chamber to be weighing operation on each specimen with the second bend
maintained at 0 6 2°F (−17 6 1°C). being at 90° to the first and on the same side. Note that all
bends shall be made with the surface of the material intended
A4.3 Procedure—Place the specimen, weight, and mandrel
to be toward the water exposure on the inside of the bend.
in the constant-temperature chamber and accomplish all opera-
tions for the bend test therein. After temperature conditioning A4.4 Results—After unfolding, test each specimen of the
the apparatus and the test unit of specimens for 4 h at within test unit hydrostatically, in accordance with 11.8, with each
62°F (61°C) of the temperature indicated in A4.2, bend each specimen placed so that the inside of the folds are in contact
specimen over the mandrel through an angle of 180°. Make the with the water and with the intersection of the two folds
bend in the middle of each specimen and complete it within 1 centered in the hydrostatic test specimen holder.

A5. HYDROSTATIC PRESSURE TEST

A5.1 Specimens—Each test unit shall consist of three speci- mm) with a cutoff valve or other suitable device at the water
mens of flat material 3 by 3 in. (76 by 76 mm) selected in inlet to the pressure tube for isolating the sample until the
accordance with 12.1. desired head is reached.
A5.2 Apparatus5—The apparatus for the hydrostatic pres- A5.3 Procedure—Clamp the test specimen face down in the
sure test shall consist essentially of a pressure tube connected holder, which has been previously filled with water, the face
to a specimen holder. The inner diameter of the pressure tube being that surface which is intended to be installed toward the
shall be 2 in. (51 mm) and the outer diameter 3 in. (76 mm) water receptor. Take care to avoid trapped air between the
with a means for introducing water for below the specimen. specimen and the water. This is done by filling the holder with
Connect an extension tube to permit a water head of 2 ft (610 water and sliding the specimen onto the holder in direct contact

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D4551 − 17
with the water after having used a piece of transparent material
for practice and for becoming familiar with the technique. Fill
the tube to achieve a 2-ft (610-mm) head.
A5.4 Requirement—Make observations at 10-min intervals
for the first hour, and at hourly intervals for the succeeding 7 h,
after which leave the specimen under hydrostatic pressure for
40 h and examine again. Any evidence of wetness on top of the
material or the formation of a droplet shall cause the material
to be rejected.

A6. PRECISION AND BIAS FOR ANNEX TEST METHODS

A6.1 Precision—Precision testing has not been possible on A6.2 Bias—No determination of bias is possible in any of
any of the annex test methods because there are presently an the annex test methods since no referee methods are available.
inadequate number of product producers to permit statistically
valid precision studies.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4551–12)
that may impact the use of this standard. (December 1, 2017)

(1) Section 2: Reinstated D374/D374M-16, had been with- (6) Section 7: Renumbered 7.2 to 7.1.
drawn 2013. (7) Subsection 11.1: Added D374M reference.
(2) Section 2: Deleted D7209 reference, standard has been (8) Deleted Section 13.
withdrawn. (9) Renumbered Sections 14 – 18 to 13 – 17.
(3) Subsection 5.2 reworded, deleted D7209 reference. (10) Subsection A1.2.1.1: Changed 63.6°F to 64°F per D618-
(4) Deleted subsection 6.3, renumbered 6.4 to 6.3. 13.
(5) Section 7: Dimensions, deleted 7.1, 7.1.1 and 7.1.2.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4659 − 19

Standard Test Methods for


Polyurethane Raw Materials: Determination of Specific
Gravity of Isocyanates 1
This standard is issued under the fixed designation D4659; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D4052 Test Method for Density, Relative Density, and API
1.1 These test methods determine the specific gravity of Gravity of Liquids by Digital Density Meter
toluenediisocyanate, polymeric (methylene phenylisocyanate), E100 Specification for ASTM Hydrometers
and liquid methylene di(phenylisocyanate). These test methods E456 Terminology Relating to Quality and Statistics
also are applicable to many other liquids. (See Note 1.) E202 Test Methods for Analysis of Ethylene Glycols and
1.1.1 Test Method A—Specific gravity by pycnometer, for Propylene Glycols
high-accuracy determination. E2251 Specification for Liquid-in-Glass ASTM Thermom-
1.1.2 Test Method B—Specific gravity by hydrometer, for a eters with Low-Hazard Precision Liquids
less accurate, but rapid, determination. E2935 Practice for Conducting Equivalence Testing in
Laboratory Applications
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3. Terminology
standard.
3.1 Definitions—Terms used in this standard are defined in
1.3 This standard does not purport to address all of the accordance with Terminology D883, unless otherwise speci-
safety concerns, if any, associated with its use. It is the fied. For terms relating to precision and bias and associated
responsibility of the user of this standard to establish appro- issues, the terms used in this standard are defined in accordance
priate safety, health, and environmental practices and deter- with Terminology E456.
mine the applicability of regulatory limitations prior to use.
3.2 Definitions of Terms Specific to This Standard:
NOTE 1—There is no known ISO equivalent to this standard. 3.2.1 specific gravity—the ratio of the weight in air of a
1.4 This international standard was developed in accor- given volume of the material at a stated temperature to the
dance with internationally recognized principles on standard- weight in air of an equal volume of water at a stated
ization established in the Decision on Principles for the temperature. It shall be expressed as specific gravity, 25/25°C,
Development of International Standards, Guides and Recom- indicating that the sample and reference water were both
mendations issued by the World Trade Organization Technical measured at 25°C.
Barriers to Trade (TBT) Committee.
4. Significance and Use
2. Referenced Documents 4.1 These test methods can be used for research or for
2.1 ASTM Standards:2 quality control to characterize isocyanates used in polyurethane
D883 Terminology Relating to Plastics products.
D891 Test Methods for Specific Gravity, Apparent, of Liquid 4.2 A general test method for specific gravity using a digital
Industrial Chemicals density meter, which applies to isocyanates as well as other
D1193 Specification for Reagent Water liquids is published in Test Method D4052.
TEST METHOD A—SPECIFIC GRAVITY BY
1
These test methods are under the jurisdiction of ASTM Committee D20 on PYCNOMETER
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular
Materials - Plastics and Elastomers. 5. Apparatus
Current edition approved Aug. 1, 2019. Published August 2019. Originally
approved in 1987. Last previous edition approved in 2014 as D4659 - 14. DOI: 5.1 Pycnometer, of 25 or 50-mL capacity, conical shape with
10.1520/D4659-19.
2
a capillary side arm overflow tube having a standard-taper 5/12
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ground-glass joint and a ground-glass vented cap. A thermom-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on eter graduated from 12 to 38°C in 0.2° divisions attached to the
the ASTM website. neck of the flask by a standard-taper 10/18 ground-glass joint.

*A Summary of Changes section appears at the end of this standard


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D4659 − 19
This thermometer is to be calibrated using the ASTM ther- 9.2 Fill the pycnometer with freshly boiled distilled water
mometer specified in 5.3. that has been cooled to 22 to 24°C. Insert the thermometer into
5.2 Water Bath—A water bath maintained at 25 6 0.05°C. the pycnometer without trapping air bubbles. Place the pyc-
nometer in a water bath at 25 6 0.05°C and allow it and its
5.3 Thermometer—An ASTM low-softening point contents to equilibrate for at least 30 min. Wipe the overflow
thermometer, calibrated from −2 to +80°C, which meets the from the side-arm capillary and cover it with the vented cap.
requirements for Thermometer S15C in Specification E2251. Remove the pycnometer from the bath, wipe dry, and weigh.
5.4 Analytical Balance—A balance having a sensitivity of at 9.3 Empty the pycnometer and rinse it with alcohol, then
least 0.1 mg. with ether. Remove the ether and dry the pycnometer under
6. Reagents and Materials vacuum for 15 min. (See Note 2.) Weigh the pycnometer.
Determine the weight, W, of the water at 25.0°C in air by
6.1 Purity of Reagents—Use reagent grade chemicals in all subtracting the weight of the empty pycnometer from the
tests. Unless otherwise indicated, it is intended that all reagents weight of the pycnometer filled with water.
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society where such NOTE 2—Other drying techniques are acceptable if ether is to be
specifications are available.3 Other grades are acceptable, avoided. It must be established that for any alternative drying method, a
clean and dry pycnometer results.
provided it is ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the 9.4 The isocyanate sample for testing must be completely
determination. liquid, that is, free of any solid material. Fill the pycnometer,
while minimizing exposure of the sample to air.
6.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water as defined 9.5 Insert the thermometer into the pycnometer without
by Type IV or better of Specification D1193. trapping air bubbles and cleanly wipe any sample off the
6.3 Chromic Acid Cleaning Solution—Prepare a saturated outside of the pycnometer. Allow the pycnometer to equilibrate
solution of chromic acid (CrO3) in concentrated sulfuric acid in the water bath for at least 30 min. Wipe any overflow from
(H2SO4, sp gr 1.84). the side arm capillary and cover it with the vented cap. Remove
the pycnometer from the bath, wipe dry, and weigh. To obtain
7. Sampling the weight, S, of the sample at 25.0°C, subtract the weight of
7.1 Since organic isocyanates react with atmospheric the empty pycnometer from the weight when filled with
moisture, take special precautions in sampling. Usual sampling sample.
methods, even when conducted rapidly, can cause contamina-
tion of the sample with insoluble urea. Therefore, blanket the 10. Calculation
sample with dry air or nitrogen at all times. (Warning— 10.1 Calculate the specific gravity at 25/25°C as follows:
Diisocyanates are eye, skin and respiratory irritants at concen- S
trations above the occupational exposure limit (TLV or PEL). Specific gravity, 25/25°C 5
W
Diisocyanates can cause skin and respiratory sensitization
(asthma) in some people. Once sensitized, it is essential to limit where:
further exposure to diisocyanates. Use a combination of S = sample used, g (see 9.5), and
engineering controls and personal protective equipment, in- W = water in the pycnometer, g (see 9.3).
cluding respiratory, skin and eye protection, to prevent over-
exposure to diisocyanates. Consult the product suppliers’ 11. Precision and Bias
Safety Data Sheet (SDS) for more detailed information about
11.1 Attempts to develop a precision and bias statement for
potential health effects and other specific safety and handling
this test method have not been successful. Data on precision
instructions for the product.)
and bias cannot be given for this reason. Anyone wishing to
8. Test Conditions participate in the development of precision and bias data can
contact the Chairman, Subcommittee D20.22 (Section
8.1 Keep laboratory humidity low, preferably around 50 %
D20.22.01), ASTM, 100 Barr Harbor Drive, West
relative humidity.
Conshohocken, PA 19428-2959.
9. Procedure 11.2 Test Method E202 is similar and does include precision
9.1 Clean the pycnometer by filling it with chromic acid data. Precision statements from E202 are restated below as an
cleaning solution and allowing it to stand for a few hours. estimate of the precision for this test method.
Empty the pycnometer and rinse well with distilled water. 11.2.1 Repeatability—It has been estimated that the maxi-
mum expected difference between two test results for the same
3
Reagent Chemicals, American Chemical Society Specifications, American material, obtained by the same operator using the same
Chemical Society, Washington, DC. For suggestions on the testing of reagents not equipment on the same day in the same laboratory due solely
listed by the American Chemical Society, see Analar Standards for Laboratory to the method is 0.0002 units.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, 11.2.2 Reproducibility—It has been estimated that the maxi-
MD. mum expected difference between two test results for the same

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D4659 − 19
material, obtained by different operators using different equip- 15.2 To avoid forming air bubbles, slowly pour the sample
ment in different laboratories due solely to the method is into the dry hydrometer cylinder. Place the cylinder in the
0.0008 units. water bath. Stir the contents of the cylinder, being careful to
11.3 Bias—There are no recognized standards by which to avoid formation of air bubbles. When the temperature of the
estimate the bias of this test method. sample is 24.8°C, slowly and carefully lower the hydrometer
into the sample liquid to a level two small scale divisions
11.4 For information on equivalence, refer to Practice below that at which it will float and then release the hydrom-
E2935. eter. Allow the hydrometer to come to rest and make sure it
TEST METHOD B—SPECIFIC GRAVITY BY does not touch the walls of the cylinder and that there are no
HYDROMETER trapped air bubbles. When the temperature of the sample
reaches 25.0°C, read the value on the hydrometer at the
12. Apparatus meniscus line of the sample.
12.1 Hydrometer—An ASTM hydrometer with a specific 15.3 Determine the temperature of the sample just before
gravity range from 1.195 to 1.255 at 15.6/15.6°C conforming and just after reading the hydrometer.
to the requirements for Hydrometer 115H in Specification 16. Calculation
E100.
16.1 Calculate the specific gravity at 25/25°C as follows
12.2 Hydrometer Cylinder—A clear glass cylinder with an (Note 3):
inside diameter at least 25.4 mm [1 in.] larger than the Specific gravity, 25/25°C 5 observed value10.0021
hydrometer and tall enough so that there is at least 1 in. NOTE 3—The correction factor +0.0021 is applied to correct the reading
between the bottom of the cylinder and the bottom of the to 25/25°C because the hydrometer was standardized at 15.6/15.6°C.
hydrometer after equilibration at 25°C.
17. Precision and Bias
12.3 Thermometer—See 5.3.
17.1 Attempts to develop a precision and bias statement for
12.4 Water Bath—See 5.2. this test method have not been successful. Data on precision
and bias cannot be given for this reason. Anyone wishing to
13. Sampling participate in the development of precision and bias data can
13.1 Since organic isocyanates react with atmospheric contact the Chairman, Subcommittee D20.22 (Section
moisture, take special precautions in sampling. Usual sampling D20.22.01), ASTM, 100 Barr Harbor Drive, West
methods, even when conducted rapidly, can cause contamina- Conshohocken, PA 19428-2959.
tion of the sample with insoluble urea. Therefore, blanket the 17.2 Test Method D891 is similar and does include preci-
sample with dry air or nitrogen at all times. (Warning— sion data. Precision statements from D891 are restated below
Diisocyanates are eye, skin and respiratory irritants at concen- as an estimate of the precision for this test method.
trations above the occupational exposure limit (TLV or PEL). 17.2.1 Repeatability—It has been estimated that the maxi-
Diisocyanates can cause skin and respiratory sensitization mum expected difference between two test results for the same
(asthma) in some people. Once sensitized, it is essential to limit material, obtained by the same operator using the same
further exposure to diisocyanates. Use a combination of equipment on the same day in the same laboratory due solely
engineering controls and personal protective equipment, in- to the method is 0.0005 units.
cluding respiratory, skin and eye protection, to prevent over- 17.2.2 Reproducibility—It has been estimated that the maxi-
exposure to diisocyanates. Consult the product suppliers’ mum expected difference between two test results for the same
Safety Data Sheet (SDS) for more detailed information about material, obtained by different operators using different equip-
potential health effects and other specific safety and handling ment in different laboratories due solely to the method is
instructions for the product.) 0.0021 units.
17.3 There are no recognized standards by which to esti-
14. Test Conditions
mate the bias of this test method.
14.1 Keep laboratory humidity low, preferably around 50 %
17.4 For information on equivalence, refer to Practice
relative humidity
E2935.
15. Procedure 18. Keywords
15.1 The isocyanate sample for test must be completely 18.1 density; hydrometer; isocyanates; polyurethane raw
liquid, that is, free of any solid material. materials; pycnometer; specific gravity

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D4659 − 19
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4659 - 14)
that may impact the use of this standard. (August 1, 2019)

(1) Removed nonmandatory language and corrected grammar (3) Removed definitions and statements of equivalency from
throughout. Precision and Bias, Sections 11 and 17.
(2) Updated 7.1 and 13.1 with latest wording from Center for
the Polyurethane Industry’s Sustainability subcommittee’s
EHS warning.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4674 − 19

Standard Practice for


Accelerated Testing for Color Stability of Plastics Exposed
to Indoor Office Environments1
This standard is issued under the fixed designation D4674; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 1.7 This international standard was developed in accor-


1.1 This practice covers the basic principles and operating dance with internationally recognized principles on standard-
procedures for using fluorescent light to determine color ization established in the Decision on Principles for the
stability of plastics when materials are exposed in typical office Development of International Standards, Guides and Recom-
environments where fluorescent overhead lighting and mendations issued by the World Trade Organization Technical
window-filtered daylight are used for illumination and where Barriers to Trade (TBT) Committee.
temperature and humidity conditions are in accordance with
2. Referenced Documents
American Society of Heating, Refrigerating, and Air-
conditioning Engineers (ASHRAE) recommendations for 2.1 ASTM Standards:2
workers’ comfort. D1729 Practice for Visual Appraisal of Colors and Color
Differences of Diffusely-Illuminated Opaque Materials
1.2 This practice describes four methods where specimens
D2244 Practice for Calculation of Color Tolerances and
are exposed to fluorescent light under controlled environmental
Color Differences from Instrumentally Measured Color
conditions. Two of the methods use an exposure device that
Coordinates
provides for mixing of fluorescent lamps and two of the
D3980 Practice for Interlaboratory Testing of Paint and
methods use devices that comply with Practice G154.
Related Materials (Withdrawn 1998)3
NOTE 1—Method I uses cool white fluorescent lamps and window glass D5870 Practice for Calculating Property Retention Index of
filtered fluorescent UVB lamps and is the same method described in Plastics
previous versions of this standard.
E691 Practice for Conducting an Interlaboratory Study to
1.3 Specimen preparation and evaluation of the results are Determine the Precision of a Test Method
covered in ASTM methods or specifications for specific G113 Terminology Relating to Natural and Artificial Weath-
materials. General guidance is given in Practice G151. More ering Tests of Nonmetallic Materials
specific information about methods for determining the change G141 Guide for Addressing Variability in Exposure Testing
in properties after exposure and reporting these results is of Nonmetallic Materials
described in Practice D5870. G147 Practice for Conditioning and Handling of Nonmetal-
1.4 The values stated in SI units are to be regarded as the lic Materials for Natural and Artificial Weathering Tests
standard. G151 Practice for Exposing Nonmetallic Materials in Accel-
erated Test Devices that Use Laboratory Light Sources
1.5 Unless otherwise specified, all dimensions are nominal. G154 Practice for Operating Fluorescent Ultraviolet (UV)
1.6 This standard does not purport to address all of the Lamp Apparatus for Exposure of Nonmetallic Materials
safety concerns, if any, associated with its use. It is the G169 Guide for Application of Basic Statistical Methods to
responsibility of the user of this standard to establish appro- Weathering Tests
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3. Terminology
Specific precautionary statements are given in Section 7. 3.1 Definitions—The definitions given in Terminology G113
NOTE 2—There is no known ISO equivalent to this standard. are applicable to this practice.

1 2
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and For referenced ASTM standards, visit the ASTM website, www.astm.org, or
is the direct responsibility of Subcommittee D20.50 on Durability of Plastics. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved April 15, 2019. Published May 2019. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1987. Last previous edition approved in 2010 as D4674 - 02a(2010), the ASTM website.
3
which was withdrawn January 2019 and reinstated in April 2019. DOI: 10.1520/ The last approved version of this historical standard is referenced on
D4674-19. www.astm.org.

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D4674 − 19
4. Summary of Practice that at least three replicates of each material be exposed to
4.1 This practice provides for the exposure of specimens to allow for statistical evaluation of results.
fluorescent light under controlled environmental conditions.
Radiant energy is provided by one of the following fluorescent 6. Apparatus
light sources: (1) VHO cool-white fluorescent lamps and glass 6.1 Test Chamber—Unless otherwise specified, the test
filtered fluorescent UV lamps, (2) VHO cool-white fluorescent chamber shall comply with the requirements of Practice G151.
lamps alone, (3) standard output cool white fluorescent lamps 6.1.1 The test chamber used for Methods I and II shall be
alone, or (4) UVA-351 fluorescent UVA lamps. designed so that simultaneous operation of VHO cool white
4.1.1 Method I is intended to simulate the conditions in an and glass filtered UV fluorescent lamps is possible, and shall be
office environment plus a portion of solar UV radiation equipped with a radiometer complying with the requirements
transmitted by window glass. Methods II and III are intended of Practice G151 and calibrated from 250 to 400 nm. Annex
to simulate only the indoor lighting component of a typical Annex A1 contains more information about the design of the
office environment. Method IV is intended to simulate only the apparatus used for Methods I and II.
effects of a portion of solar UV radiation transmitted through 6.1.2 The test chamber used for Methods III and IV shall
window glass. conform to the requirements of Practice G154.
NOTE 3—A comparison of the four listed methods has not been 6.2 The spectral distribution of the UVB-313, UVA-340,
performed, and as such, results obtained from each method cannot be and UVA-351 shall comply with the requirements of practice
considered as equivalent.
NOTE 4—For more information on the use of fluorescent UV lamps to
G154. The spectral power distribution of the cool white lamps
simulate solar UV radiation behind window glass, refer to Annex A1 of used shall comply with the requirements given in Annex Annex
Practice G154. A2.
4.1.2 Do not compare Comparison of results obtained from 6.3 Window glass—Unless otherwise specified the window
specimens exposed using the methods described should not be glass shall be good grade clear, flat, drawn “single strength”
made unless correlation has been established between the sheet glass free of bubbles or other imperfections and between
methods being compared for the materials being tested. 2.0 and 2.5 mm in thickness. The glass shall be preaged in the
4.2 Color change is determined periodically throughout the device for at least 24 hours prior to use.
course of the exposure by comparison of the exposed speci- 6.4 For Methods I and II, place the apparatus in an envi-
mens to unexposed specimens, using either visual or instru- ronment that meets ASHRAE recommendations of 20 to
mental procedures. 25.5°C and 40 to 50 % relative humidity. For Methods III and
IV follow the requirements of Practice G154 for the area in
5. Significance and Use which the instruments are used.
5.1 Tests conducted in accordance with this practice are 6.5 Instrument Calibration—To ensure standardization and
intended to induce property changes associated with use accuracy, the instruments associated with the exposure appa-
exposure to light and heat in typical office environments. These ratus (for example, timers, thermometers, UV sensors, and
exposures are not intended to simulate the deterioration caused radiometers) require periodic calibration to ensure repeatability
by localized phenomena such as handling, dirt contamination, of test results. Whenever possible, calibration should needs to
etc. be traceable to national or international standards. Unless
NOTE 5—Caution: Refer to practice G151 for full cautionary guidance
otherwise specified, calibration schedule and procedure shall
applicable to all laboratory weathering devices. Additional information on be in accordance with manufacturer’s instructions.
sources of variability and on strategies for addressing variability by design
and data analysis of laboratory accelerated exposure tests is found in 7. Hazards
Guide G141.
7.1 Never look directly at the operating lamps unless
5.2 Variation in results may be expected are possible be-
wearing UV protective eyewear. The apparatus specified in
tween the different methods described in this practice. For
Section 6 shall be constructed so that the operator will not be
example, differences in spectral distribution of the lamps used
exposed to hazardous levels of UV radiation.
and variations in the irradiance for a single type of lamp can
cause significant differences in test results. Therefore, any no 7.2 Discard or recycle lamps in accordance with any rel-
reference to the use of this practice should be made unless evant local ordinances when they are no longer suitable for the
accompanied by a report prepared in accordance with Section tests described.
12 that describes needs to include a reference to the method
used. 8. Test Specimens
5.3 Reproducibility of test results between laboratories has 8.1 The recommended specimen size is a rectangular flat
been shown to be good when the stability of materials is piece 50 by 80 by 4 mm (minimum thickness). This size is
evaluated in terms of performance ranking compared to other adequate for visual or instrumental evaluation. Other specimen
materials or to a control. Therefore, exposure of a similar dimensions may be used by mutual agreement among the
material of known performance (a control) at the same time as parties concerned but exposed surfaces need to be coplanar for
the test materials is strongly recommended. It is recommended most consistent results.

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D4674 − 19
9. Test Conditions (1) Replace the cool white lamps if UVOFF is greater than
or equal to one.
9.1 Conduct exposures in accordance with one of the
following exposure methods. 9.1.1.7 Program the device so that the cool white lamps
9.1.1 Method I: operate continuously and the fluorescent UV lamps are turned
9.1.1.1 Use apparatus conforming to the requirements de- on once per hour for the fraction of time calculated in section
scribed in Annex Annex A1. 9.1.1.6. Continue the exposure for the total time calculated in
section 9.1.1.4.
NOTE 6—For Method I, the contribution of fluorescent UV lamp
radiation to the total UV actinic exposure is adjusted by changing the 9.1.1.8 Reposition the specimens at time intervals equal to
percentage of time the specimens are exposed to the various lamp types. 25 6 5 % of the total time calculated in section 9.1.1.4. Move
9.1.1.2 This method provides for exposure of specimens to specimens just to the right of the center line of the exposure
radiant energy from an array of very high output (VHO) cool area to the position farthest to the right in the exposure area and
white fluorescent lamps plus intermittent radiant energy from move remaining specimens one position to the left. Move
window glass filtered fluorescent UV lamps. The total UV specimens just to the left of the center line of the exposure to
radiant exposure from both sources is calculated by determin- the position farthest to the left in the exposure area and move
ing the total UV irradiance from each type of lamp separately remaining specimens in this half one position to the right.
and calculating the product of the total UV irradiance and 9.1.1.9 Maintain chamber air temperature between 30 and
exposure time in Watt-hours/m2 (W-h/m2). 40°C during the exposure. If the air temperature exceeds 40°C,
9.1.1.3 Place test specimens in the exposure area, leaving at the device must be shut off and the cause for the high
least a 25 mm empty border around the exposure area. temperature corrected before exposures can continue.
9.1.1.4 Run the device with both the cool white and fluo- 9.1.1.10 Conduct exposures for a total time agreed upon by
rescent UV lamps on for at least 20 minutes, then turn off the all interested parties. Periodically remove test and control
fluorescent UV lamps and record the UV irradiance with only specimens for color measurement and relevant physical prop-
the cool white lamps operating (CWE in W/m2, 250-400 nm). erty tests.
Calculate the exposure time required for the desired CWE 9.1.2 Method II:
radiant exposure as follows: 9.1.2.1 Use apparatus conforming to the requirements of
CWH Annex A, but without the fluorescent UV lamps.
CWt 5 (1) 9.1.2.2 Place test specimens in the exposure area, leaving at
CWE
least a 25 mm empty border around the exposure area.
where:
9.1.2.3 Operate the device for at least 20 minutes then
CWt = exposure time for cool white lamps, record the UV irradiance (CWUV, in W/m2, 250-400 nm).
CWH = desired UV radiant exposure for cool white lamps
Calculate the exposure time necessary for the desired cool
alone, and
white UV irradiance exposure in accordance with section
CWE = UV irradiance measured with only with the cool
9.1.1.4.
white lamps operating.
9.1.2.4 Reposition the specimens during the exposure as
9.1.1.5 Run the device with only the fluorescent UV lamps described in section 9.1.1.8.
on and record the UV irradiance (UVE in W/m2, 250-400 nm). 9.1.2.5 Maintain chamber air temperature between 30 and
The UV actinic exposure from the filtered fluorescent UV 40°C during the exposure. If the air temperature exceeds 40°C,
lamps is set at 12 % of the UV actinic exposure for the cool the device must be shut off and the cause for the high
white lamps. Calculate the total operating time for the fluores- temperature corrected before exposures can continue.
cent UV lamps as follows:
9.1.2.6 Conduct exposures for a total time agreed upon by
0.12 3 CWH all interested parties. Periodically remove test and control
UVt 5 (2)
UVE specimens for color measurement and relevant physical prop-
where: erty tests.
UVt = exposure time for fluorescent UV lamps, 9.1.3 Method III:
CWH = desired UV radiant exposure for cool white lamps 9.1.3.1 Use apparatus conforming to the requirements of
alone, and Practice G154 and equipped with F40T12 cool white lamps.
UVE = UV irradiance measured with only with the fluores- Place specimens in the devices, and fill all spaces not used by
cent UV lamps operating. test specimens with blank metal panels. Operate the device
NOTE 7—Although an office environment sees some UV exposure due with lamps on continuously and with the black panel tempera-
to sunlight through window glass, most photodegradation originates from ture controlled at 50 6 3°C.
fluorescent lighting. The 12 % is an estimate of a representative office
environment. 9.1.3.2 Specimen Repositioning—Periodic repositioning of
the specimens during exposure is not necessary if the irradi-
9.1.1.6 Calculate the fraction of time per hour for which the ance at the positions farthest from the center of the specimen
fluorescent UV lamps are turned off (UVOFF) as follows: area is at least 90 % of that measured at the center of the
CWt 2 UVt exposure area. Irradiance uniformity shall be determined in
UVOFF 5 (3)
UVt accordance with Practice G151.

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D4674 − 19
9.1.3.3 Conduct exposures for a total time agreed upon by cover for the purpose of showing the effects of exposure on one
all interested parties. Periodically remove test and control panel. Misleading results may be obtained by using this
specimens for color measurement and relevant physical prop- method, since the masked portion of the specimen is still
erty tests. exposed to temperature and humidity that in many cases will
9.1.4 Method IV: affect results.
9.1.4.1 Use apparatus conforming to the requirements of 10.6 Exposure to Test Conditions—Unless otherwise
Practice G154 and equipped with UVA 351 lamps that comply specified, expose specimens in accordance with one of the
with the requirements of Practice G154. Place specimens in the methods described in Section 9. Maintain these conditions
devices, and fill all spaces not used by test specimens with throughout the exposure. Interruptions to service the apparatus
blank metal panels. Operate the device with lamps on continu- and to inspect specimens shall be minimized.
ously and with the black panel temperature controlled at
50 6 3°C. 10.7 Inspection—If it is necessary to remove a test specimen
9.1.4.2 Specimen Repositioning—Periodic repositioning of for periodic inspection, take care not to handle or disturb the
the specimens during exposure is not necessary if the irradi- test surface. After inspection, the test specimen shall be
ance at the positions farthest from the center of the specimen returned to the test chamber with its test surface in the same
area is at least 90 % of that measured at the center of the orientation as previously tested.
exposure area. Irradiance uniformity shall be determined in 10.8 Apparatus Maintenance—The test apparatus requires
accordance with Practice G151. periodic maintenance to maintain uniform exposure conditions.
9.1.4.3 Conduct exposures for a total time agreed upon by Perform required maintenance and calibration in accordance
all interested parties. Periodically remove test and control with manufacturer’s instructions.
specimens for color measurement and relevant physical prop- 10.9 Color changes initiated by accelerated exposure may
erty tests. continue after removal of the specimens from exposure to
9.1.5 Other exposure conditions may be used as long as the radiation. Unless otherwise specified, evaluate the final color
exact conditions are detailed in the report. Obtain agreement change within 24 hours after the test is completed, preferably
between all concerned parties for the specific exposure cycle less than one hour, to eliminate possible misleading conse-
used. quences of post actinic exposure reaction. (Color change
initiated by accelerated exposure may continue after removal
10. Procedure of specimens from exposure to radiation.)
10.1 Prepare specimens in accordance with relevant stan-
dards and identify each in accordance with Practice G147. 11. Periods of Exposure and Evaluation of Test Results
10.2 Determine which property or properties of the test and 11.1 In most cases, periodic evaluation of test and control
control specimens will be evaluated. If non-destructive tests materials is necessary to determine the variation in magnitude
are used, measure the property or properties on each test and and direction of property change as a function of exposure time
control specimen prior to exposure and after each exposure or radiant exposure.
increment. Use of instrumental measurements is recommended 11.2 The time or radiant exposure necessary to produce a
whenever possible. Retain a supply of unexposed file speci- defined change in a material property can be used to evaluate
mens of all materials evaluated. or rank the stability of materials. This method is preferred over
10.2.1 When destructive tests are used, a separate set of evaluating materials after an arbitrary exposure time or radiant
specimens will be needed for each exposure increment. It is exposure.
recommended that sufficient file specimens be retained so that 11.2.1 Exposure to an arbitrary time or radiant exposure
the property of interest can be determined on unexposed file may be used for the purpose of a specific test if agreed upon
specimens each time the exposed materials are evaluated. between the parties concerned or if required for conformance
to a particular specification. When a single exposure period is
NOTE 8—Since the stability of file specimen may also be time-
dependent, users are cautioned that over prolonged exposure periods, or use, select a time or radiant exposure that will produce the
where small differences in the order of acceptable limits are anticipated, largest performance differences between the test materials or
comparison of exposed to file specimens may not be valid. between the test material and the control material.
10.3 Mounting of Test Specimens—Attach the specimens to 11.2.2 The minimum exposure time used shall be that
the specimen tray or specimen holders in the equipment in such necessary to produce a substantial change in the property of
a manner that the specimens are not subject to any applied interest for the least stable material being evaluated. An
stress. To assure uniform exposure conditions, fill all of the exposure time that produces a significant change in one type of
spaces, using blank panels of corrosion resistant material. material cannot be assumed to be applicable to other types of
materials.
10.4 Evaluation of color and appearance changes of ex- 11.2.3 The relation between time to failure in an exposure
posed materials shall be made based on comparisons to conducted in accordance with this practice and service life in
unexposed specimens of the same material that have been its end use environment requires determination of a valid
stored in the dark. acceleration factor. Do not use arbitrary acceleration factors
10.5 Unless otherwise specified, do not mask or shield relating time in an exposure conducted in accordance with this
Masking or shielding the face of test specimens with an opaque practice and time in its end use environment because they can

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D4674 − 19
give erroneous information. The acceleration factor is material- standard shows how rank correlation was used to compare the between lab
dependent and is only valid if it is based on data from a results for materials tested in accordance with Method I.
NOTE 11—Guide G169 shows examples using analysis of variance to
sufficient number of separate real time and laboratory acceler- compare materials.
ated exposures so that results used to relate times to failure in
each exposure can be analyzed using statistical methods. 12. Report
NOTE 9—An example of a statistical analysis using multiple-laboratory 12.1 The report shall include the following:
and exterior exposures to calculate an acceleration factor is described by 12.1.1 Material identification and source (if known).
Simms4. See Practice G151 for more information and additional cautions 12.1.2 Exposure apparatus type.
about the use of acceleration factors.
12.1.3 Total exposure time, h.
11.3 After each exposure increment, evaluate or rate 12.1.4 Exposure method used (I, II, III or IV).
changes in exposed test specimens in accordance with appli- 12.1.5 Radiant dosage and wavelength in which it was
cable ASTM test methods. measured (CWH for Methods I and II).
11.3.1 For some materials, changes may continue after the 12.1.6 Quantity and types of lamps used.
specimen has been removed from the exposure apparatus. In 12.1.7 For Methods I and II:
such cases, it is best if measurements (visual or instrumental) 12.1.7.1 Initial and final CW Irradiance (CWE)
should be are made within a standardized time period or as 12.1.7.2 Initial and final UV Irradiance (UVE)
agreed upon between the interested parties. The standardized 12.1.7.3 Hours CW Light time (CWt)
time period needs to consider conditioning prior to testing. 12.1.7.4 Hours UV Light time (UVt)
11.4 Use of results from exposures conducted in accordance 12.1.7.5 UV off time interval (UVOFF – Method I only)
with this practice in specifications: 12.1.8 Basis for evaluation:
11.4.1 If a standard or specification for general use requires 12.1.8.1 Results from visual or instrumental tests used to
a definite property level after a specific time or radiant evaluate specimens,
exposure in an exposure test conducted in accordance with this 12.1.8.2 Results from visual or instrumental tests used to
practice, base the specified property level on results from evaluate masked areas or file specimens,
round-robin experiments run to determine the test reproduc- 12.1.9 Description of the method used for visual or instru-
ibility from the exposure and property measurement proce- mental analysis of the specimens,
dures. Conduct these round robins in accordance with Practice 12.1.10 If instrumental color measurements are used, the
E691 or Practice D3980 and include a statistically representa- type of equipment and color-difference equation must be
tive sample of all laboratories or organizations who would stated.
normally conduct the exposure and property measurements.
11.4.2 If a standard or specification for use between two or 13. Precision and Bias
three parties require a definite property level after a specific 13.1 Precision
time or radiant exposure in an exposure test conducted in 13.1.1 The repeatability and reproducibility of results ob-
accordance with this practice, base the specified property level tained in exposures conducted in accordance with this practice
on two independent experiments run in each laboratory to will vary with the materials being tested, the material property
determine the reproducibility for the exposure and property being measured, and with the variability in temperature and
measurement process. The reproducibility of the exposure/ irradiance within and between exposure devices. In a round-
property measurement process is then used to determine the robin on Method I conducted in 1986,6 laboratories reported
minimum level of property after the exposure that is mutually color (CIE L, a, b) and ∆E for eight materials. Five replicate
agreeable to all parties. specimens of each material were tested. Seven laboratories
11.4.3 When reproducibility in results from an exposure test participated in the round-robin, but variability in color mea-
conducted in accordance with this practice has not been surement or exposure conditions, or both resulted in data from
established through round-robin testing, specify performance only four laboratories being used for statistical analysis in
requirements for materials in terms of comparison (ranked) to accordance with Practice E691. The precision data for the eight
a control material used. materials tested by the four laboratories is shown in Table 1.
11.4.3.1 Conduct analysis of variance to determine whether 13.1.2 Using the precision data obtained in the round-robin,
any differences between test materials and control materials is two samples of material Aa tested in a single device cannot be
statistically significant. Expose replicates of the test specimen judged to be different (at a 95 % confidence level) unless the
and the control specimen so that statistically significant per- ∆E between the unexposed and exposed specimens differs by
formance differences can be determined. more than 0.59. Similarly, two samples of material Aa tested in
different laboratories unless the ∆E difference is larger than
NOTE 10—Fischer illustrates use of rank comparison between test and
control materials in specifications.5 The precision and bias section of this 1.05 units. The reproducibility data in Table 1 show how the
precision varies with material and the tolerances needed to
account for variability in exposure and property measurement.
4
Simms, J.A., Journal of Coatings Technology, Vol. 50, 1987, pp. 45–53. The variability shown in this round-robin studies restricts the
5
Fischer, R., Ketola, W., “Impact of Research on Development of ASTM
Durability Testing Standards,” Durability Testing of Non-Metallic Materials, ASTM
6
STP 1294, Robert Herling, ed., American Society for Testing and Materials, Supporting data have been filed at ASTM International Headquarters and may
Philadelphia 1995. be obtained by requesting Research Report RR: D20–1135.

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D4674 − 19
TABLE 1 Precision Data for ∆E of Eight Materials Exposed for Time T100 in Round-Robin Exposures Conducted in Accordance with
Method I of This Practice
Material Average Repeatability Reproducibility Repeatability Reproducibility
∆E Standard Standard Limit Limit
Deviation Deviation
Aa 1.99 0.21 0.37 0.59 1.05
Ab 1.61 0.11 0.42 0.31 1.19
Ba 1.53 0.10 0.17 0.28 0.48
Bb 0.39 0.08 0.19 0.23 0.54
Ca 9.25 0.30 1.24 0.85 3.51
Cb 1.07 0.29 0.44 0.82 1.25
Da 3.63 0.25 0.83 0.71 2.35
Db 0.33 0.07 0.26 0.20 0.74

TABLE 2 Average ∆E for Five Replicates of Each Material Exposed to Time T100 in Accordance to Method I Reported by Laboratories
Participating in Round-Robin on This Practice
Material Lab 1 Lab 2 Lab3 Lab 4 Lab 5 Lab 6 Lab 7 Lab Ave
Aa 2.36 1.88 3.66 1.67 1.29 2.14 1.77 2.11
Ab 1.73 1.54 2.14 1.32 1.20 1.26 1.86 1.58
Ba 1.64 1.66 1.33 1.45 1.77 1.45 1.64 1.56
Bb 1.56 0.28 1.22 1.69 0.25 0.11 1.12 0.47
Ca 9.94 9.96 10.81 8.46 8.40 7.49 8.83 9.13
Cb 1.16 0.96 1.38 0.79 0.93 0.59 1.55 1.05
Da 4.35 4.80 4.57 3.12 3.28 3.38 2.74 3.75
Db 0.71 0.20 0.70 0.26 0.35 0.15 0.60 0.42

TABLE 3 Rank Order for Eight Materials Based on ∆E Obtained in Exposure in Accordance with Method I of This Practice (1 = Smallest
∆E, 8 = Largest ∆E)
Material Lab 1 Lab 2 Lab3 Lab4 Lab 5 Lab 6 Lab 7 Lab Ave
Aa 6 6 6 6 5 6 5 6
Ab 5 4 5 4 4 4 6 5
Ba 4 5 3 5 6 5 4 4
Bb 1 2 2 1 1 1 2 2
Ca 8 8 8 8 8 8 8 8
Cb 3 3 4 3 3 3 3 3
Da 7 7 7 7 7 7 7 7
Db 2 1 1 2 2 2 1 1

TABLE 4 Rank Correlation Coefficients between Individual Labs and between a Lab and the Rank Based on Average ∆E for All Labs
Lab 1 Lab 2 Lab3 Lab4 Lab 5 Lab 6 Lab 7 Lab Ave
Lab 1 1.0000 0.9995 0.9995 0.9997 0.9992 0.9997 0.9995 0.9997
Lab 2 0.9995 1.0000 0.9992 0.9997 0.9995 0.9997 0.9992 0.9997
Lab 3 0.9995 0.9992 1.0000 0.9990 0.9982 0.9990 0.9995 0.9997
Lab 4 0.9997 0.9997 0.9990 1.0000 0.9997 1.0000 0.9990 0.9995
Lab 5 0.9992 0.9995 0.9982 0.9997 1.0000 0.9997 0.9987 0.9990
Lab 6 0.9997 0.9997 0.9990 1.0000 0.9997 1.0000 0.9990 0.9995
Lab 7 0.9995 0.9992 0.9995 0.9990 0.9987 0.9990 1.0000 0.9997
Lab Ave 0.9997 0.9997 0.9997 0.9995 0.9990 0.9995 0.9997 1.0000

use of “absolute standards” such as requiring a specific rank ordering based on the average ∆E and Table 4 shows the
property level after a specific exposure period. rank correlation coefficients between individual labs for each
13.1.3 The same round-robin study demonstrated that the lab compared to the average for all labs.
∆E values for the eight materials could be ranked with a high
level of reproducibility between laboratories. Table 2 shows 13.2 Bias
the average ∆E for the eight materials reported by the seven 13.2.1 Bias cannot be determined because no acceptable
labs that participated in the round-robin. Table 3 shows the standard weathering reference materials are available.

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ANNEXES

(Mandatory Information)

A1. REQUIREMENTS FOR APPARATUS USED FOR METHODS I AND II

A1.1 The interior of the test chamber shall be constructed NOTE A1.1—Typical spectral power distributions for the UVA-340 and
using UV reflective aluminum with a clear chromate or UVB-313 lamps filtered by window glass can be found in Appendix X1 of
non-chrome conversion coating. Practice G154.

A1.2 The test chamber shall consist of a flat area used for A1.4 The specimen table shall have the same reflecting
exposure of specimens and an arched “roof” on which are surface as the lamp reflector. It shall have a vertical adjustment
placed 1500 mA F48T12/CW/VHO cool white fluorescent to control specimen-to-lamp distance.
lamps. The arched roof shall contain two apertures where 430 A1.5 The apparatus shall include a properly calibrated
mA fluorescent UV lamps are placed behind a soda lime glass
radiometer to measure irradiance at the center of the exposure
filter that is 2.4 6 0.2 mm thick.
area. The radiometer shall be capable of recording irradiance
A1.3 The apparatus shall be equipped with timing devices between 250 and 400 nm with appropriate cosine response.
and timing meters to control on time for the 1500 mA cool
white and 430 mA fluorescent UV lamps and to record the total A1.6 The apparatus shall be equipped with fans or other
operating time for each type of lamp. The spectral power means of cooling to maintain air temperature in the exposure
distribution of the fluorescent UV lamps shall conform to the chamber between 30 and 40°C while the apparatus is operat-
requirements of the UVA-340 or UVB 313 lamps given in ing. The apparatus shall be equipped with a thermostatic sensor
Practice G154. Fig. A1.1 shows a typical instrument configu- that will cause lamps to turn off if the upper temperature limit
ration. The dimensions shown produce a configuration where within the exposure area is exceeded.
irradiance uniformity within the exposure area meets the
requirements of Practice G151. Other configurations and di-
mensions can be used if uniform conditions can be achieved.

FIG. A1.1 Cross Section Diagram of Representative Test Apparatus for Methods I and II.

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A2. SPECTRAL POWER DISTRIBUTIONS AND TABULAR DATA FOR FLUORESCENT COOL WHITE LAMPS

A2.1 Spectral Irradiance of Cool White Fluorescent


Lamps—The spectral power distribution of cool white
fluorescent lamps shall comply with the requirements specified
in Table A2.1.

TABLE A2.1 Specification for Cool White Lamps (Irradiance Expressed as a Percent of Integrated Irradiance from 300-400 nm or from
300-700 nm)
(nm) minimum maximum
As percent of 300–400 nm irradiance
<300 0.0 % 1.4 %
300–320 4.0 % 28.0 %
321–360 0.0 % 14.0 %
361–400 65.0 % 90.0 %
As percent of 300–700 nm irradiance
300–400 0.0 % 5.0 %
401–700 94.0 % 100.0 %

NOTE 1—The sum of the percentages given in the “minimum” and “maximum” will not necessarily add up to 100 % because they represent limits based
on measurements made on a number of different cool white lamps. However, the data for any individual lamp will add up to 100 %.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4726 − 18 An American National Standard

Standard Specification for


Rigid Poly(Vinyl Chloride) (PVC) Exterior-Profile Extrusions
Used for Assembled Windows and Doors1
This standard is issued under the fixed designation D4726; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* environmental practices and determine the applicability of


1.1 This specification establishes requirements for the ma- regulatory limitations prior to use.
terial properties, including dimensional stability, 1.8 This international standard was developed in accor-
weatherability, and extrusion quality, of rigid poly(vinyl chlo- dance with internationally recognized principles on standard-
ride) (PVC) exterior profile extrusions used for assembled ization established in the Decision on Principles for the
windows and doors. Methods for testing and for identifying Development of International Standards, Guides and Recom-
exterior profile extrusions that comply with this specification mendations issued by the World Trade Organization Technical
are also provided. Barriers to Trade (TBT) Committee.
1.2 The use of rigid PVC recycled plastic in this product 2. Referenced Documents
shall be in accordance with the requirements in Section 6. 2.1 ASTM Standards:2
NOTE 1—Information with regard to application, assembly, and instal- D618 Practice for Conditioning Plastics for Testing
lation should be obtained from the manufacturers of the profiles and of the D883 Terminology Relating to Plastics
windows and doors. D1042 Test Method for Linear Dimensional Changes of
NOTE 2—Refer to Specification D3678 for interior profile extrusions.
Plastics Caused by Exposure to Heat and Moisture
1.3 Color-hold guidelines are provided in an appendix for D1435 Practice for Outdoor Weathering of Plastics
the manufacturer’s product development and quality perfor- D1600 Terminology for Abbreviated Terms Relating to Plas-
mance use. tics
1.4 Color-hold guidelines are presently limited to white, D2244 Practice for Calculation of Color Tolerances and
grey, beige, light brown, and dark brown (see Figs. X1.1 Color Differences from Instrumentally Measured Color
through X1.5). Additional colors will be added as color Coordinates
guidelines are developed. D3678 Specification for Rigid Poly(Vinyl Chloride) (PVC)
Interior-Profile Extrusions
1.5 The values stated in inch-pound units are to be regarded
D3892 Practice for Packaging/Packing of Plastics
as standard. The values given in parentheses are for informa-
D4216 Specification for Rigid Poly(Vinyl Chloride) (PVC)
tion only.
and Related PVC and Chlorinated Poly(Vinyl Chloride)
NOTE 3—There is no known ISO equivalent to this standard. (CPVC) Building Products Compounds
1.6 The text of this standard references notes and footnotes, D4226 Test Methods for Impact Resistance of Rigid Poly-
which provide explanatory material. These notes and footnotes (Vinyl Chloride) (PVC) Building Products
(excluding those in tables and figures) shall not be considered E631 Terminology of Building Constructions
as requirements of this standard. E805 Practice for Identification of Instrumental Methods of
Color or Color-Difference Measurement of Materials
1.7 The following safety hazards caveat pertains only to the
G147 Practice for Conditioning and Handling of Nonmetal-
test methods portion, Section 11, of this specification: This
lic Materials for Natural and Artificial Weathering Tests
standard does not purport to address all of the safety concerns,
if any, associated with its use. It is the responsibility of the user 3. Terminology
of this standard to establish appropriate safety, health, and
3.1 General—Definitions are in accordance with Terminolo-
gies D883 or E631 and D1600, unless otherwise indicated.
1
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.24 on Plastic Building
2
Products. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Aug. 1, 2018. Published September 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1987. Last previous edition approved in 2015 as D4726 – 15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4726-18. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D4726 − 18
3.2 Definitions of Terms Specific to This Standard: (Section 3), Materials and Manufacture (Section 6), Physical
3.2.1 color-hold guidelines—target color regions within a Requirements (Section 7), and Performance Requirements
three-dimensional model which constitute acceptable appear- (Section 8) are met by the extrusions containing PVC recycled
ance retention levels of color change resulting from weathering plastic.
of a specific product type and color.
6.3 The PVC compound in the extruded section shall have
3.2.2 temperate northern climate—in weather testing, a visual uniform color and be free of any visual surface or
North American metropolitan area testing site located within structural changes, such as peeling, chipping, cracking, flaking,
73 to 100° W longitude and 37 to 45° N latitude. or pitting.
4. Classification 6.4 Rework Material—Clean, homogeneous PVC rework
4.1 Color Regions—The color region for a color is deter- material or rework material containing PVC capstock gener-
mined by measuring the Hunter L, a, b color values for a ated from the manufacturer’s own production of the same class
sample. Use the integer value (by truncating any fractional compound is acceptable for use by the same manufacturer
results) to determine the color region for the color using the providing that the extruded profiles meet all the requirements
following region boundaries. of this specification. Clean principally PVC rework material
4.1.1 Region 1—Beige: containing non-PVC capstock is acceptable for use in the
substrate of a capstocked product by the same manufacturer,
L = 60 to 87
a = –2.5 to 4.0 providing that the extruded profiles meet all of the require-
b = 6.5 to 23 ments of this specification.
4.1.2 Region 2—Dark Brown: 6.5 The PVC compound shall have successfully met the
L = 13 to 33 weathering requirements for six months at each climatic testing
a = –1.0 to 6.0
b = 1.0 to 6.5
site prescribed in A1.1.1 prior to use in production of exterior-
profile extrusions for either market development or sales.
4.1.3 Region 3—Gray:
L = 33 to 74 NOTE 6—The six-month-test requirement constitutes a screening pro-
a = –3 to 4 cess to eliminate catastrophic failure in the marketplace.
b = –5.5 to 5.5
4.1.4 Region 4—Light Brown: 7. Physical Requirements
L = 30 to 60 7.1 Dimensions—The size, thickness, and dimensional tol-
a = –1.5 to 12.5
b = 3.0 to 12.5
erances of the exterior profiles shall be as agreed upon between
the supplier and the purchaser in the purchase order, or by
4.1.5 Region 5—White:
established internal process control standards.
L = 83 to 100
a = –4 to 0 7.2 Dimensional Stability—The dimensional stability of the
b = –5.5 to +5.5 exterior-profile extrusions shall be determined in accordance
NOTE 4—L, a, b is determined in accordance with the Hunter L, a, b with 11.3. Extrusions over 0.040 in. (1.02 mm) shall have a
opponent color space system in Test Method D2244. maximum average shrinkage of 2.2 % for all sides measured,
5. Significance and Use with no single value exceeding 2.4 %. Extrusions of 0.040 in.
(1.02 mm) or less shall have a maximum average shrinkage of
5.1 The purpose of this specification is to establish a 3 %.
recognized standard of quality for rigid poly(vinyl chloride)
(PVC) exterior weatherable profile extrusions for use in 7.3 Impact Resistance—Flat sections of the exterior profile
assembling windows and doors. The information contained in extrusion shall have a minimum brittle impact failure of 1.0
this specification is intended to be helpful to producers, in.·lb/mil (4450 J/m) when tested in accordance with Test
distributors, and users, and to promote understanding between Methods D4226, Procedure B, using impactor C.125. Refer to
buyers and sellers. It is also intended to serve as the basis for 11.4.
specification requirements of exterior windows and doors
which are made from rigid PVC profile extrusions in their 8. Performance Requirements
construction. 8.1 Weathering:
6. Materials and Manufacture 8.1.1 The exposures listed in Annex A1 shall be conducted
in order to meet the requirements of this specification. All
6.1 The profile extrusions used for assembled windows and
exposures shall be conducted at an angle of 45° S, plywood-
doors shall be made principally of weatherable, rigid poly(vi-
backed, in accordance with Practice D1435 and Practice G147.
nyl chloride) (PVC) compounds meeting or exceeding the
requirements of Class 1-20131-13 as defined in Specification 8.1.2 After six-month and 1-year exposure times, the mini-
D4216. mum mean impact for 20 measurements conducted on the
exposed specimens shall be at least 0.6 in·lb/mil (2670 J/m).
NOTE 5—Non-PVC materials may be used as a capstock. Test impact in accordance with 11.4, A1.4, and A1.5.
6.2 Rigid PVC recycled plastic is acceptable for use in this 8.1.3 After each exposure time, the tested specimens shall
product if all the requirements in the sections on Terminology maintain a visual uniform color and be free of any visual

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D4726 − 18
changes in appearance at the surface, such as peeling, chipping, 11.2 Conditioning of Specimens—Condition the test speci-
cracking, flaking, and pitting when tested in accordance with mens in accordance with Procedure A of Practice D618. For the
Annex A1. purpose of quality control testing, the minimum conditioning
NOTE 7—It is recommended that manufacturers use the color-hold
time shall be four hours.
guidelines in Appendix X1 to ensure quality performance. 11.3 Dimensional Stability:
8.1.4 Weatherability conformance testing requirements are 11.3.1 Determine the dimensional stability in accordance
to reflect performance of a “typical” extrusion system profile with Test Method D1042, except that one or more specimens
representing a specific PVC compound and a specific extrusion shall be exposed to either of the following test cycles:
technology. In no case is there an implied requirement for 11.3.1.1 30 min immersed in water maintained at 180 6 2°F
testing all the various shaped profiles. The lengthy outdoor (82 6 1 °C), or
weatherability testing shall be performed concurrently with 11.3.1.2 30 min conditioned in a forced-ventilation oven at
market development of new applications and sales of profiles 180 6 2°F (82 6 1 °C).
to existing markets. Completion of weatherability testing prior 11.3.2 Specimens shall condition for no less than 1 h in
to marketing of the product is not required. The profile accordance with Procedure A of Practice D618, prior to
extrusion producer shall immediately respond in terms of measurement. If a specimen were to fail, select and retest two
compound change or extrusion technology change to unsatis- additional specimens.
factory weatherability behavior of the profiles under test in any 11.4 Impact Test—Determine the impact strength in accor-
climatic test site at any stage of the weatherability testing. dance with Test Methods D4226, Procedure B, using the C.125
impactor.
9. Workmanship, Finish, and Appearance
12. Packing, Packaging, and Package Marking
9.1 The extrusions shall meet internal process control stan-
dards in section, color, and finish. The extrusions shall be 12.1 The exterior profile extrusions shall be packaged in
substantially straight and free from defects that might affect such a manner as to provide reasonable protection against
appearance or serviceability. damage in ordinary handling, transportation, and storage.
12.2 Provisions of Practice D3892 shall apply to this speci-
10. Sampling fication.
10.1 Select samples using a statistically acceptable proce- 12.3 Marking on each package of extruded profile extru-
dure. The samples shall be representative of the compound sions shall include the following:
used. 12.3.1 Manufacturer’s name or trademark;
12.3.2 Identity of code number of extrusion profiles;
11. Test Methods
12.3.3 Class of compound (Specification D4216) used in
11.1 General—Use the inspection and test procedures con- profiles;
tained in this section to determine the conformance of products 12.3.4 The designation ASTM D4726, affirming that the
to the requirements of this specification. A producer or dis- product so marked has been qualified to all the provisions of
tributor representing products as conforming to this specifica- this specification, and
tion shall use statistically based sampling plans that are 12.3.5 The date and any other relevant information, such as
appropriate to each manufacturing process. Keeping essential factory, machine, production shift, and so forth, either directly
records are necessary to document with a high degree of or all or partly coded.
assurance the claim that all of the requirements of this
specification have been met. Additional sampling and testing of 13. Keywords
the product, as agreed upon between the supplier and the 13.1 color-hold guidelines; doors; exterior-profile extru-
purchaser, is not precluded by this section. sions; poly(vinyl chloride) (PVC); recycled plastic; windows

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D4726 − 18
ANNEXES

(Mandatory Information)

A1. WEATHERABILITY PROCEDURE

A1.1 Summary of Procedure of Determining A1.3.3 The number of specimens or the size of the specimen
Weatherability must be sufficient to obtain at least 20 impact locations of the
A1.1.1 Flat section specimens cut from finished product dropped dart for each weathering interval.
lineals or laboratory extruded samples are exposed in accor- A1.3.4 The thickness of any test specimen must differ from
dance with Practice D1435 and Practice G147 at 45° S, the average test specimen by no more than 10 %.
plywood-backed, in a hot, dry (desert) climate; a hot, humid
climate; and in a northern temperate climate for periods of six A1.4 Conditioning
months, one year and two years. A1.4.1 Condition the test specimens, including specimens
A1.1.2 Degree of retention of the original impact strength removed from the weather exposure, at 73.4 6 3.6°F (23.0 6
due to weather exposure in each exposure site is measured after 2.0 °C) and 50 6 10 % relative humidity for not less than 24 h
six-months and one-year exposure. before testing. In no case shall weathered specimens be
oven-dried before testing.
A1.1.3 The acceptability of color uniformity, and surface
changes resulting from weathering at each test site and each NOTE A1.2—The operational fluctuations are allowable deviations from
the specified temperature and relative humidity settings. They do not
exposure frequency is determined by visual observation in
imply that these settings can be higher or lower than that specified. If the
comparison to the unexposed specimens. operational fluctuations are greater than the maximum allowed, correct the
cause of the problem before continuing the conditioning.
A1.2 Significance
A1.2.1 The processing of poly(vinyl chloride) (PVC) com- A1.5 Procedure
pounds has influence on impact retention and some influence A1.5.1 Obtain test specimens in accordance with A1.3.
on appearance retention. For this reason samples prepared for A1.5.2 Measure the impact resistance on an unexposed
impact retention must be processed in a manner similar to the specimen in accordance with Test Methods D4226, Procedure
commercial product while still permitting the use of laboratory B, with a C.125 impactor and record permanently.
scale equipment.
A1.5.3 Mark the specimens permanently so as to not lose
NOTE A1.1—It is recommended that manufacturers use the color-hold their identity during weathering. Weather specimens at 45°S,
guidelines in Appendix X1 to ensure quality performance.
plywood-backed, in accordance with Practice D1435 in both a
A1.2.2 Poly(vinyl chloride) compounds undergo complex dry/hot and hot/humid, and northern temperate climate zones.
changes when exposed to the weather. Changes in appearance Remove specimens for testing after six-months, one-year, and
are caused by chemical changes in the PVC, additives, or two-year exposure. Further testing is optional. More frequent
pigments. Changes in appearance are caused by selective exposure increments are preferred to some applications.
erosion of some pigments faster than others. Changes in impact
A1.5.4 After exposure, evaluate the appearance of the
strength are due to chemical changes in the PVC or additives,
exposed specimens.
or due to physical changes on the surface as a result of erosion
and crazing. NOTE A1.3—Additional color development is known to occur for PVC
products after removal from exposure to solar radiation. This change in
A1.3 Sampling and Specimen Preparation appearance is referred to as “Dark Time Yellowing.” For two locations
representing hot/humid and northern temperate climate zones, visual color
A1.3.1 Select samples using a statistically acceptable pro- comparisons within 48 h of removal is strongly recommended for PVC
cedure. The samples shall be representative of the product to be products. For a hot/dry climate zone, it is strongly recommended the
qualified. visual color comparison be made within 8 h of removal from the exposure
rack.
A1.3.2 If commercial parts are used, cut them into sections
so that flat test specimens at least 1.5 in. (38 mm) wide can be A1.5.5 Wash the exposed specimens in accordance with the
obtained. The back surface of the specimen must lay as flat as procedure in Annex A2.
possible on the specimen support anvil. Cut the flat sections A1.5.6 Condition in accordance with A1.4.
such that there are no ridges or raised areas remaining on the A1.5.7 The acceptability of color uniformity, and surface or
back surface of the specimen that would make contact with the structural changes resulting from weathering at each test site
specimen support anvil. The specimens shall be free of obvious and each exposure frequency is determined by visual observa-
imperfections, grooves, ribs, and so forth. Material prepared in tion in comparison to the unexposed specimens.
the laboratory by a similar process is an alternate to a
commercial part. If the commercial product is extruded, the A1.5.8 Note and record any nonuniform change in color.
laboratory specimen must be extruded; if the commercial A1.5.9 Measure average impact resistance of the weathered
product is a laminate of two materials, the laboratory specimen specimens, weathered side up, using the same method used for
must be laminated with the two materials, and so forth. the unexposed specimen (A1.5.2).

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D4726 − 18

A2. WASHING WEATHERED SPECIMENS

A2.1 Scope A2.3.2 Wash the specimen lightly with mild detergent using
a sponge or soft cloth.
A2.1.1 This procedure provides a consistent and reproduc-
A2.3.2.1 The scrubbing action shall not be excessive and
ible practice for washing weathered specimens. The procedure shall be limited to back and forth scrubbing along the grain or
is designed to minimize any effects of altering the surface of pattern, if one exists.
the specimen in other than a predictable manner. A2.3.2.2 Avoid circular scrubbing.
A2.2 Equipment A2.3.3 Evaluate specimen visually to determine if the
specimen is “soil free.”
A2.2.1 Mild Detergent.
A2.3.4 If not “soil free,” lightly wipe the specimen once
A2.2.2 Sponge or Soft Cloth. over the surface with a “sopping wet” sponge in the direction
of the grain or pattern, if one exists.
A2.3 Procedure
A2.3.5 Reflush the specimen with distilled or deionized
A2.3.1 Flush the exposed specimen with distilled or deion- water and dry in a vertical position, placed so that water will
ized water. run off with the grain or pattern, if one exists.

APPENDIX

(Nonmandatory Information)

X1. COLOR-HOLD GUIDELINES WEATHERING TEST

X1.1 Scope NOTE X1.1—Five color regions are presently defined as specific
color-hold guidelines.
X1.1.1 Color-hold guideline weatherability testing provides
a method for estimating the acceptability of color change in a X1.2.3 Color-hold guidelines are unique and specific to a
window and door profile product over an extended period of product application, such as window and door profiles and may
service. Changes in appearance are caused by chemical not be transposable for use on other product applications.
changes in the PVC, additives, or pigments. Changes in NOTE X1.2—In any product application, color-hold guidelines are
appearance are caused by selective erosion of some pigments related to a perceived acceptable level of color change. Therefore, window
faster than others. and door color-hold guidelines may be acceptable for transposition for
building railings or fence profile applications, but not for siding applica-
X1.1.2 It has been shown that commercial window and door tions.
profile products which demonstrate weathering behavior that
approximates these target guidelines during a two-year test X1.3 Establishing Window and Door Color Regions
program exhibit acceptability for the marketplace in terms of
X1.3.1 The window and door manufacturer’s color panel
changes in appearance.
uses the following steps to establish the window and door color
X1.1.3 These tests are designed for the window and door regions.
manufacturer’s product development and quality performance Step 1—All commercial unexposed window and door profile
use only and are not for regulatory use. colors are divided into rational similar color regions represent-
ing a visibly definable hue (white, beige, dark brown, gray, and
X1.2 Significance and Use
light brown). See Figs. X1.1-X1.5. Each color is then measured
X1.2.1 Color-hold guidelines provide boundary target color in Hunter L, a, b units and plotted in color space.
regions within a three-dimensional model, which constitutes Step 2—The color region itself is then defined by the
acceptable appearance retention levels of color change result- extreme Hunter L, a, b units within the population of colors.
ing from weathering of a specific window or door profile Step 3—Any specific color being evaluated within the color
product type, formulation, and color. region becomes the control for color-difference studies. Refer
X1.2.2 Each color region is defined by the manufacturers of to X1.3.
vinyl window and door profiles as specific color-hold guide- Step 4—Simulated two-year weathered samples for each
lines (see Note X1.1). Regardless of where a specific color falls color region encompassing areas within that region are pre-
within the region, it becomes the control on each of the three pared.
graphs plotting color difference of each manufacturer’s formu- Step 5—A visual examination and rating of each simulated
lation and color. weathered sample is conducted by a panel of window and door

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D4726 − 18

FIG. X1.1 White Color-Hold Guidelines

manufacturers and color specialists to establish a visual aver- Step 7—The final reference ellipses of color-hold guidelines
age rating of limits of acceptability of color change for the for each region are then established by adjustment of the
window and door application. After visual examination, the preliminary data by use of the real world data. Refer to X1.3.
acceptable delta (∆) limits are plotted three dimensionally and The ellipses are then normalized and the mathematical equa-
considered preliminary limits. tions for each set of ellipses are developed.
Step 6—Real world data from two-year weathering studies Step 8—Concurrent with development of the color-hold
in three locations, representing hot/dry, hot/humid, and north- guidelines for each color region, outdoor weathering of all
ern temperate climate zones are then plotted in terms of change commercial window and door profile samples will be contin-
of Hunter L, a, b from the control for each of the colors within ued in three locations, representing hot/dry, hot/humid, and
that region. northern temperate climate zones in a five-year program

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D4726 − 18

FIG. X1.2 Gray Color-Hold Guidelines

followed each five years by a new study, including new colors


and formulations representing current commercial products.

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D4726 − 18

FIG. X1.3 Beige Color-Hold Guidelines

X1.4 Summary of Procedure for Determining Weather- determined by reference to the appropriate color-hold guideline
ing ellipses for that specific color or, as an alternative, by reference
X1.4.1 Flat section specimens cut from finished product to the appropriate color-hold guideline equation for that spe-
window and door profiles are exposed in three locations cific color.
representing hot/dry, hot/humid, and northern temperate cli-
mate zones. X1.5 Sampling and Specimen Preparation
X1.4.2 Color change caused by weather exposure at each X1.5.1 Select samples using a statistically acceptable pro-
exposure site is measured after six months, one year, and two cedure. The samples shall be representative of the window and
years of exposure. door profile product to be qualified.
X1.4.3 The acceptability in the change in color resulting X1.5.2 If commercial parts are to be used, they shall be cut
from weathering at each test site and exposure frequency is into specimens that are flat and are free of any imperfections.

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D4726 − 18

FIG. X1.4 Light Brown Color-Hold Guidelines

Cut a sufficient number of specimens to allow removal of a X1.6 Weathering Practice


specimen at each weathering time interval specified at each
X1.6.1 Prepare test specimens in accordance with X1.5.
testing site, plus retained unexposed specimens. Alternatively,
samples may be washed, measured, and returned to the test X1.6.2 Mark each specimen permanently so as to ensure
site. retention of identity during and after weathering.
X1.5.3 Samples prepared in the laboratory by the same X1.6.3 Measure in replicate the original tristimulus X, Y,
process (extrusion) and melt temperature may be used as an and Z values for each specimen using 2° observer and
alternative to a commercial sample. The laboratory sample Illuminant C, specular components included, in accordance
must be extruded under similar conditions to those used to with Practice E805. Calculate the Hunter L, a, b units in
prepare the commercial product. accordance with the equations in the section on Hunter L, a, b
X1.5.4 The thickness of any test specimen shall be the same Color Space and Color-Difference Equation in Test Method
thickness as the window and door profile commercial product, D2244, using the average of the replicate measurements and
differing from the average test specimen by no more than 10 %. record them in a permanent record.

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D4726 − 18

FIG. X1.5 Dark Brown Color-Hold Guideline

X1.6.4 Weather specimens at an angle of 45° S, plywood- time between exposure and testing. Color measurement shall
backed, in accordance with Practice D1435 in three locations, be completed within seven days after removal from the
representing hot/dry, hot/humid, and northern temperate cli- exposure rack.
mate zones. X1.6.6.1 Additional color development is known to occur
X1.6.5 Remove specimens for testing after six months, one for PVC products after removal from exposure to solar
year, and two years of exposure. radiation. This color change is referred to as “Dark Time
X1.6.6 It is recommended that exposed specimens be evalu- Yellowing.” Weathering locations representing hot/humid and
ated for color characterization at the test site. If this is not northern temperate climate zones, color measurements within
possible, use an expedient shipping procedure to minimize 48 h of removal is strongly recommended for PVC products.

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D4726 − 18
For a hot/dry climate zone, it is strongly recommended the X1.6.14.3 Insert the ∆L, ∆a, and ∆b values into the Gray
color measurement be made within 8 h of removal from the Colorhold Ellipsoid Equation to calculate the ellipsoid value.
exposure rack. Gray Colorhold Ellipsoid:
X1.6.7 Wash the exposed specimens in accordance with the ~ ∆L 2 1.20! 2 ~ ∆a10.15! 2 ~ ∆b 2 0.10! 2
1 1 51 (X1.1)
procedure in Annex A2. ~ 7.30! 2 ~ 1.85! 2 ~ 3.00! 2
X1.6.8 Measure and record the color of the exposed speci-
~ 4.20 2 1.20! 2 ~ 20.2510.15! 2 ~ 20.90 2 0.10! 2
mens in accordance with X1.6.3 after each exposure frequency. 1 1
~ 7.30! 2 ~ 1.85! 2 ~ 3.00! 2
X1.6.9 Calculate and record the change in L, a, b color
coordinates for each specimen exposure frequency by refer- 50.16910.0310.111
ence to the original color (X1.6.3) and the exposed color
50.283
(X1.6.8).
X1.6.10 Note and record any nonuniform change in color The ellipsoid value is less than 1.00, so the outdoor exposure
on any specimen. specimen is within the gray colorhold guideline.
X1.6.11 Determine the acceptability of the change in color X1.7 Color Hold Guideline Equations
resulting from weathering at each test site and exposure X1.7.1 White:
frequency by reference to the appropriate series of color-hold
guideline ellipses for that specific color. The target three- ~ ∆L 2 0.00! 2 ~ ∆a 2 0.00! 2 ~ ∆b 2 3.00! 2
1 1 51 (X1.2)
dimension color space is plotted as guideline ellipses for each ~ 6.00! 2 ~ 2.30! 2 ~ 5.50! 2
color (∆a versus ∆b), (∆a versus ∆L), and (∆b versus ∆L) in X1.7.2 Gray:
Fig. X1.1(a) to 5(c). For example, in the case of white window ~ ∆L 2 1.20! 2 ~ ∆a10.15! 2 ~ ∆b 2 0.10! 2
and door profiles, use Fig. X1.1(a), 1(b), and 1(c). 1 1 51 (X1.3)
~ 7.30! 2 ~ 1.85! 2 ~ 3.00! 2
X1.6.12 Plot the specific change in the color coordinates X1.7.3 Beige:
when compared to the unexposed specimen color coordinates
(X1.6.3) by plotting on each of the guideline ellipses for that ~ ∆L'20.85! 2 ~ ∆a"10.15! 2 ~ ∆b'20.60! 2
1 1 51 (X1.4)
color. To meet the color-hold guidelines, the plotted change in ~ 5.65! 2 ~ 2.65! 2 ~ 5.20! 2
color for ∆a, ∆b, and ∆L will fall essentially within the X1.7.3.1 In order to duplicate the original hand-drawn
acceptance regions in all three color ellipses. ellipses for Beige, two axes rotations were made to the
X1.6.13 Report any deviation and extent of deviation from ellipsoid equation. The ∆b – ∆a plane was rotated –0.50
the target guideline ellipses by ∆a, ∆b, and ∆L for any test site radians, and the ∆L– ∆a plane was rotated –0.30 radians.
and exposure frequency. Report any deviation from uniform X1.7.3.2 To calculate the ellipsoid value for Beige, counter-
color change in any specimen. Report any other appearance rotations of the ∆L, ∆a, and ∆b data must be made. Note that
change in any specimen. ∆a is rotated twice, and ∆a" is used to calculate the ellipsoid
X1.6.13.1 As an alternative to plotting the color change data value.
on the color hold guideline ellipses, the equations for the ∆a'5 ~ ∆b 2 1∆a 2 ! 0.5 ~ sin~ arctan~ ∆a/∆b ! 10.5!!
corresponding guidelines set of ellipses may be used. The X1.7.3.3 Calculations for ∆L', ∆a", and ∆b' used in the
calculations are performed by inserting the delta L, delta a and ellipsoid equation for Beige:
delta b values into the equation and solving for the value on the
∆L' 5 ~ ∆L 2 1∆a' 2 ! 0.5 ~ cos ~ arctan~ ∆a'/∆L ! 10.3!! (X1.5)
left side of the equation. If the left side of the equation is less
than or equal to 1, the product meets the color-hold guidelines. ∆a" 5 ~ ∆L 2 1∆a' 2 ! 0.5 ~ sin ~ arctan~ ∆a'/∆L ! 10.3!! (X1.6)

X1.6.14 An Example of an Ellipsoid Calculation: ∆b' 5 ~ ∆b 2 1∆a 2 ! 0.5 ~ cos ~ arctan~ ∆a/∆b ! 10.5!! (X1.7)
X1.6.14.1 Take an initial color reading of the specimen. X1.7.4 Lt. Brown:
Example: L = 75.25, a = 0.50, b = 2.85 ~ ∆L 2 1.45! 2 ~ ∆a10.45! 2 ~ ∆b 2 0.05! 2
By definition, this specimen is in the Gray Color Region. ~ 5.45! 2
1
~ 3.65! 2
1
~ 3.95! 2
51 (X1.8)
X1.6.14.2 Take a color reading after an outdoor exposure.
Example: L = 79.45, a = 0.25, b = 1.95 X1.7.5 Dk. Brown:
The color difference (exposed - initial) is: ∆L = 4.20, ∆a = ~ ∆L 2 2.05! 2 ~ ∆a 2 0.20! 2 ~ ∆b10.30! 2
1 1 51 (X1.9)
–0.25, ∆b = –0.90 ~ 5.05! 2 ~ 1.90! 2 ~ 2.50! 2

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D4726 − 18
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4726–15)
that may impact the use of this standard. (August 1, 2018)

(1) Deleted D7209 reference in Section 2. (14) Reworded A1.5.4.


(2) Removed D7209 reference in 6.2. (15) Reworded A1.5.5.
(3) Reworded 6.3. (16) Added Note A1.3.
(4) Deleted 6.5 and 6.6. (17) Reworded A1.5.8.
(5) Reworded, removed color reference in 8.1.3. (18) Reworded A2.1.1.
(6) Reworded 9.1. (19) Reworded A2.2.1.
(7) Deleted A1.1.2. (20) Reworded X1.1.1.
(8) Reworded A1.2.1. (21) Added Note X1.3.
(9) Added Note A1.1. (22) Reworded X1.4.1.
(10) Reworded A1.2.2. (23) Reworded X1.6.4.
(11) Reworded A2.2.1. (24) Added X1.6.6.1.
(12) Added Note A1.2. (25) Reworded X1.6.13.
(13) Deleted A1.5.2. (26) Added X1.6.13.1.

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of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4754 − 18

Standard Test Method for


Two-Sided Liquid Extraction of Plastic Materials Using FDA
Migration Cell1
This standard is issued under the fixed designation D4754; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 1.7 Analytical procedures must be available to quantitate


1.1 This test method covers the use of the FDA migration the migrant(s) generated by this test method.
cell in the extraction of components and permits quantitation of 1.8 The values stated in SI units are to be regarded as the
individual migrants from plastic materials by suitable extract- standard.
ing liquids, including liquid foods and food-stimulating sol- 1.9 This standard does not purport to address all of the
vents. safety concerns, if any, associated with its use. It is the
1.2 This test method provides a two-sided, liquid extraction responsibility of the user of this standard to establish appro-
test for plastic materials that can be formed into film, sheet, or priate safety, health, and environmental practices and deter-
disks. mine the applicability of regulatory limitations prior to use.
1.3 This test method has been applied to a variety of Specific hazards statements are given in Section 8.
migrant/polymer systems in contact with numerous foods and NOTE 2—There is no known ISO equivalent to this test method.
food simulants.2 Though most of the migrants examined were 1.10 This international standard was developed in accor-
radiolabeled, the use of the FDA cell has been validated for dance with internationally recognized principles on standard-
migration studies of unlabeled sytrene from polystyrene.3 ization established in the Decision on Principles for the
1.4 This test method has been shown to yield reproducible Development of International Standards, Guides and Recom-
results under the conditions for migration tests requested by the mendations issued by the World Trade Organization Technical
FDA. However, if the data is to be submitted to the FDA, it is Barriers to Trade (TBT) Committee.
suggested that their guidelines be consulted.
2. Referenced Documents
1.5 Because it employs two-sided extraction, this test
method may not be suitable for multi-layered plastics intended 2.1 ASTM Standards:4
for single-sided food contact use. D883 Terminology Relating to Plastics
D1898 Practice for Sampling of Plastics (Withdrawn 1998)5
1.6 The size of the FDA migration cell as described may
E691 Practice for Conducting an Interlaboratory Study to
preclude its use in determining total nonvolatile extractives in
Determine the Precision of a Test Method
some cases.
IEEE/ASTM SI 10 Standard for Use of the International
NOTE 1—For more information, see Practice D1898, the AOAC System of Units (SI): The Modernized Metric System
Methods of Analysis on Flexible Barrier Materials Exposed for
Extraction, and the Guidance for Industry: Preparation of Premarket
2.2 Association of Offıcial Analytical Chemists (AOAC)
Submissions for Food Contact Substances: Chemistry Recommendations, Methods of Analysis:
December 2007. Flexible Barrier Materials Exposed for Extraction6

1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
4
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2018. Published May 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1987. Last previous edition approved in 2011 as D4754 – 11. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4754-18. the ASTM website.
2 5
“A Study of Indirect Food Additive Migration,” Arthur D. Little, Inc., FDA The last approved version of this historical standard is referenced on
Contract No. 223-77-2360. www.astm.org.
3 6
Supporting data have been filed at ASTM International Headquarters and may Available through the Association of Official Analytical Chemists, 481 North
be obtained by requesting Research Report RR:D20-1141. Frederick Avenue, Suite 500, Gaithersburg, Maryland 20877-2417 USA.

*A Summary of Changes section appears at the end of this standard


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D4754 − 18
6.1.1 Glass Vials, 23-mL,
6.1.2 Mininert® Slide Valve Caps,
6.1.3 Stainless Steel Wire (20-gage), and
6.1.4 Glass Bead (5-mm diameter), containing hole slightly
larger than diameter of stainless steel wire.8 (Available at local
hobby shops.)
NOTE 4—The apparatus, disk size, and number of disks are described
for the 23-mL vial. Alternative vial sizes and corresponding test specimen
sizes may be substituted. (The volume-to-surface area ideally should be
between 155 and 0.31 mL/cm2.) Note that validation tests have only been
conducted using the 23-mL vials.
NOTE 5—Recommend one-time use of mininert valve (that is, discard-
ing it at completion of study).
6.2 Hot-Air Oven or Static Thermostatted Water Bath, with
suitable safety provisions and capable of maintaining the
desired extraction temperature within 61°C.
6.3 Thermostatted Shaker Water Bath—Some migrant/
plastic/liquid combinations may involve significant partition-
ing and would benefit by having the cells shaken throughout
FIG. 1 FDA Migration Cell
the migration study.
6.4 Liquid Syringes, for removing liquid aliquots from the
2.3 Federal Document: cells and transferring them to the analytical instrumentation.
Guidance for Industry: Preparation of Premarket Submis- 6.5 Analytical Instrumentation, as required by the method
sions for Food Contact Substances: Chemistry chosen to determine the migrant(s).
Recommendations, December 20077
7. Reagents and Materials
3. Terminology
7.1 Purity of Reagents—All solvents shall be HPLC or
3.1 General—The units, symbols, and abbreviations used in chromatographic grade and shown to be free of interferences in
this test method are in accordance with Terminology D883 and the detection region of the migrant(s).
Practice IEEE/ASTM SI 10.
8. Hazards
4. Summary of Test Method
8.1 The usual safety precautions for handling flammable
4.1 Specimens of plastic materials, formed in the shape of solvents are recommended when such solvents are used for
disks, are threaded onto a stainless steel wire with alternating extraction.
glass bead spacers and placed in a glass vial. Solvent is added
to the vial and the vial is capped and maintained at the desired 9. Sampling
extraction temperature. Aliquots of the liquid are removed at
various times and the migrant(s) in the liquid determined by 9.1 Sample the plastic in accordance with Practice D1898.
suitable analytical methods. 9.2 Select representative samples of the plastic to be tested
from available stock on hand. Film, pellets, powders, sheet,
NOTE 3— Significant migration loss due to volatility may occur if
migration is carried out at temperatures exceeding 50°C for periods and, in some cases, actual end-use articles are suitable. Protect
greater than 2 weeks. the samples from exposure to liquids or contamination by
migration from contact with other materials.
5. Significance and Use
NOTE 6—See RR:D20-1141 for details regarding sample test speci-
5.1 Knowledge of migrants from plastic materials may mens.
serve many useful purposes, such as testing for compliance
with food additive regulations. The procedure described in this 10. Test Specimen
test method is recommended as suitable for obtaining such data 10.1 Test specimens in the form of round disks (11 by 1
on many migrant(s)/plastic(s) combinations. mm) are prepared from the plastic to be tested. Disks can be
stamped out of sheets of actual end-use articles of non-brittle
6. Apparatus plastic by means of the appropriate sized cork borer.
6.1 FDA Migration Cell (Fig. 1), consisting of: Alternatively, disks can be formed by using a heated press and
an appropriate shim or mold containing holes the size of the
disk. Holes can be put in the center of the disk by means of a
7
Available from Division of Food Contact Notifications, Office of Food Additive drill or a heated wire.
Safety, Center for Food Safety and Applied Nutrition, Food and Drug
Administration, College Park, MD 20740, USA. https://www.fda.gov/Food/
GuidanceRegulation/GuidanceDocumentsRegulatoryInformation/
8
IngredientsAdditivesGRASPackaging/ucm081818.htm Glass beads sold at hobby shops have been found satisfactory for this purpose.

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D4754 − 18
NOTE 7—Whenever possible, plastic from actual end-use articles TABLE 1 Precision for Migration of Residual Styrene from
should be tested. Polystyrene
NOTE 8—When actual end-use articles are tested, the cut edges of the Values in ppm
disks may have a different structure than the surfaces, and henceforth the Time, h
Avg SrA SRB rC RD
migration rates may be altered. Because the area of the surfaces is much
greater than that of the cut edges, the effect of the edges would be limited. 4 0.222 0.022 0.11 0.062 0.31
If a significant edge effect is suspected, however, tests can be run 24 0.979 0.080 0.12 0.226 0.34
72 2.282 0.153 0.27 0.433 0.76
comparing disks formed by using a heated press with disks cut from a
168 3.875 0.198 0.46 0.560 1.30
sheet formed under similar conditions. 240 4.790 0.197 0.62 0.558 1.75
336 5.711 0.276 0.82 0.781 2.32
11. Preparation of Apparatus A
Sr = within-laboratory standard deviation of the average,
B
11.1 Alternately thread glass beads and 14 plastic disks onto C
SR = between-laboratories standard deviation of the average,
r = 2.83 Sr, and
the stainless steel wire (see Fig. 1). Prepare at least 4 sets for D
R = 2.83 SR.
each liquid extractant used. Place resulting stacks of disks into
23 mL glass vials. Add 22 mL of extraction liquid and screw
Mininert® caps tightly onto the vials. 13.3 A second way to express the test results is in milli-
11.2 Use the above prepared vials to determine the total grams of migrant(s) per square meter of sample exposed, E, as
amount of migrant(s). follows:
11.3 To calculate migration rates, the samples should be
washed to remove any surface bloom of the migrant(s). E 5 ~ W 2 B ! / @ ~ 2π R 2 1CT! N #
Maintain the above prepared vials at the extraction temperature where:
for 2 h. Discard the liquid in the vials and replenish with fresh W = total weight of migrant(s) in the liquid, mg,
extracting liquid. B = weight of migrant(s) in the blank, mg,
NOTE 9—Depending upon the conditions under which the test speci- R = radius of the disk, m,
mens were prepared, removal of any migrant surface bloom might not be C = circumference of disk, m,
warranted. Under these conditions, simply omit the wash step for T = thickness of disk, m, and
removing migrant surface bloom. N = number of disks per cell.
12. Procedure 13.4 A third and more rigorous way to express the test
results is to calculate diffusion and partition coefficients for the
12.1 Place properly prepared vials in thermostatted oven or
plastic/migrant(s)/liquid system used. These calculations,
bath.
however, are beyond the scope of this test method. A brief
12.2 To prepare standards for quantitating the migration, description is contained in Appendix X1.
place extraction solvent(s) and known quantities of the mi-
grant(s) to be studied in a vial containing the support stand with 14. Report
glass bead spacers. Place these standard vials in the same 14.1 Report the test results, either as concentration of
thermostatted oven or bath. migrant(s) per unit volume of liquid, or concentration of
12.3 To prepare the blank, place only the extraction sol- migrant(s) per square metre of disk area.
vent(s) in a vial containing the support stand with glass bead 15. Precision and Bias3
spacers. Place these blank vials in the same thermostatted oven
or bath. 15.1 Table 1 is based on a round-robin conducted in 1984 in
accordance with Practice E691. Twelve laboratories reported
12.4 At pre-selected times, typically 5 to 8 samplings over results (ppm) for styrene migration from polystyrene disks into
a 2-week period, withdraw µL aliquots from each sample, 50/50 ethanol/water at 49°C. The disks were prepared at one
standard, and blank vial and analyze using selected methodol- source. Five replicate sample cells were then setup by each
ogy. laboratory which conducted the studies. One aliquot was taken
NOTE 10—At each sampling, check to see if cell caps are tight. from each cell at six times over 2 weeks. A test result was
NOTE 11—Volume withdraw is dictated by analytical procedure being obtained from the analysis of each aliquot. Each laboratory
utilized. If aliquots of more than 1 % by volume are removed during reported 30 test results.
samplings, separate vials should be used for each test period.
NOTE 12— The following explanations of Ir and IR (see 15.2) are only
12.5 Use response of standards on each day of analysis to intended to present a meaningful way of considering the approximate
quantitate the migrant(s). precision of this test method. The data in Table 1 should not be rigorously
applied to acceptance or rejection of material, as those data are specific to
13. Calculation the round-robin and may not be representative of other lots, conditions,
materials, or laboratories. Users of this test method should apply the
13.1 The test results can be calculated in a number of ways
principles outlined in Practice E691 to generate data specific to their
depending upon the application of the data. laboratory and materials, or between specific laboratories. The principles
13.2 One simple way to express the test results is to of 15.2 through 15.2.3 would then be valid for such data.
calculate the concentration of the migrant(s) in the liquid at a 15.2 Concept of r and R—Since Sr and SR have been
given time in some unit such as parts per million (ppm) or parts calculated from data produced by 12 laboratories, and for test
per billion (ppb). results that were averages from testing 5 sample cells:

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D4754 − 18
15.2.1 Repeatability, Sr—Precision under repeatability participating laboratories analyzed standards at four different
conditions, represented as Repeatability Standard Deviation. concentrations, six times over the 2-week migration period.
15.2.2 Reproducibility, SR—Precision under reproducibility From the detector response for these four standards, an average
conditions, represented as Reproducibility Standard Deviation. detector response per 1 ppm of styrene was calculated (that is,
15.2.3 Repeatability Limit, r—The value below which the slope of linear least squares fit, forced through origin). The
absolute difference between two individual test results obtained coefficient of variation for the six average detector responses
under repeatability conditions may be expected to occur with a for the 12 laboratories ranged from 0.6 to 9.5 % and averaged
probability of approximately 0.95 (95 %). 4.9 %.
15.2.4 Reproducibility Limit, R—The value below which the 15.4 Bias—There are no recognized standards on which to
absolute difference between two individual test results obtained base an estimate of bias for this test method.
under reproducibility conditions may be expected to occur with
a probability of approximately 0.95 (95 %). 16. Keywords
15.3 The integrity of this cell was evaluated by carrying 16.1 diffusion; food packaging; indirect additives; migration
standards along with the actual migration cells. Each of the 12 cell; migration testing; polymer extraction

APPENDIX

(Nonmandatory Information)

X1. STYRENE DIFFUSION COEFFICIENTS (Dp) IN POLYSTYRENE (49°C)

X1.1 Although slightly beyond the scope of this test TABLE X1.1 Diffusion Coefficients
method, a diffusion coefficient for component migration can be Laboratory Dp × 10 −12
cm/s
calculated from the data obtained. The only additional infor- 1 1.9
2 1.6
mation needed is the component concentration in the polymer 3 1.7
disks. 4 1.5
5 1.9
X1.1.1 Diffusion of a migrant in a polymeric material is 6 1.7
governed by Fick’s Law. In its simplest form, where no 7 1.4
8 1.8
partitioning between the polymer and the solvent in contact 10 3.3
with it occurs, this migration can be expressed by: 11 2.0
16 1.9
Mt 5 2Cp~ DpT/π ! 1/2 19 2.5
avg = 1.9 (1.8 if #10
where: omitted)
Mt = mg/cm2 at time, T, s, CV = 26.6 % (16.3 % if #10
omitted)
Cp = mg/cm3 in polystyrene disks, and
Dp = diffusion coefficient in disks, cm2/s.
X1.1.2 From the slope, m, of a linear, least squares fit of X1.2 Sytrene migration at 49°C was calculated from the
Mt/Cp versus T ⁄ . 12 data reported by the twelve laboratories participating in this
round-robin. The residual styrene concentration in the polysty-
X1.1.3 Dp can be calculated as follows: rene disks was determined by HPLC analysis to be 2348 ppm
Dp 5 π ~ m/2 ! 2 (n = 4, CV = 3.6 %). The Dp values are given in Table X1.1.

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SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D4754 – 11) that may impact the use of this standard. (May 1, 2018)

(1) Added government document web address.


(2) Removed footnotes 8 and 10 since products are now
available from a wider range of suppliers.

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4756 − 15 An American National Standard

Standard Practice for


Installation of Rigid Poly(Vinyl Chloride) (PVC) Siding and
Soffit1
This standard is issued under the fixed designation D4756; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D3679 Specification for Rigid Poly(Vinyl Chloride) (PVC)


1.1 This practice covers the basic requirements for and the Siding
methods of installation of rigid vinyl siding, soffits, and D4477 Specification for Rigid (Unplasticized) Poly(Vinyl
accessories on the exterior wall and soffit areas of buildings. In Chloride) (PVC) Soffit
all applications, refer also to the specific manufacturer’s E631 Terminology of Building Constructions
installation instructions and the requirements of applicable E2112 Practice for Installation of Exterior Windows, Doors
building codes. and Skylights
1.2 This practice covers aspects of installation relating to 3. Terminology
effectiveness and durability in service.
3.1 General—Definitions are in accordance with Terminolo-
1.3 The various application systems are located in the
gies D883 and E631 and abbreviations with Terminology
following sections of this practice:
D1600 unless otherwise indicated.
Substrate, Surface Preparation Section 8
Application of Horizontal Siding Section 9 3.2 Definitions of Terms Specific to This Standard:
Application of Vertical Siding Section 10 3.2.1 backerboard—a flat material used on the face of the
Application of Soffits and Fascia Section 11
Special Details Section 12 house, applied between the studs and the siding (or over
existing wall surface) to provide an even surface for the
1.4 The values stated in inch-pound units are to be regarded
installation of the vinyl siding.
as standard. The values given in parentheses are mathematical
conversions to SI units that are provided for information only 3.2.2 buttlock—the bottom of a siding or soffit panel, or
and are not considered standard. accessory piece, opposite the nail hem, which locks onto the
1.5 This standard does not purport to address all of the preceding panel.
safety concerns, if any, associated with its use. It is the 3.2.3 crimp—small protrusions, typically approximately 1⁄2
responsibility of the user of this standard to establish appro- in. (12.7 mm) long, 1⁄8 in. (3.2 mm) wide, and projecting 1⁄8 in.
priate safety and health practices and determine the applica- (3.2 mm) formed by a crimper (snaplock punch). (See Fig. 2.)
bility of regulatory limitations prior to use.
3.2.4 crimper—a special hand tool designed to form crimps
NOTE 1—There is no known ISO equivalent to this standard. (snaplock ears) intended to hold partial panels in place. (See
Fig. 2.)
2. Referenced Documents
3.2.5 face nail—the action of fastening directly on to the
2.1 ASTM Standards:2 “face,” or exposed surface, of a panel (instead of using the nail
D883 Terminology Relating to Plastics slot).
D1600 Terminology for Abbreviated Terms Relating to Plas-
3.2.6 fascia—the trim covering the ends of roof rafters. (See
tics
Fig. 1.)
3.2.6.1 fascia board—a board attached to the ends of the
1
rafters between the roofing material and the soffit overhang.
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and
is the direct responsibility of Subcommittee D20.24 on Plastic Building Products. 3.2.6.2 fascia cap or cover—the covering around a fascia
Current edition approved Feb. 1, 2015. Published February 2015. Originally board.
approved in 1991. Last previous edition approved in 2013 as D4745 – 13. DOI:
10.1520/D4756-15.
2
3.2.7 flashing—special membrane pieces or manufactured
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
trim pieces used to supplement siding panels in weather
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on protection around joints, penetrations, and openings, such as
the ASTM website. windows, doors, mechanical penetrations, and roof-wall

*A Summary of Changes section appears at the end of this standard


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D4756 − 15

FIG. 1 Terminology for Buildings, Siding and Accessories

3.2.10 rake (roof)—the inclined, usually projecting edge of


a sloping roof.
3.2.11 rake (wall)—the board or molding placed along the
sloping sides of a gable to cover the ends of the siding.
3.2.12 snaplock ears—see crimp and Fig. 2.
3.2.13 snaplock punch—see crimper and Fig. 2.
3.2.14 soffıt—the underside surface (typically horizontal) of
roof overhangs.
3.2.15 starter strip—an accessory applied directly to the
surface of the building and used to secure the first course of
siding to the home. Starter strips can either be a part manufac-
tured for the specific purpose or created by cutting the nailing
hem and adjacent lock from a siding panel.
3.2.16 undersill trim (utility trim)—an accessory strip used
to receive and hold the crimped edge of horizontal or vertical
siding that has had its normal lock removed.
3.2.17 zip tool (unlocking tool)—a special hand tool used to
separate interlocked siding panels. (See Fig. 2.)

FIG. 2 Siding Installation Tools 4. Delivery of Materials


4.1 All manufactured materials shall be delivered in the
intersections, designed and intended to move incidental water original packages, containers, or bundles bearing the size or
to the building exterior. type product, or both, brand name, and manufacturer (or
3.2.8 furring/furring strip—a wooden or steel framing supplier) identification, manufacturer’s lot number, and the
material, usually a nominal 1 by 2 in. (25.4 by 50.8 mm) used ASTM specification to which it conforms.
to even the surface in preparation for installation of siding. To
“fur” a surface means to apply these strips. 5. Protection of Materials
3.2.9 nailslot punch—a special hand tool used to create slots 5.1 Do not store in any location or in any manner where the
for attachment of field-modified siding or accessories. (See Fig. temperature of the siding, soffit or accessories is likely to
3.) exceed 130°F (54°C).

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D4756 − 15

FIG. 3 Typical Siding Profiles

5.2 Store the cartons on a flat surface and support the entire 7.4.3 Trim Channels—Produced of poly(vinyl chloride) in a
length of the cartons. variety of designs and sizes for use around openings and edges
5.3 Store the cartons away from areas where falling objects of wall and soffit surfaces. (See Fig. 5.)
or other construction activity could impact the cartons. Keep 7.5 Fasteners:
the cartons dry. 7.5.1 Nails—Corrosion-resistant with head diameter 5⁄16 in.
5.4 Do not store the cartons in stacks more than 6 boxes (7.9 mm) minimum, shank diameter 1⁄8 in. (3.2 mm), length
high. sufficient to penetrate not less than 3⁄4 in. (19 mm) into framing
or furring.
6. Environmental Conditions 7.5.2 Staples—Corrosion-resistant, 16 gage minimum, with
3⁄8 to 1⁄2-in. (9.5 to 12.7-mm) crown, length sufficient to
6.1 Vinyl siding and accessories will expand when heated
penetrate not less than 3⁄4 in. (19 mm) into framing or furring.
and contract when cooled. If siding is installed in hot weather
7.5.3 Screws—Corrosion resistant, self-tapping type, No. 8
and the siding is very warm it will be partially “expanded.”
truss head or pan head length sufficient to penetrate wall
Provide allowance for more future “contraction” than expan-
thickness of steel stud or 3⁄4 in. into framing or furring.
sion.
6.2 Leave 1⁄4 in. (6.4 mm) clearance between the ends of NOTE 2—To minimize the possibility of any color variation use material
from a single manufacturer’s lot number for application to one building.
panels and trim and any receiver such as J-channels and corner
posts to allow for thermal expansion. If installing during 8. Substrate, Surface Preparation
weather colder than 40°F (4.4°C), increase the minimum
8.1 Water-resistive Barrier—Vinyl siding must be installed
clearance to 3⁄8 in. (9.5 mm) to allow for additional expansion
over a water-resistive barrier system that includes (1) a
during warmer weather.
continuous water-resistive material, and (2) properly integrated
7. Materials flashing around all penetrations and where vinyl siding inter-
faces with other building products. Refer to the vinyl siding
7.1 Horizontal Wall Siding—See Specification D3679. manufacturer’s installation instructions and the minimum re-
7.2 Vertical Wall Siding—See Specification D3679 quirements of the local building code for specific product
7.3 Soffıt Panels—See Specification D4477. applications and requirements.
7.4 Accessories: 8.2 All caulking to prevent moisture penetration must be
7.4.1 Starter Strip—For horizontal siding made of poly(vi- done before siding application. Do not use caulk where it could
nyl chloride) or corrosion-resistant metal. restrict the normal expansion of the vinyl siding.
7.4.2 Corner Posts—Of two types: for inside corners and for 8.3 Apply vinyl siding over sheathing or other rigid surface
outside corners of poly(vinyl chloride). that provides a smooth, flat surface. Do not apply vinyl siding

FIG. 4 Typical Soffit Profiles

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D4756 − 15
9.1.1 When applied, vinyl siding products must be attached
“loosely,” leaving approximately a 1⁄32-in. (0.8-mm) space
between the vinyl and the fastener head or crown to permit
thermal movement. (See Fig. 6.)
9.1.2 Center fasteners in slots of siding and accessories to
permit possible expansion and contraction. (See Fig. 7.) If a
nail slot does not allow centering/securing into framing,
furring, or other permitted nailable surface, use a nail hole slot
punch to extend the slot and allow centering of the fastener.
9.1.3 Do not face nail siding panels. (See Fig. 8.)
9.1.4 Allow clearance at panel ends for thermal expansion
between corner posts, J-channels, and other receivers in
accordance with 6.2.
9.2 Installation of Accessories—Accessories, including
starter strips, corner posts and door/window trim, are installed
prior to application of the siding, adhering to the provisions of
9.1 and those which follow.
9.2.1 Corner Posts—Outside and inside corner posts will
start 1⁄4 in. (6.4 mm) below the top, and end 3⁄4 in. (19.1 mm)
below the bottom edge of the first course of siding which will
be installed later. Attach each leg of the corner posts with
fasteners, spaced not over 12 in (305 mm) apart centered in
FIG. 5 Typical Siding Accessories
nailing slots except the top fastener that is located at the upper
end of a nailing slot.
9.2.1.1 If more than one length of corner post is required,
directly to studs without sheathing. If permitted by the vinyl lap the upper piece over the lower piece by cutting away 1 in.
siding manufacturer, a contoured foam underlayment fitted for (25.4 mm) of the nailing flange on the top piece. Lap 3⁄4 in. (19
the specific style of vinyl siding is permitted to be utilized. mm) allowing 1⁄4 in. (6.4 mm) for expansion. (See Fig. 9.)
Apply over wood furring strips when the underlying surface is 9.2.1.2 As an alternative for inside corners, install two
uneven. J-channels with the web of one abutting the adjacent wall and
8.4 Drive fasteners into framing or furring. Driving of the web of the other J-channel abutting the shorter outer flange
fasteners directly into sheathing or existing siding is permitted of the first J-channel. Attach as specified in 9.1.1.
in accordance with the siding manufacturer’s instructions, 9.2.2 Starter Strip—Determine the lowest point along the
where substantiated by windload testing conducted in accor- area to receive siding and install starter strips located so that
dance with Specification D3679. the bottom edge of the initial course of siding will be on a level
line and typically approximately 1⁄4 in. (6.4 mm) below that
8.5 On existing structures, secure any loose boards, replace
point. Allow space for corner posts, J-channels, etc., and keep
any rotted ones, recaulk around windows, doors, and other
ends of starter strips 1⁄4 to 1⁄2 in. (6.4 to 12.7 mm) apart. Space
areas as necessary to protect from moisture penetration prior to
fasteners not more than 10 in. (254 mm) apart, centered in nail
the installation of siding or accessories. Use furring as needed
slots.
to create an even surface.
9.2.3 Door/Window Trim:
8.6 Flashing—Refer to Practice E2112 for installation of 9.2.3.1 Install flashing around windows and doors in accor-
flashing around windows, doors, penetrations and points of dance with 8.1 and 8.6 before installing trim.
interface between the vinyl siding and other building compo- 9.2.3.2 J-channel is installed on each side and the top of
nents. If available, also refer to the instructions provided by the door and window frames, and under window sills. Always
manufacturer of the window, door, or other object that will install the bottom J-channel first, followed by the side
penetrate the siding. channels, and then the top channel.
8.7 Furring—Masonry and uneven surfaces, as examples, 9.2.3.3 Extend the bottom and top J-channel the length of
require wood furring strips nominal 1 by 2 in. (25.4 by 50.8 the window frame plus the width of the visible face of the side
mm) applied vertically and typically spaced 16 in. (406 mm)
on center for horizontal siding and applied horizontally and
typically spaced 12 in. (305 mm) on center for vertical siding.

9. Application of Horizontal Siding


9.1 General Requirements—Vinyl siding and accessories
expand and contract as much as 1⁄2 in. (12.7 mm) over a 12 ft
(3.65 m) length with changes in temperature. For this reason
adhere to the following provisions: FIG. 6 Attachment of Vinyl Siding

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D4756 − 15

FIG. 7 Fastening Location in Siding Slots

FIG. 10 Installation of Bottom and Side J-Channels under Win-


dow (for clarity, 45 degree miter of side J-channel is
FIG. 8 Face Nailing of Vinyl Siding Prohibited
not shown)

FIG. 9 Joining Corner Posts

J-channels (typically 3⁄4 in. (19 mm)) on each side. Extend the
side J-channels the height of the window or door frame plus the FIG. 11 Installation of Top and Side J-Channels Above Window
or Door (note mitered face of top J-channel)
width of the visible face of the top and bottom J-channels.
9.2.3.4 In the bottom J-channel, cut a notch in the web at
each end the width of the visible face of the side J-channel. In
both side J-channels, cut a notch at the top end and a tab at the
bottom end. Miter the bottom ends of the visible face of the
side J-channels at a 45 degree angle. In the top J-channel cut
along the bends at both ends of the J-channel to create a tab the
same length as the exposed face of the side J-channel. Miter the
end of the visible face of both ends of the top J-channel at a 45
FIG. 12 Fastening of Initial Siding Panel
degree angle.
9.2.3.5 Install the bottom J-channel. Install each of the side
J-channels, with the mitered visible face over the face of the 9.3.2 Engage the bottom of the first panel and the starter
bottom J-channel. Bend the tabs in the side J-channels into the strip. If backerboard insulation is used, drop it in behind the
bottom J-channel. (See Fig. 10.) panel now. Make sure the panel is locked, but not pulled tight,
9.2.3.6 Install optional head flashing across the top of the and fasten leaving 1⁄4 to 3⁄8 in. (6.4 to 9.5 mm) gap at the corner
window or door frame. Install the top J-channel with the posts, in accordance with 6.2. (See Fig. 12.) Space fasteners
mitered face over the face of the side J-channels. Bend the tabs not over 16 in. (406 mm) on center. Greater spacing is
in the top J-channel into the side J-channels. (See Fig. 11.) permitted in accordance with the siding manufacturer’s
9.3 Siding Panel Installation: instructions, where substantiated by windload testing con-
9.3.1 General Considerations—To make overlapped siding ducted in accordance with Specification D3679.
joints less noticeable on the sides of a building, start at the rear 9.3.3 Lap the next panel over the first by approximately
corner and install toward the front. On the front and rear of one-half of the factory cut notch, provided the overlap is at
buildings start at the corners and install toward the entrance least 3⁄4 in. (25.4 mm) but not greater than 11⁄4 in. (38.1 mm).
door. Avoid use of short panel lengths under 24 in. (610 mm). (See Fig. 13.) Insert backerboard (if used) and fasten.
(See Fig. 13.) When lapping, place factory-cut ends of panels 9.3.4 To field-notch a panel where the factory notch has
on top of field-cut ends for best appearance. been cut off, cut away 11⁄2 in. (38 mm) of the nailing flange and

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D4756 − 15

FIG. 13 Lapping Siding Panel

FIG. 15 Installation of Siding Under Window


lock. Cut a 1⁄8 by 11⁄2-in. (3.2 by 38-mm) notch from the bottom
step of the panel, cutting away the hook on the back as well.
9.3.5 At the bottom of the window, snugly install between
the side J-channels and against the underside of the sill, a piece
of undersill trim cut to the exact width of the window. Use the
proper thickness of furring behind it to keep the pitch of the
panel consistent.
9.3.6 If the top of the siding panel will extend above the
bottom of the window, cut a section out of the panel to fit under
FIG. 16 Installation Over Window or Door
the opening. Be sure the uncut portion of this panel extends on
both sides of the window. Measure the panel to fit. Hold the
siding panel under the window and mark the width of the
opening on it. Allow 1⁄4 in. (6.4 mm) clearance at the edges for
insertion into each side of the J-channel. Measure the space
between the bottom edge of the S-lock on the previous panel
and the top of the undersill trim, minus 1⁄4 in. (6.4 mm) for
insertion into the undersill trim receiver. Remove cut section.
Punch snap locks every 6 in. (152 mm) along the horizontal cut FIG. 17 Installation of J-channel on Gable
edge. Slide the panel up into position so the bottom locks into
the previous panel and the top snaps into the undersill trim and
fasten. (See Figs. 14 and 15.)
9.3.7 Over a window or door, measure for the cuts. Mark the
bottom portion of the panel and cut out the unwanted section.
Install the panel. (See Fig. 16.) If necessary, place a piece of
furring into the J-channel behind the cut edge of the siding to
reduce wind movement and maintain the proper plane of this
siding. Leave enough gap at the top of the cutout to permit
locking onto the previous course.
9.3.8 At a gable, install J-channel along the rake boards, or FIG. 18 Using a Pattern to Match Panel End Cuts to Gable Angle
at the top of the wall if there are no rake boards. (See Fig. 17.)
Lap the channels if necessary by cutting 1 in. (25.4 mm) off the
end leaving only the face and then lap 3⁄4 in. (19 mm). Miter the 9.3.8.1 To ensure that the angle of the ends of the siding
ends that meet at the peak to make a neat joint. panels match the angle of the gable, make a pattern from two
pieces of scrap siding. Hold one piece on the lock of the last
installed panel, place the other piece against the gable and
mark the horizontal piece. (See Fig. 18(a).) Cut along the mark
and use this piece as a pattern for the remaining siding panels
on that side. Make another pattern for the other end of the
panels. (See Fig. 18(b).)
9.3.8.2 Lock each precut siding panel into the siding panel
below and slide it into J-channel allowing 1⁄4-in. (6.4-mm)
expansion gap between the end of the siding and back of the
FIG. 14 Preparation of Siding Panel Under Window J-channel.

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D4756 − 15
9.3.8.3 Cut the panel for the top of the gable to match the
angle of the gable. Use furring behind the top of this panel if
necessary to maintain the proper plane of the siding.
9.3.8.4 If the nail hem of the panel for the top of the gable
is cut off to fit the space, face nail the panel. Drill a hole
slightly larger than the size of the nail shank in the center of
this triangular panel. Lock the panel in place and drive one nail
FIG. 21 Undersill Trim Splice
into the pre-drilled hole. Do not nail it tight. Nailing into the
panel without a pre-drilled hole has the potential to crack or
kink the vinyl. (See Fig. 19.)

FIG. 22 Determining Width of Final Siding Panel under Eave


FIG. 19 Nailing of Panel at Top of Gable
that point all along the area to be covered with siding. Leave 1⁄4
9.3.9 The final panel under an eave is handled like the in. (6.4 mm) gap at all corner posts and J-channels. To lap two
portion under a window. Nail undersill trim to the top of the pieces of J-channel, cut away 1 in. (25.4 mm) of the nailing
sidewall (see Fig. 20), flush with the underside of the eave. If flange of the overlapping piece and lap 3⁄4 in. (19 mm). Drill
more than one length of undersill trim is needed, splice by minimum 3⁄16 in. (4.8 mm) diameter weep holes spaced no
cutting out 11⁄4 in. (31.7 mm) inch from the back and nailing more than 24 in. (610 mm) apart in the bottom web of the
flange of one piece of trim, then inserting the second strip J-channel.
inside the first, leaving 1⁄4 in. (6.4 mm) for expansion. (See Fig. 10.3 Corner Posts—Install inside and outside corner posts.
21.) To determine the amount of the top panel to be cut off, Leave a 1⁄4 in. (6.4 mm) gap between the top of the corner post
measure from the bottom of the eave or soffit to the bottom of and eaves or soffits. Extend the corner post to 1⁄4 in. (6.4 mm)
the preceding panel lock in several places along the full length below the lowest edge of the J-channel that serves as the
of the panel and subtract 1⁄4 in. (6.4 mm). (See Fig. 22.) Cut the bottom receiver. Fasten the corner posts by placing the upper-
panels to provide this width. Punch snap-locks every 6 in. (152 most fasteners at the top of the top nail slots, and placing other
mm) along the cut edge and slide it up into position. fasteners spaced not over 12 in. (305 mm) apart centered in nail
slots.
10. Application of Vertical Siding
10.4 Top of Sidewalls—If vinyl soffits are to be installed,
10.1 For general requirements, see 9.1 and 9.2. install the soffits before installation of J-channels at the top of
10.2 Bottom Receiver—Determine the lowest point along all sidewalls. For vinyl soffit installation see Section 11. Install
the area to be covered with siding and install J-channels located J-channels along the top of all wall areas that will receive
so that the lower edge of the J-channel is 1⁄4 in. (6.4 mm) below vertical siding. Lap where necessary, removing 1 in. (25.4 mm)
of the nailing flange of the overlapping piece and lap 3⁄4 in. (19
mm). (See Fig. 23.)
10.5 Trim around all windows and doors as described in
9.2.3, using J-channel at least as wide as the butt height of the
vertical siding.
10.6 For most sidewall applications vertical siding is in-
stalled from one corner across the wall to the other corner. To
FIG. 20 Undersill Trim at Top of Sidewall produce a balanced appearance, measure the width of the wall

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D4756 − 15
mark and cut the ends of all other panels required for this side
of the gable end. Make another pattern for the other side of the
gable. (See Fig. 24.)
10.11 If it will take more than one course to span the height
of the house, terminate the first course into an inverted
J-channel, leaving a 1⁄4 in. (6.4 mm) clearance. Install a head
flashing on top of the J-channel. Then install an upward-facing
J-channel on top of the head flashing. Install the second course
of vertical panels, leaving a 3⁄8 in. (9.5 mm) clearance to the
bottom J-channel. (See Fig. 25.)
FIG. 23 J-Channel Installation at Top of Sidewall
10.12 At windows and doors, cut the panels to fit the
opening allowing 1⁄4 in. (6.4 mm) for expansion.
and divide by the face exposure of the siding panels. Divide 10.12.1 If the panel is cut down in the V-groove, fasten a
any fractional remainder by two and cut siding panels to that wood furring stop as shown in Fig. 26, with fasteners that do
width to be used as the first and last panels. not penetrate the legs of the J-channel or corner post, insert the
NOTE 3—For instance, if a wall requires 20 full panels plus an cut side over the furring strip and into the J-channel, locking
additional 8 in., the first and last panel would be cut to a width of 4 inches. the other side into the last panel. (See Fig. 26.)
Be sure to allow for the depth of the receiving channels when measuring 10.12.2 If the panel is cut on the flat surface, install undersill
the wall width. trim, backed by a furring strip, into the J-channel using
10.7 Initial Siding Panel—To start the first panel, install fasteners that do not penetrate the leg of the J-channel. Punch
utility trim into the receiving pocket of a corner post. Shim the snap locks along the edge of the panel at 6-in. (152-mm)
utility trim so that it matches the level of the siding panel face. intervals; snap it into the space below the return of the
Punch snap locks every 6 in. (152 mm) along to cut edge of the J-channel, locking the other side into the last panel. (See Fig.
vertical siding, and insert into the utility trim. Where the first 27.)
panel will be a full panel, including buttlock, cut the nail hem 10.13 At corners, insert a J-channel of height appropriate for
and top lock from a separate siding panel and install in the the depth of the panel into the receiver of the corner post.
receiving pocket. Hook the buttlock of the first panel over the 10.13.1 If panel is cut in the bottom of the V-groove, insert
top lock to secure the panel. into the J-channel. Install a furring strip prior to panel insertion.
10.7.1 Make sure that the first siding panel is plumb. Fasten This will prevent the panel from detaching. (See Fig. 28.)
the panel by installing the top fastener in the top of the 10.13.2 If the panel is cut on the flat surface, place a piece
uppermost nail slot, Place other fasteners spaced not over 12 in. of undersill trim, backed by furring, into the receiver of the
(305 mm) apart centered in nail slots. Leave 1⁄4 in. (6.4 mm) corner post. Punch snap locks along the cut edge of the panel
clearance at the top and 3⁄8 in. (9.5 mm) clearance to the bottom at 6-in. (152-mm) intervals and snap it into the undersill trim.
receiver. (See Fig. 29.)
10.7.2 For vertical siding under gables and other situations
where the siding is to be visually centered, install back-to- back 11. Application of Soffits and Fascia (See Fig. 30)
J-channels or an H-divider bar at the center of the wall. Install 11.1 Requirements for Proper Ventilation:
utility trim or the cut nail hem and top lock of a siding panel 11.1.1 Calculation of perforated soffit needed for ventila-
in each J-channel, as described in 10.7. Install the vertical tion.
siding from the center toward each corner. As an alternative for 11.1.1.1 Proper attic ventilation is important for any home
non-gabled walls, carefully measure the wall and install the or dwelling. Consult a local building official for the appropriate
siding starting at one side, trimming the first section so that a requirements for a specific geographical area, and use vented
seam or center of a panel falls at the center of the wall. soffit or other vented products as necessary.
10.8 Install the vertical siding panels by locking it into the 11.2 Installation of Soffıt on an Open Rafter (See Fig. 31):
previous panel, and nailing as described in 10.7.1. 11.2.1 Provide two parallel slots to hold and support the
10.9 The last panel at the corner opposite the starting corner soffit panels.
is to be cut to the same width as the first panel. Install it into
the receiving pocket of the corner post using utility trim or the
cut nail hem and top lock of a siding panel, as described in
10.7. Drive a trim nail through the utility trim and edge of the
siding panel, inside the receiving pocket, to prevent the panel
from sliding down inside the trim.
10.10 For application of vertical siding to gables, make a
pattern for end-cuts along the gables using two pieces of scrap
siding. Lock one piece on the starter strip just under the eave.
Hold the edge of the other piece against, and in line with, the
roof line. Mark and cut the vertical piece. Use it as a pattern to FIG. 24 Pattern Preparation for Gable End-Cuts

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FIG. 29 Corner Installation with Panel Cut on Flat Surface

FIG. 25 Joining Area-Multicourse Installation

FIG. 30 Application of Soffit and Fascia

FIG. 26 Installation with Panel Cut in V-Groove

FIG. 31 Installation of Soffit on Open Rafter


FIG. 27 Installation with Panel Cut on Flat Surface
hem into the nailing strip. If nailing strips are not used, drive
a trim nail through the end of each V-groove in the soffit into
the underside of the fascia board.
11.2.5 Where two soffit surfaces meet, a T-channel or two
1⁄2-in. (12.7-mm) J-channels properly supported and nailed

back-to-back will provide support for the soffit panel.


11.2.6 At the ends, pieces of F-channel or 1⁄2-in. (12.7-mm)
J-channel, are installed to finish the job.
11.3 Installation of Soffıt on an Enclosed Rafter (See Fig.
32.):
FIG. 28 Corner Installation with Panel Cut in V-Groove 11.3.1 Provide two parallel slots to hold and support the
soffit panels.
11.3.1.1 Fasten an F-channel to the outer bottom edge of the
11.2.1.1 Fasten an F-channel directly to wall at 6 to 12-in. fascia board.
(152 to 305-mm) intervals. Center the fasteners in the nail slot.
11.2.1.2 Fasten an F-channel on the outer bottom edge of
the fascia board.
11.2.2 Cut a soffit panel to fit into the slots of the
F-channels. Allow 1⁄4 in. (6.4 mm) per side for expansion.
11.2.3 Slide the soffit panels into the F-channel slots. Panels
are hooked together. On panel sections over 16 in. (406 mm)
wide, intermediate nailing supports are required.
11.2.4 Secure each soffit panel with at least one fastener. If
nailing strips are used, place fasteners through the soffit nail FIG. 32 Installation of Soffit on Enclosed Rafter

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D4756 − 15
11.3.1.2 Nail a quarter round Frieze moulding or a J-channel
to the wooden soffit or an F-channel to the wall so that the slot
to hold the soffit is parallel to the slot in the F-channel on the
fascia board.
11.3.2 Cut a soffit panel to fit into the slots of the
F-channels. Allow 1⁄4 in. (6.4 mm) per side for expansion.
11.3.3 Slide the soffit panels into the F-channel slots. Panels
are hooked together.
11.3.4 At the ends, pieces of F-channel or 1⁄2-in. (12.7-mm)
J-channel are installed to finish the job.
FIG. 34 Punch Snaplock Ears on Fascia Cover
11.4 Installation of Fascia:
11.4.1 Install undersill trim molding at the top of the fascia
boards. (See Fig. 33.)
11.4.2 Measure the cover required and cut the fascia cover
to proper width. Punch snaplock “ears” every 6 in. (152 mm)
along the top of the fascia using a snaplock punch. (See Fig.
34.) Position the panel and secure the bottom lip of the fascia
over the F-channel or J-channel, (see Fig. 35.), and snap into
the undersill trim.
11.5 Installation of Corner Cap:
11.5.1 Trim the fascia cover ends at the corners as in Fig.
36. FIG. 35 Positioning of Fascia Cover
11.5.2 Prefabricate or fashion corner caps from a piece of
fascia cover. Cut a 51⁄2-in. (140-mm) length of fascia cover and
mark a vertical centerline on the back as shown in Fig. 37. Cut
out a 90° section of bottom flange from the center, leaving 45°
on each side. Using a hand seamer, fold along the centerline to
form a right angle.
11.5.3 Punch the top edge of a corner cap with a snaplock
punch. Hook the bottom ends of the cap over the fascia flange
and push the top into the undersill trim slot to lock into place.
(See Fig. 38.)
FIG. 36 Trimming Fascia Corner Ends
12. Special Details
12.1 Fitting Siding Around Faucets or Railing—Use a
commercially-available trim ring to fit siding to a penetration
such as a faucet, light fixture, or railing attachment, following
manufacturer’s instructions (See Fig. 39.) If a commercial trim
ring is not available for the application, follow these steps to fit
the siding to the penetration:
12.1.1 Always begin a course of siding at an obstruction
such as a faucet or wrought iron railing to avoid excess lap
joints.
12.1.2 Cut a slot 1⁄4 in. (6.4 mm) bigger than the obstruction, FIG. 37 Prefabricating Corner Cap
matching the contour of the obstruction. Install the first piece
of siding as shown in Fig. 40(a).

12.1.3 Match the contour of the obstruction in the end of the


next panel and lap it over the first one. (See Fig. 40(b).)
12.1.4 Apply flexible caulk around the obstruction to seal
the penetration, but do not caulk the siding overlap.
12.2 Installing Siding Around Electric Boxes—Place
J-channel around the service box, meter, or outlet cover in the
same manner as for windows (see 9.2.3).
12.3 Shutter Installation:
12.3.1 Pre-drill holes through the shutters for attachment
FIG. 33 Installation of Undersill Trim screws and mark their location on the siding. (See Fig. 41.)

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D4756 − 15

(a) Notch and install first (b) Notch and install second
FIG. 40 Fitting Siding

FIG. 38 Installation of Corner Cap

FIG. 41 Shutter Installation


FIG. 39 Commercial Trim Ring

12.3.2 Drill expansion holes through the siding (siding


only) where attachment screws will be located, a minimum of
1⁄4 in. (6.4 mm) larger than the diameter of the screw. (See Fig.

41.)
12.3.3 When attaching the shutters do not fasten such that
the shutter bears tightly against the siding otherwise expansion
of the siding will be restricted. (See Fig. 41.)
13. Keywords
13.1 crimp; horizontal siding; installation practice; poly(vi-
nyl chloride) (PVC); vertical siding; vinyl siding; vinyl soffits

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D4756 − 15

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue D4756 – 13
that may impact the use of this standard (February 1, 2015).

(1) Revised 1.1 to include a reference to applicable building (3) Revised Section 10 to describe proper installation without
codes. use of a vertical starter strip.
(2) Revised 7.4.1 to remove reference to a vertical starter strip

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4803 − 18 An American National Standard

Standard Test Method for


Predicting Heat Buildup in PVC Building Products1
This standard is issued under the fixed designation D4803; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 1.10 This international standard was developed in accor-


1.1 This test method covers prediction of the heat buildup in dance with internationally recognized principles on standard-
rigid and flexible PVC building products above ambient air ization established in the Decision on Principles for the
temperature, relative to black, which occurs due to absorption Development of International Standards, Guides and Recom-
of the sun’s energy. mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
NOTE 1—This test method is expected to be applicable to all types of
colored plastics. The responsible subcommittee intends to broaden the 2. Referenced Documents
scope beyond PVC when data on other materials is submitted for review.
NOTE 2—There are no ISO standards covering the primary subject 2.1 ASTM Standards:2
matter of this test method. D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plas-
1.2 Rigid PVC exterior profile extrusions for assembled
tics
windows and doors are covered in Specification D4726.
D4703 Practice for Compression Molding Thermoplastic
1.3 Rigid PVC exterior profiles for fencing are covered in Materials into Test Specimens, Plaques, or Sheets
Specification F964. D3679 Specification for Rigid Poly(Vinyl Chloride) (PVC)
1.4 Rigid PVC siding profiles are covered in Specification Siding
D3679. D4216 Specification for Rigid Poly(Vinyl Chloride) (PVC)
and Related PVC and Chlorinated Poly(Vinyl Chloride)
1.5 Rigid PVC soffit profiles are covered in Specification (CPVC) Building Products Compounds
D4477. D4477 Specification for Rigid (Unplasticized) Poly(Vinyl
1.6 Rigid PVC and Rigid CPVC plastic building products Chloride) (PVC) Soffit
compounds are covered in Specification D4216. D4726 Specification for Rigid Poly(Vinyl Chloride) (PVC)
1.7 The text of this test method references notes and Exterior-Profile Extrusions Used for Assembled Windows
footnotes which provide explanatory material. These notes and and Doors
footnotes (excluding those in tables and figures) shall not be E631 Terminology of Building Constructions
considered as requirements of this test method. F964 Specification for Rigid Poly (Vinyl Chloride) (PVC)
Exterior Profiles Used for Fencing and Railing
1.8 Units—The values stated in inch-pound units are to be
regarded as the standard. The values given in parentheses are 3. Terminology
mathematical conversions to SI units that are provided for 3.1 Definitions—Definitions are in accordance with Termi-
information only and are not considered standard. nologies D883 or E631 and abbreviations with Terminology
1.9 This standard does not purport to address all of the D1600 unless otherwise indicated.
safety concerns, if any, associated with its use. It is the 3.2 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro- 3.2.1 heat buildup—the increase in temperature above that
priate safety, health, and environmental practices and deter- of ambient air due to the amount of energy absorbed by a
mine the applicability of regulatory limitations prior to use. specimen from the sun.
Specific safety hazard statements are given in Section 7.
3.2.2 temperature rise—the increase in temperature above
that of ambient (laboratory) air due to absorption of energy
from a heating lamp (source).
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.24 on Plastic Building
2
Products. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2018. Published October 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1989. Last previous edition approved in 2018 as D4803 - 10(2018)ɛ1. Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D4803-18. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D4803 − 18
4. Summary of Test Method
4.1 The PVC product (extruded product, injection molded
part, or compression molded) is cut apart to obtain a flat test
specimen at least 3 by 3 by 0.060 6 0.020 in. (76 by 76 by 1.5
6 0.5 mm).
4.2 The test specimen is heated under the infrared reflective
heat lamp to determine the temperature rise above ambient
(laboratory) temperature relative to a black control sample.
4.3 The temperature rise data, obtained in the laboratory for
a given test specimen, is then used to predict the heat buildup,
which may occur outdoors due to the sun.

5. Significance and Use


5.1 Heat buildup in PVC exterior building products due to
absorption of the energy from the sun may lead to distortion
problems. Heat buildup is affected by the color, emittance,
absorptance, and reflectance of a product. Generally, the darker
the color of the product, the more energy is absorbed and the
greater is the heat buildup. However, even with the same
apparent color, the heat buildup may vary due to the specific
pigment system involved. The greatest heat buildup generally
occurs in the color black containing carbon black pigment. The
black control sample used in this test method contains 2.5 parts
of furnace black per 100 parts of PVC suspension resin. The
maximum temperature rise above ambient temperature for this
black is 90°F (50°C) for a 45° or horizontal surface when the
sun is perpendicular to the surface and 74°F (41°C) for a
vertical surface assuming that the measurements were done on
FIG. 1 Apparatus for Measuring Temperature Rise
a cloudless day with no wind and heavy insulation on the back
of the specimen.3 See Appendix X1.
6.1.4 Digital Read-Out Temperature Meter, Type J; or
5.2 This test method allows the measurement of the tem- equivalent.
perature rise under a specific type heat lamp, relative to that of
a black reference surface, thus predicting the heat buildup due NOTE 3—The type of insulation may affect absolute temperature rise.
to the sun’s energy. However, the calculated values of predicted maximum heat buildup,
relative to a black does not appear to be affected, based on a laboratory
5.3 The test method allows prediction of heat buildup of study comparing white rigid hydrous calcium silicate heat insulation with
various colors or pigment systems, or both. aluminum foil insulation having equivalent thermal resistance.
NOTE 4—The intensity of the heat lamp has an effect on absolute
5.4 This test method gives a relative heat buildup compared temperature rise, however, it does not appear to influence the calculated
to black under certain defined severe conditions but does not values of predicted maximum heat buildup relative to the black control.
predict actual application temperatures of the product. These The 250-W infrared heat lamp was selected because a higher intensity
lamp results in excessive temperature rise. This leads to excessive
will also depend on air temperature, incident angle of the sun, softening of the specimen under study, especially in the case of the black
clouds, wind velocity, insulation, installation behind glass, etc. control. A lower intensity lamp requires a longer testing time and,
therefore, is considered undesirable.
6. Apparatus 6.2 The thermocouple shall be inserted through a 0.125-in.
6.1 Testing Apparatus—The apparatus shall be constructed (3.18-mm) hole in the bottom of the box, so that it extends 0.25
essentially as shown in Fig. 1 and shall consist of the in. (6.35 mm) above the bottom surface of the box. The
following: thermocouple bends under the weight of the specimen, but
6.1.1 Wooden Box, opened from the top and the front and shall retain contact with the specimen when the specimen is in
lined with 1-in. (25.4-mm) thick white rigid hydrous calcium place. The lamp shall be installed perpendicular to the thermo-
silicate heat insulation. couple.
6.1.2 White Infrared Heat Lamp, 250-W.4 6.3 The distance from the bottom of the box to the bottom
6.1.3 Thermocouple, 40-gage Type J (iron-constantan); or surface of the lamp shall be 15.5 6 1 in. (39.4 6 2.5 cm).
equivalent.
NOTE 5—Calculated heat buildup for the specimens is independent of
the distance between the light source and the surface of the specimen.
However, shorter distances lead to very high maximum equilibrium
3
Summers and Brown, SPE Technical Papers, XXV, 1979, p. 403. temperatures, especially for dark colors, which might cause distortion of
4
A G.E. heat lamp has been found satisfactory for this purpose. the specimen. Larger distances between the light source and the specimen

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D4803 − 18
cause less test sensitivity and less reproducibility.
6.4 Install the apparatus in a room characterized by still air
without drafts due to air conditioning, etc.
7. Safety Precautions
7.1 The heating lamp is hot during the test. Touching it will
cause burns.
8. Sampling
8.1 Select samples in a statistically acceptable manner. The
samples shall be representative of the color or pigment system,
or both, under study. FIG. 2 Time for Maximum Equilibrium Temperature Rise as a
Function of the Sample Thickness for Poly(Vinyl Chloride)
9. Test Specimens
9.1 Test flat test specimens measuring 3 6 0.125 in. square
11.2 Heat buildup:
by 0.060 6 0.020 in. thick (76 6 3.2 mm square by 1.5 6 0.5
mm), cut from the selected samples. ∆Tlu
∆T 5 3 ∆Tb (2)
∆Tlb
9.2 A control specimen conforming in size with the speci-
fication in 9.1 shall be prepared from any rigid PVC compound where:
containing 2.5 parts Black Pearls 7005 or equivalent furnace ∆T = predicted heat buildup of the specimen under study
type carbon black without any other pigmentation. See Practice due to heating by the sun,
D4703. ∆Tlu = temperature rise above ambient temperature in the
laboratory for the specimen under study,
10. Procedure ∆Tlb = temperature rise above ambient temperature in the
10.1 Maintain the ambient air temperature in the laboratory, laboratory for a black control sample,
measured 3 ft from the side of the testing box, at 75 6 5°F. ∆Tb = heat buildup for a black control sample under con-
10.2 Set the specimen on the bottom of the box so that its trolled conditions due to absorption of the sun’s
center is in contact with the thermocouple. Use two-sided energy (found experimentally),
adhesive tape between the specimen and the box to ensure ∆Tb = for vertical position, 74°F or 41°C, and
contact with the thermocouple. ∆Tb = for horizontal position, 90°F or 50°C.
10.3 Turn on the heat lamp and digital read out temperature NOTE 7—Conversion equations for ∆Tb are as follows:
meter. °C 2 2 ° C 1 5 ~ °F 2 2 32! 5/9 2 ~ °F 1 2 32! 5/9
10.4 From the temperature meter, record the equilibrium °C 2 2 °C 1 5 5/9°F 2 5/9 3 32 2 5/9°F15/9 3 32
temperature of the specimen. The maximum interval shall be ∆°C 5 5/9∆°F ~ conversion equation!
five minutes. Equilibrium is defined as an increase of less than 11.3 To determine maximum temperature the specimen can
1°F in any given five-minute interval. achieve outdoors under the most severe conditions (clear skies,
NOTE 6—It is expected that equilibrium is reached between 20 and 30 no wind, sun is perpendicular to the specimen), the predicted
minutes for the standard 0.060 6 0.020 in. thick (1.5 6 0.5 mm) heat buildup temperature must be added to the ambient
specimen. Individual formulations may require different durations of time. temperature.
See Fig. 2 for relationship of the time required to reach equilibrium
temperature and the thickness of the PVC specimens. 12. Report
10.5 Measure the maximum temperature of the control 12.1 The report shall include the following:
specimen prior to the specimens under study but within 2 h of 12.1.1 Complete identification of the specimen tested, color,
the other temperature rise measurements. manufacturer’s code,
11. Calculation 12.1.2 Temperature rise above ambient air temperature in
the laboratory for the black control specimen,
11.1 Temperature rise above ambient temperature: 12.1.3 Temperature rise above ambient air temperature in
∆Tlu 5 Tm 2 Ta (1) the laboratory for the specimen under study, and
12.1.4 Heat buildup, degrees Fahrenheit (degrees Celsius),
where:
of the test specimen under study.
∆Tlu = temperature rise above ambient temperature in the
laboratory under the heat lamp, 13. Precision and Bias
Tm = maximum temperature of the specimen, as read from
13.1 For precision and bias data, see Table 1.
the digital temperature meter, and
Ta = ambient air temperature in the laboratory. 14. Keywords
14.1 heat buildup; PVC building products; sun energy
5
Available from Cabot Corp., P.O. Box 188, Tuscola, IL 61953. absorption; weathering

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D4803 − 18
TABLE 1 Precision and BiasA,B
Material Color Mean Values as a Percentage of the Mean
Heat Sr SR Ir IR
Buildup,
°C
M1 Gray 31.25 3.3 5.1 9.3 14.4
M2 Beige 27.76 4.7 6.8 13.3 19.2
M3 Beige 29.63 3.1 8.8 8.8 24.9
M4 Gray 24.08 2.3 5.8 6.5 16.4
M5 Brown 34.56 6.0 7.5 17.0 21.2
M6 White 20.18 5.8 10.9 16.4 30.8
M7 Brown 33.38 6.0 3.6 17.0 10.2
M8 Beige 26.75 7.5 4.5 21.2 12.7
M9 Green 28.12 4.4 7.5 12.5 21.2
M 10 Brown 39.34 2.7 2.8 7.6 7.9
M 11 Beige 27.32 4.3 6.6 12.2 18.7
M 12 Brown 34.49 6.4 4.0 18.1 11.3
M 13 Green 34.28 2.8 4.4 7.9 12.4
Precision (Average) → 4.8 6.1 13.6 17.3

A
Table 1 is based on a round-robin study conducted in 1985, involving 13 materials
tested by 6 laboratories. Each test result was based on 44 individual determina-
tions. Each laboratory obtained 8 test results for each material. Supporting data
have been filed at ASTM International Headquarters and may be obtained by
requesting Research Report RR:D20-1142.
B
In Table 1, for the materials indicated:
Sr = pooled within-laboratories standard deviation of the average of 40 test
specimens,
SR = pooled between-laboratories standard deviation of the average of 40 test
specimens,
Ir = 2.83 Sr—repeatability, and
IR = 2.83 SR—reproducibility.

APPENDIX

(Nonmandatory Information)

X1. CORRELATION OF HEAT LAMP TO SOLAR ENERGY HEATING OF VINYL

NOTE 1—Source: Summers and Brown, SPE Technical Papers, XXV, 1979, p. 403.
FIG. X1.1 Correlation of Heat Lamp to Solar Energy Heating of Vinyl

SUMMARY OF CHANGES

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D4803 − 18
Committee D20 has identified the location of selected changes to this standard since the last issue
(D4803 - 10(2018)ɛ1) that may impact the use of this standard. (October 1, 2018)

(1) Revised 9.1 and 9.2 to provide a more precise specification


for specimen size.
(2) Revised 10.4 to specify the conditions considered to
represent equilibrium, and to place advisory material into a
Note.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4890 − 18

Standard Test Methods for


Polyurethane Raw Materials: Determination of Gardner and
APHA Color of Polyols1
This standard is issued under the fixed designation D4890; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D6166 Test Method for Color of Pine Chemicals and Re-
1.1 These test methods measure visually the color of clear lated Products (Instrumental Determination of Gardner
polyester and polyether liquids. They apply only to materials Color)
whose colors have light-absorption characteristics similar to E177 Practice for Use of the Terms Precision and Bias in
those of the standards. An alternative method is Test Method ASTM Test Methods
D1209 (see Note 1). E308 Practice for Computing the Colors of Objects by Using
the CIE System
1.2 Units—The values stated in SI units are to be regarded E691 Practice for Conducting an Interlaboratory Study to
as standard. No other units of measurement are included in this Determine the Precision of a Test Method
standard. E1164 Practice for Obtaining Spectrometric Data for Object-
1.3 This standard does not purport to address all of the Color Evaluation
safety concerns, if any, associated with its use. It is the 2.2 ISO Standards:3
responsibility of the user of this standard to establish appro- ISO 4630-1 Clear Liquids—Estimation of Colour by the
priate safety and health practices and determine the applica- Gardner Colour Scale—Part 1: Visual Method
bility of regulatory limitations prior to use. ISO 4630-2 Clear Liquids—Estimation of Colour by the
Gardner Colour Scale—Part 2: Spectroscopic Method
NOTE 1—Test Method A of this standard is equivalent to ISO 6271-1.
Test Method B of this standard is equivalent to ISO 4630-1. ISO 6271-1 Clear Liquids—Estimation of Colour by the
Platinum-Cobalt Scale—Part 1: Visual Method
1.4 This international standard was developed in accor-
ISO 6271-2 Clear Liquids—Estimation of Colour by the
dance with internationally recognized principles on standard-
Platinum-Cobalt Scale—Part 2: Spectroscopic Method
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 3. Terminology
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 3.1 For definitions of terms used in these test methods see
Terminology D883.
2. Referenced Documents
4. Summary of Test Method
2.1 ASTM Standards:2
4.1 In Test Method A, the color of the material to be tested
D883 Terminology Relating to Plastics
is compared to a series of color standards with defined
D1193 Specification for Reagent Water
chromaticity coordinates, prepared in one of three ways. The
D1209 Test Method for Color of Clear Liquids (Platinum-
results are reported as the color standard, which best matches
Cobalt Scale)
the sample.
D5386 Test Method for Color of Liquids Using Tristimulus
Colorimetry 4.2 In Test Method B, the color of the material to be tested
is compared to a series of platinum-cobalt color standards,
designated by mg of Pt/mL of standard solution. The results are
1
These test methods are under the jurisdiction of Committee D20 on Plastics and
reported as the color standard, which best matches the sample
are the direct responsibility of Subcommittee D20.22 on Cellular Materials - Plastics (see Note 2).
and Elastomers.
Current edition approved Aug. 1, 2018. Published August 2018. Originally NOTE 2—Color of liquids are also measured by visible spectroscopy
approved in 1988. Last previous edition approved in 2013 as D4890 - 13. DOI: and the results converted to any of several color scales. These results are
10.1520/D4890-18. converted to the APHA scale by appropriate manipulations, as for example
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.

*A Summary of Changes section appears at the end of this standard


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D4890 − 18
in Test Method D5386 and ISO 6271-2. These results are converted to the color equivalence to a freshly prepared solution containing 3 g
Gardner scale by appropriate manipulations, as for example in Test of K2Cr2O7 in 100 mL of H2SO4 (sp gr 1.84).
Method ISO 4630-2.
9.3 Hydrochloric Acid (1 to 17)—Mix 1 volume of concen-
5. Significance and Use trated hydrochloric acid (HCl, sp gr 1.19) with 17 volumes of
5.1 These test methods are suitable for quality control, as water.
specification tests, and for research. Color is an important 9.4 Hydrochloric Acid (0.1 N)—Prepare 0.1 N HCl.
property of urethane products.
9.5 Potassium Chloroplatinate (PtCl6).
6. Sampling 9.6 Potassium Dichromate (K2Cr2O7).
6.1 Polyesters and polyethers usually contain molecules 9.7 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
covering an appreciable range of molecular weights. These (H2SO4).
have a tendency to fractionate during solidification. Unless the
material is a liquid or finely ground solid it is necessary to melt 10. Gardner Color Reference Standards5
(using no higher temperature than necessary) and mix the resin 10.1 The primary standards for color shall consist of solu-
well before removing a sample for analysis. Many polyols are tions defined by their spectral transmittance in 1-cm cell with
hygroscopic and care must be taken to provide minimum parallel sides. The chromaticity coordinates of these solutions
exposure to atmospheric moisture during the sampling. shall conform to those given in Table 1 when determined on a
1-cm layer of the solution in accordance with Practice E1164
7. Purity of Reagents and Test Methods E308 and D6166.
7.1 Purity of Reagents—Reagent-grade chemicals shall be 10.2 For comparison, permanent solutions of known color
used in all tests. Unless otherwise indicated, it is intended that are more satisfactory. The approximate composition of solu-
all reagents shall conform to the specifications of the Commit- tions giving each of the 18 Gardner colors is also given in
tee on Analytical Reagents of the American Chemical Society, Table 1. The solutions shall be made from K2PtCl6 in 0.1 N
where such specifications are available.4 Other grades are HCl, or, in the darker colors, from stock solutions of FeCl3,
acceptable, provided it is first ascertained that the reagent is of CoCl2, and HCl (see 9.1, 9.2, and 9.3). Pre-prepared Gardner
sufficiently high purity to permit its use without reducing the color standard solutions are commonly available for purchase.
accuracy of the determination.
10.3 If the solutions in 10.2 are unavailable, solutions of
7.2 Purity of Water—Unless otherwise indicated, references K2Cr2O7 (sp gr 1.84) are used as reference standards. The
to water shall be understood to mean reagent water as defined approximate composition of these standards is also given in
by Type IV or better of Specification D1193. Table 1. Each solution must be freshly made for the color
comparison, using gentle heat, if necessary, to effect solution.
TEST METHOD A—GARDNER COLOR
10.4 Secondary reference standards are available in the
8. Apparatus form of 18 colored glass disks, which are set into a pair of
8.1 Gardner-Holdt Tubes, of clear glass, with closed, flat, larger, plastic disks and the latter mounted to rotate in a
even bottoms, and having the following approximate dimen- housing for holding the sample tube and glass disk in close and
sions and markings: fixed proximity.
8.1.1 A uniform internal length of 112 mm, 11. Procedure
8.1.2 A uniform internal diameter throughout the length of
the tube of 10.75 mm, and 11.1 Fill the tube with sample, free of solid particles or air
8.1.3 An etched line around the outside of the tube 5 mm bubbles, so that the apparent upper edge of the liquid meniscus
from the open end and a second etched line around the outside is even with the lower etched line on the tube.
of the tube 13 mm from the open end. 11.2 Determine the color by comparison with the reference
standard solutions prescribed in Table 1, by comparing the
9. Reagents sample and the standard in Gardner-Holdt viscosity tubes as
9.1 Cobalt Chloride Solution—Prepare a solution contain- described. Make the comparison at 25 6 5°C by placing tubes
ing 1 part by weight of cobalt chloride (CoCl2 × 6H2O) to 3 close together and looking through them against a white
parts of HCl (1 to 17). background or by comparison to the standards in a color disk.
9.2 Ferric Chloride Solution—Prepare a solution containing 12. Report
approximately 5 parts by weight of ferric chloride
12.1 Report the color of the sample in terms of the Gardner
(FeCl3 × 6H2O) and 1.2 parts of HCl (1 to 17). Adjust to exact
standard number that is nearest to it in color. If the sample

4 5
Reagent Chemicals, American Chemical Society Specifications, American The sole source of supply of the glass color standards and color standard
Chemical Society, Washington, DC. For suggestions on the testing of reagents not solutions known to the committee at this time is BYK-Gardner USA, 9104 Guilford
listed by the American Chemical Society, see Analar Standards for Laboratory Road, Columbia, MD 21046. If you are aware of alternative suppliers, please
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia provide this information to ASTM International Headquarters. Your comments will
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, receive careful consideration at a meeting of the responsible technical committee,1
MD. which you may attend.

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D4890 − 18
TABLE 1 Gardner Reference Standard Color Solutions
Chromaticity CoordinatesA Potassium Iron-Cobalt Solutions Potassium
Gardner Color Standard Chloroplatinate,
Ferric Chloride Cobalt Chloride Dichromate, g/100 mL
Number Y x y g/1000 mL of 0.1 Hydrochloric Acid, mL
Solution, mL Solution, mL Sulfuric AcidB
N HCl
1 80 0.3177 0.3303 0.550 ... ... ... 0.0039
2 79 0.3233 0.3352 0.865 ... ... ... 0.0048
3 76 0.3329 0.3452 1.330 ... ... ... 0.0071
4 75 0.3437 0.3644 2.080 ... ... ... 0.0112
5 74 0.3558 0.3840 3.035 ... ... ... 0.0205
6 71 0.3767 0.4061 4.225 ... ... ... 0.0322
7 67 0.4044 0.4352 6.400 ... ... ... 0.0384
8 64 0.4207 0.4498 7.900 ... ... ... 0.0515
9 61 0.4343 0.4640 ... 3.8 3.0 93.2 0.0780
10 57 0.4503 0.4760 ... 5.1 3.6 91.3 0.164
11 45 0.4842 0.4818 ... 7.5 5.3 87.2 0.250
12 36 0.5077 0.4638 ... 10.8 7.6 81.6 0.380
13 30 0.5392 0.4458 ... 16.6 10.0 73.4 0.572
14 22 0.5646 0.4270 ... 22.2 13.3 64.5 0.763
15 16 0.5857 0.4089 ... 29.4 17.6 53.0 1.041
16 11 0.6047 0.3921 ... 37.8 22.8 39.4 1.280
17 6 0.6290 0.3701 ... 51.3 25.6 23.1 2.220
18 4 0.6477 0.3521 ... 100.0 0.0 0.0 3.00
A
Chromaticity coordinates for CIE standard illuminant C and the CIE 1931 (2°) standard observer.
B
The dichromate color standards have been found to be less reliable than chloroplatinate or iron-cobalt color standards. They are included in Table 1 for reference only.

appears exactly halfway between two standards, report the test results for the same material, obtained by the same
color number of the darker standard. operator using the same equipment on the same day in the same
laboratory due solely to the method is 0.7 units.
13. Precision and Bias6
13.6 Reproducibility Limit, R—The value below which the
13.1 Table 2 is based on an interlaboratory study conducted absolute difference between two individual test results obtained
in 2011. Six laboratories tested two different polyurethane under reproducibility conditions is expected to occur with a
materials. Every “test result” represents an individual determi- probability of approximately 0.95 (95 %). For the data gener-
nation. Each laboratory reported three replicate test results for ated in Table 2, the maximum expected differences between
each material. Practice E691 was followed for the design and two test results for the same material, obtained by different
analysis of the data; the details are given in ASTM Research operators using different equipment in different laboratories
Report No. D20-1257. due solely to the method is 2.0 units.
13.2 Caution—The explanation of the repeatability (r) and 13.7 Any judgment in accordance with the repeatability and
reproducibility (R) is only intended to present a meaningful reproducibility statements shown above would have an ap-
way of considering the approximate precision of this test proximate 95 % (0.95) probability of being correct.
method. Do not apply the data in Table 2 to acceptance or
rejection of materials, as these data apply only to the materials 13.8 Bias—There are no recognized standards by which to
tested in the round robin and are unlikely to be rigorously estimate bias of this method.
representative of other lots, formulations, conditions, materials, TEST METHOD B—APHA COLOR
or laboratories. Users of this test method need to apply the
principles outlined in Practice E691 to generate data specific to 14. Apparatus
their materials and laboratory (or between specific laborato- 14.1 Nessler Tubes, matched 100-mL, tall-form.
ries). The principles would then be valid for such data
13.3 Repeatability—Precision under repeatability condi- 15. Reagents
tions. 15.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
13.4 Reproducibility—Precision under reproducibility con- chloric acid (HCl).
ditions. 15.2 Potassium Chloroplatinate (K2PtCl6).
13.5 Repeatability Limit, r—The value below which the 15.3 Cobaltous Chloride Hexahydrate (CoCl2 · 6H2O).
absolute difference between two individual test results obtained
under repeatability conditions is expected to occur with a 16. Preparation of Color Standards
probability of approximately 0.95 (95 %). For the data gener- 16.1 Pre-prepared platinum-cobalt standards are commonly
ated in Table 2, the maximum expected difference between two available for purchase or prepared by the following. Measure
500 mL of water into a 1000-mL volumetric flask. Add 100 mL
6
of the HCl and mix well. Weigh 1.245 g of K2PtCl6 to the
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D20-1257. Contact ASTM Customer nearest 1 mg and transfer to the flask (see Note 3). Add 1.0 g
Service at service@astm.org. of crystallized CoCl2 · 6H2O. Dilute the solution in the flask to

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D4890 − 18
TABLE 2 Gardner Color (Gardner Color Standard Number)
A
Material Average Repeatability Reproducibility Repeatability Reproducibility
Standard Standard Limit Limit
Deviation Deviation
x̄ Sr SR r R
Jeffol 5.2 0.2 0.4 0.7 1.3
SD-441
Jeffol 9.6 0.2 1.0 0.7 2.7
SA-499
A
The average of the laboratories’ calculated averages.

the mark with water and mix thoroughly. The color of this TABLE 3 APHA Color Standards
standard solution is equivalent to 500 units (500 mg metallic Color Standard Number
Number 500 Standard,
Water, mL
platinum/L), that is each milliliter of standard contains 0.5 mg mL

of metallic platinum. 1 0.2 99.8


3 0.6 99.4
NOTE 3—If potassium chloroplatinate is not available, dissolve 0.500 g 5 1.0 99.0
of pure metallic platinum in aqua regia with the aid of heat; then remove 10 2.0 98.0
15 3.0 97.0
HNO3 by repeated evaporation with fresh portions of HCl. Dissolve this
18 3.6 96.4
product as directed in 16.1. 20 4.0 96.0
16.2 Prepare the required color standards by diluting the 25 5.0 95.0
30 6.0 94.0
No. 500 standard solution as shown in Table 3. If more exact 40 8.0 92.0
color comparison is desired, prepare additional standards to 50 10.0 90.0
supplement those given below. One color unit is equivalent to 60 12.0 88.0
70 14.0 86.0
1 mg metallic platinum/liter. Protect these standards against 80 16.0 84.0
evaporation and contamination when not in use. 90 18.0 82.0
100 20.0 80.0
17. Procedure 120 24.0 76.0
140 28.0 72.0
17.1 Transfer 100 mL of the sample to one of two matched 160 32.0 68.0
100-mL tall-form Nessler tubes. Fill the second tube to the 180 36.0 64.0
200 40.0 60.0
mark with the standard that seems to match the color of the 300 60.0 40.0
sample as indicated by a preliminary estimation. Compare the 400 80.0 20.0
500 100.0 0.0
colors of the sample and the standard by viewing vertically
down through the tubes against a white background. Replace
the liquid in the second tube with lighter or darker standards
until an exact match is obtained.
18. Report their materials and laboratory (or between specific laborato-
18.1 Report the color of the sample in terms of the color ries). The principles would then be valid for such data.
standard number that is nearest to it in color. If the sample 19.3 Repeatability—Precision under repeatability condi-
appears exactly halfway between two standards, report the tions.
color number of the darker standard.
19.4 Reproducibility—Precision under reproducibility con-
19. Precision and Bias ditions.
19.1 The precision of this test method is based on an 19.5 Repeatability Limit, r—The value below which the
interlaboratory study conducted in 2011. Six laboratories tested absolute difference between two individual test results obtained
four different polyurethane materials. Every “test result” rep- under repeatability conditions is expected to occur with a
resents an individual determination. Each laboratory reported probability of approximately 0.95 (95 %). For the data gener-
three replicate test results for each material. Practice E691 was ated in Table 4, the maximum expected difference between two
followed for the design and analysis of the data; the details are test results for the same material, obtained by the same
given in ASTM Research Report No. D20-1257. operator using the same equipment on the same day in the same
laboratory due solely to the method is 0.7 units.
19.2 Caution—The explanation of the repeatability (r) and
reproducibility (R) is only intended to present a meaningful 19.6 Reproducibility Limit, R—The value below which the
way of considering the approximate precision of this test absolute difference between two individual test results obtained
method. Do not apply the data in Table 4 to acceptance or under reproducibility conditions is expected to occur with a
rejection of materials, as these data apply only to the materials probability of approximately 0.95 (95 %). For the data gener-
tested in the round robin and are unlikely to be rigorously ated in Table 4, the maximum expected differences between
representative of other lots, formulations, conditions, materials, two test results for the same material, obtained by different
or laboratories. Users of this test method need to apply the operators using different equipment in different laboratories
principles outlined in Practice E691 to generate data specific to due solely to the method is 26 units.

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D4890 − 18
TABLE 4 APHA Color (APHA Color Standard Number)
A
Material Average Repeatability Reproducibility Repeatability Reproducibility
Standard Standard Limit Limit
Deviation Deviation
x̄ Sr SR r R
Jeffol 10.6 0.2 7.4 0.7 20.8
G 31-35
Jeffol 80.8 0.2 11.1 0.7 31.1
S-490
A
The average of the laboratories’ calculated averages.

20. Keywords
20.1 APHA; color; Gardner; platinum-cobalt scale; polyols;
polyurethane raw materials; Pt-Co scale

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4890–13)
that may impact the use of this standard. (August 1, 2018)

(1) Corrected spelling throughout. (3) Updated Precision and Bias statements to comply with
(2) Removed non-mandatory language throughout. D4968.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5117 − 17

Standard Test Method for


Dye Penetration of Solid Fiberglass Reinforced Pultruded
Stock1
This standard is issued under the fixed designation D5117; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D883 Terminology Relating to Plastics


1.1 This dye-penetrant test method covers a means of D3918 Terminology Relating to Reinforced Plastic Pul-
evaluating solid fiberglass all-roving reinforced pultruded rod truded Products
or bar stock for longitudinal wicking. There are generally three E456 Terminology Relating to Quality and Statistics
mechanisms that promote wicking such as delaminations,
longitudinal continuous voids, or the presence of hollow fibers. 3. Terminology
Any or all of them will be operating at a given time. 3.1 Definitions—For definitions of technical terms pertain-
NOTE 1—Occasionally the flaws listed above may be detected by this
ing to plastics used in this test method, see Terminology D883.
test, but other tests are usually required. 3.2 For definitions of terms that appear in this standard
1.2 The values stated in either SI units or inch-pound units relating to reinforced plastic pultruded products, refer to
are to be regarded separately as standard. The values stated in Terminology D3918.
each system are not necessarily exact equivalents; therefore, 3.3 For definitions of terms that appear in this standard
each system shall be used independently of the other. Combin- relating to quality and statistics, refer to Terminology E456.
ing values from the two systems has the potential to result in
3.4 Definitions of Terms Specific to This Standard:
nonconformance with the standard.
3.4.1 wicking—transmission of a gas or liquid due to pres-
1.3 This standard does not purport to address all of the sure differential or capillary action along fibers incorporated in
safety concerns, if any, associated with its use. It is the a fiberglass reinforced pultruded product.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- 4. Summary of Test Method
mine the applicability of regulatory limitations prior to use.
For specific hazard statements, see 10.3 and 10.6. 4.1 All-roving pultruded rod stock is tested by placing the
specimen(s) on end into the dye penetrant to a specified depth
NOTE 2—There is no known ISO equivalent to this test method. and observing the wicking action as spots, or dots, on the
1.4 This international standard was developed in accor- opposite, dry face.
dance with internationally recognized principles on standard-
4.2 The wicking action through the length of the specimen
ization established in the Decision on Principles for the
is due to the capillary action of the penetrant through the open
Development of International Standards, Guides and Recom-
pathways in the composite. These pathways are typically
mendations issued by the World Trade Organization Technical
occupied by air and are caused by continuous voids, cracks, or
Barriers to Trade (TBT) Committee.
hollow fibers, or all three, simultaneously.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:2
D618 Practice for Conditioning Plastics for Testing 5.1 This test method is useful for establishing the integrity
of composite rod. The presence of voids, cracks, and hollow
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics fibers are considered detrimental to the structural integrity of
and is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset- the composite and causes reduced electrical resistance and
ting Plastics. increased current leakage.
Current edition approved Dec. 15, 2017. Published January 2018. Originally
approved in 1990. Last previous edition approved in 2009 as D5117 - 09. DOI: 5.2 A perfect composite would be flaw-free, and there
10.1520/D5117-17.
2
would be no possibility of wicking. Composites of this type are
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
virtually nonexistent, as there will typically be entrapped air in
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on the resin developed during manufacturing, occasional hollow
the ASTM website. fibers, and occasional cracks due to thermal stresses.

*A Summary of Changes section appears at the end of this standard


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5.3 This test method is intended to provide a tool for 8.2 Specimens shall not be taken from material that has
measuring the extent of wicking in a composite over very short been damaged or subjected to previous testing.
lengths of material for comparative purposes. The presence of 8.3 Select at least three 1-in. (2.54 cm) length specimens
wicking over 1 in. (2.54 cm) lengths will not necessarily imply taken at random locations along the rod stock to be tested.
that the composite will perform unsatisfactorily for its intended These shall be cut dry with a diamond-dust blade to ensure a
end-use. Therefore, interpretation of test results shall be made smooth test surface.
carefully.
8.4 In order to prevent the problem of wicking up the sides
5.4 This test method was developed as a technique for of some composites, paint a ring of clear nail polish or other
estimating quality and consistency of pultruded rod and bar suitable inhibitor below the top surface and around the circum-
stock, which is a composite of resin and all-roving reinforce- ference of each test specimen.
ment. This test method will be useful for a manufacturer to
determine whether any gross changes in quality have taken
9. Conditioning
place due to process or raw material changes as the manufac-
turing process also affects the quality of the product. 9.1 Condition the test specimens at 23 6 2°C (73.4 6
3.6°F) and 50 6 10 % relative humidity for not less than 40 h
5.5 Since the results of this test are so sensitive to sample
prior to test in accordance with Procedure A of Practice D618.
size, penetrant type, penetrant used, viscosity, duration of test,
and other factors, no attempt to arrive at or recommend 9.2 Test Conditions—Conduct all testing in the standard
development of a specification for these materials has been laboratory atmosphere of 23 6 2°C (73.4 6 3.6°F) and 50 6
made. A specification shall be negotiated between supplier and 10 % relative humidity, unless otherwise specified.
end user and such specification shall be made with great care.
10. Procedure
6. Apparatus
10.1 Preheat the ultraviolet light source for 15 min or in
6.1 Dye Penetrant3 accordance with the manufacturer’s recommendations. Posi-
6.2 Ultraviolet Light Source—The penetrant used is tion the light to shine on the pan (penetrant) surface.
fluorescent, and requires a black lamp light source. 10.2 Place a thin, spongy material such as common house-
6.3 Dark Room—An area for viewing the presence of hold plastic foam sponge on the bottom of the pan to support
fluorescent spots on the test specimens is required. the specimens. This material aids in properly wetting the
6.4 Hood—There is a need to provide adequate air ventila- bottom surface of the specimen and reduces possible problems
tion for the elimination of any annoying vapors from the associated with air entrapment.
penetrant. These vapors are nontoxic, but has potential to be an 10.3 Add sufficient dye to the pan such that the specimens
irritant. will be immersed to a depth of 1⁄8 in. (0.32 cm) while resting on
6.5 Shallow Pan, for holding the penetrant is required. A the sponge. This depth shall be predetermined with an extra
thin, spongy material that can be placed in the pan to support piece of rod stock.
the specimen on one end. 10.4 Warning—Avoid hand contact with the penetrant to
6.6 Stop Watch, or other means for timing the length of the preclude possible contamination of the specimens during
test is required. handling. Wash hands thoroughly before proceeding, if contact
with the penetrant were to occur.
6.7 Magnifying Glass, 5×, recommended for identifying
Place each specimen on end in the penetrant to the depth
very small fluorescent specks, or dots, on the specimen’s upper
specified in 10.3 and staggered from the rest of the group. The
face. It is not regarded as essential.
actual time of immersion for each shall be recorded if more
7. Materials than six specimens are to be tested at one time. Otherwise, all
specimens shall be considered to be immersed at the same
7.1 This test method was developed for use on solid time. When more than six specimens are tested, an interval of
pultruded all-roving rod and bar stock reinforced with fiber- 30 s between the respective immersions shall be observed. For
glass. An evaluation employed 1 in. diameter rod stock using example, if a group of nine specimens were to be tested, one
epoxy, vinyl ester and polyester resins. It was determined that could be added at T = 0, the next at T = 30 s, and the last at
this test method is applicable for all three resin series. T = 4.0 min.
7.2 Use rod-stock representative of typical production lots
10.5 Immerse each specimen such that its lower face is
and select random specimens for testing.
inserted into the dye normal to the supporting sponge to ensure
8. Sampling and Test Specimens optimum coating of its surface. Press down lightly on the upper
face of the specimen to effect its positive sealing.
8.1 Take at least three test specimens for each sample.
10.6 See Warning in 10.4.
3
Zyglo Penetrex ZL 30A dye penetrant, manufactured by Magnaflex, or 10.7 Position the specimens in the penetrant in a row left to
equivalent, is suitable for this purpose. During the initial round-robin work, three right such that the first, second, etc. can be easily identified.
standard penetrants of the industry were evaluated. The above referenced penetrant
provided the most discriminating, rapid, and consistent results. 10.8 Record the time for the appearance of the first dot.

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D5117 − 17
10.9 Count upper face wicking dots (fluorescent specks) 11.1.5 The average of the individual wicking data for each
following 30 min of penetrant immersion. For a large group of sample,
specimens, the counting must be completed between 29 min, 11.1.6 Date of test, and
45 s and 30 min, 15 s for each specimen. 11.1.7 Any deviations from the test method shall be
10.9.1 The immersion time of 30 min for all specimens is included, such as alternate penetrant source, etc.
particularly critical and must be observed within the limits
specified under 10.9 if meaningful data are to be obtained. In 12. Precision
fact, the time at which the extent of wicking is determined has
been found to be the greatest single source of error in 12.1 Repeatability—The value below which the absolute
interlaboratory comparisons of wicking data. difference between two individual test results obtained under
repeatability conditions is expected to occur with a probability
10.10 If an error is made, or if a specimen falls into the
of approximately 0.95 (95 %).
penetrant, reject that specimen and run a retest from retained TABLE Number of Wicking Dots
stock.
Polyester Epoxy Vinyl Ester
10.11 Test at least three specimens per sample.
Repeatability 7.85 4.17 13.5
10.12 Record the time to the first dot. Record the total
number of wicking dots, or specks, for each specimen after 12.2 Reproducibility—The value below which the absolute
30-min immersion, discounting those that have merged as one. difference between two individual test results obtained under
If the latter condition exists, discontinue the test for that reproducibility conditions is expected to occur with a probabil-
particular specimen and test another. ity of approximately 0.95 (95 %).
TABLE Number of Wicking Dots
11. Report Polyester Epoxy Vinyl Ester

11.1 Report the following information: Reproducibility 9.41 4.17 14.6


11.1.1 Complete identification of the material tested, includ-
ing resin type, machine identification, dimensions, reinforce- 12.3 The above precision data were generated as the result
ment type, manufacturer’s code, etc., of an industry round-robin in which seven laboratories
11.1.2 Conditioning procedure used, if different than participated, using rod stock from a single supplier’s standard
stipulated, inventory.
11.1.3 Test room conditions,
11.1.4 Individual specimens tested, with individual wicking 13. Keywords
data, 13.1 dye penetration test; pultruded rod; rod stock; wicking

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5117 - 09)
that may impact the use of this standard. (December 15, 2017)

(1) Added “them will” and removed “which may” in 1.1. (7) Removed “Definitions of Terms Specific to This Standard:”
(2) Added “such as delaminations, longitudinal continuous and added “Definitions—For definitions of technical terms
voids, or the presence of hollow fibers” in 1.1. pertaining to plastics used in this test method, see Terminology
(3) Removed “The specimen’s cross-section may reflect D883.” in 3.1.
delaminations, longitudinal continuous voids, or the presence (8) Added “3.2 For definitions of terms that appear in this
of hollow fibers, or all three.” in 1.1, Note 1. standard relating to reinforced plastic pultruded products, refer
(4) Removed “The results of a wicking test are dependent on to D3918.”
specimen type and size, penetrant type, time of exposure in the (9) Removed “3.1.1 wicking—transmission of a gas or liquid
penetrant, penetrant viscosity, etc. Any attempt to use a due to pressure differential or capillary action along fibers
wicking test to establish specification criteria should be made incorporated in a fiberglass reinforced pultruded product.”
with great care.” and added “See the significance and use (10) Added “3.3 For definitions of terms that appear in this
section for cautions in using this test method.” in 1.2. standard relating to quality and statistics, refer to Terminology
(5) Added “are not necessarily” and “has the potential to” and E456.”
removed “may not be” and “may” in 1.3. (11) Added “3.4 Definitions of Terms Specific to This Stan-
(6) Added D883 Standard Terminology Relating to Plastics and dard:”
E456 Standard Terminology Relating to Quality and Standards (12) Added “3.4.1 wicking—transmission of a gas or liquid
and removed “E691 Practice for Conducting an Interlaboratory due to pressure differential or capillary action along fibers
Study to Determine the Precision of a Test Method” to 2.1. incorporated in a fiberglass reinforced pultruded product.

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D5117 − 17
(13) Added “are” and “simultaneously” and removed “can be” (24) “should” changed to “shall” in 10.3.
and “in the reinforcement” in 4.2. (25) Added “if contact with the penetrant were to occur.” and
(14) Added “causes” and removed “may cause” in 5.1. removed “should contact with the penetrant occur.” in 10.4.
(15) Added “manufacturing” and removed “manufacture” in (26) “should” changed to “if” and “exist” changed to “exists”
5.2. in 10.12.
(16) “should be made with care” changed to “shall be made (27) Added “12.1 Repeatability Limit—The value below
carefully” and “may” changed to “will” in 5.3. which the absolute difference between two individual test
(17) Deleted “The manufacturing process may also affect the results obtained under repeatability conditions is expected to
quality of the product. It should be useful for a manufacturer in occur with a probability of approximately 0.95 (95%).” and
determining whether any gross changes in quality have taken removed “12.1 Repeatability—The critical difference table
place due to process or raw material changes.” and added “This below was obtained on the same material by a single operator
test method will be useful for a manufacturer to determine
using the same instrument. Two averages of wicking data taken
whether any gross changes in quality have taken place due to
within a single laboratory for a 1 in. (2.54 cm) diameter
process or raw material changes as the manufacturing process
fiberglass reinforced solid rod stock can be considered signifi-
also affects the quality of the product.” in 5.4.
(18) Deleted “It is suggested that such a specification should be cantly different at 95 % confidence if the values differ by more
negotiated between supplier and end user.” and added “A than those listed in the following table.” in 12.1.
specification shall be negotiated between supplier and end user (28) Added “12.2 Reproducibility Limit—The value below
and such specification shall be made with great care.” in 5.5. which the absolute difference between two individual test
(19) Added “has potential to” and removed “could” in 6.4. results obtained under reproducibility conditions is expected to
(20) Added “It was determined that this test method is appli- occur with a probability of approximately 0.95 (95%).” and
cable for all those three resin series.” and removed “It is removed “12.2 Reproducibility—The critical difference table
recognized that this test method will be used with other resin shown below represents data obtained by two different opera-
system and rod-stock sizes.” in 4.2. tors using different instruments in different laboratories. Two
(21) Added “to support the specimen on one end.” and re- averages of wicking data taken in different laboratories for a 1
moved “and upon which the specimens may rest is recom- in. (2.54 cm) diameter fiberglass reinforced solid rod stock can
mended” in 6.5. be considered significantly different at 95 % confidence if the
(22) “should” changed to “shall” in 8.3. values differ by more than those listed in the following table.”
(23) Added “standard laboratory atmosphere” and removed in 12.2
“Standard Laboratory Atmosphere” in 9.2.

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of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5132 − 20

Standard Test Method for


Horizontal Burning Rate of Polymeric Materials Used in
Occupant Compartments of Motor Vehicles1
This standard is issued under the fixed designation D5132; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This test method is intended for use as a small-scale 2.1 ASTM Standards:2
laboratory procedure for comparing the relative horizontal D883 Terminology Relating to Plastics
burning rates of polymeric materials used in occupant com- D5025 Specification for Laboratory Burner Used for Small-
partments of motor vehicles. Scale Burning Tests on Plastic Materials
1.2 During the course of combustion, gases or vapors, or E176 Terminology of Fire Standards
both, are evolved that are potentially hazardous to personnel. E456 Terminology Relating to Quality and Statistics
Adequate precautions shall be taken to protect the operator. E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.3 Units—The values stated in SI units are to be regarded E2935 Practice for Conducting Equivalence Testing in
as standard. Laboratory Applications
1.4 This test method, Federal Safety Standard MVSS 302, 2.2 Federal Safety Standard:
SAE J369, and ISO 3795 address the same subject matter, but MVSS 302 (49 CFR 571.302) Flammability of Interior
differ in technical content. Materials-Passenger Cars, Multipurpose Passenger
1.5 This standard is used to measure and describe the Vehicles, Trucks and Buses3
response of materials, products, or assemblies to heat and 2.3 SAE Standard:
flame under controlled conditions, but does not by itself SAE J369 Flammability of Polymeric Interior Materials -
incorporate all factors required for fire hazards or fire risk Horizontal Test Method4
assessment of materials, products, or assemblies under actual
2.4 ISO Standard:
fire conditions.
ISO 3795 Road vehicles, and tractors and machinery for
1.6 This standard does not purport to address all of the agriculture and forestry—Determination of burning be-
safety concerns, if any, associated with its use. It is the havior of interior materials5
responsibility of the user of this standard to establish appro- ISO 13943 Fire Safety—Vocabulary
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3. Terminology
Specific hazard statements are given in Section 7.
1.7 Fire testing is inherently hazardous. Adequate safe- 3.1 Definitions—For definitions of terms relating to plastics,
guards for personnel and property shall be employed in the definitions in this test method are in accordance with
conducting these tests. Terminology D883. For terms relating to fire, the definitions in
NOTE 1—There is no known ISO equivalent to this standard. this test method are in accordance with Terminology E176 and
ISO 13943. In case of conflict, the definitions given in
1.8 This international standard was developed in accor-
Terminology E176 shall prevail. For terms relating to precision
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
2
mendations issued by the World Trade Organization Technical For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Barriers to Trade (TBT) Committee. Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3
United States Code of Federal Regulations, 49 CFR 571.302, 36 FR 28991,
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics available from Superintendent of Documents, U.S. Government Printing Office,
and is the direct responsibility of Subcommittee D20.30 on Thermal Properties. Washington, DC 20402.
4
Current edition approved Feb. 1, 2020. Published March 2020. Originally Available from Society of Automotive Engineers (SAE), 400 Commonwealth
approved in 1990. Last previous edition approved in 2019 as D5132 – 19. DOI: Dr., Warrendale, PA 15096-0001.
10.1520/D5132-20.

*A Summary of Changes section appears at the end of this standard


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D5132 − 20
and bias and associated issues, the terms used in this test 6.1.1 Test Chamber—A chamber approximately 380 by 355
method are in accordance with the definitions in Terminology by 200 mm constructed of 1.25–1.50 mm steel sheet and
E456. fabricated in accordance with Fig. 1.
6.1.2 Laboratory Burner—Constructed in accordance with
4. Summary of Test Method Specification D5025.
4.1 This test method employs a standard test specimen (100 NOTE 2—It is acceptable to mount the burner on the door, as shown in
by 356 mm) with a thickness up to 13 mm, mounted in a Fig. 6, to ensure proper alignment.
U-shaped metal frame. The specimen is ignited by means of a 6.1.3 Gas Supply—Methane or natural gas having a heating
38 mm high flame from an appropriate burner, and the burning value of 37 6 1 MJ/m3.
rate of the material is determined. 6.1.4 Specimen Holder Support—A device capable of main-
4.2 The rate of burning is determined by measurements of taining the specimen holder horizontally in place so that the top
the horizontal distance burned in relation to the time of of the burner tube is positioned 19 mm below the top surface
burning, and reported for each set of specimens. of the bottom U-shaped frame when placed in the specimen
holder support, as shown in Fig. 2 and Fig. 3. The base of the
5. Significance and Use support shall not obstruct the ventilation holes in the base of
5.1 This test method provides a standard laboratory proce- the cabinet.
dure for measuring and comparing the burning rates of NOTE 3—Limited data indicates that the use of a “drip tray” under the
polymeric materials under specified controlled conditions. specimen holder does not significantly affect the test results. If differences
are observed by the testing laboratory, the drip tray shall be removed.
5.2 The rate of burning is affected by such factors as density,
direction of rise, and type and amount of surface treatments. 6.1.5 Specimen Holder—Two matching U-shaped frames of
The thickness of the finished specimens must also be taken into non-corroding metal stock 25 mm wide and 10 mm high. The
account. These factors must be considered in order to compare interior dimensions of the U-shaped frames are 50 mm wide by
materials on the same basis. 330 mm long. A specimen that softens and bends at the flaming
end so as to cause erratic burning is kept horizontal by supports
5.3 In this procedure, the specimens are subjected to one or consisting of thin, heat-resistant wires, spanning the width of
more specific sets of laboratory test conditions. If different test the U-shaped frame under the specimen at 25-mm intervals. A
conditions are substituted or the end-use conditions are device that is suitable for use for supporting this type of
changed, it is not always possible by or from this test method material is an additional U-shaped frame containing the
to predict changes in the fire-test-response characteristics specimen, spanned by 0.25-mm wires of heat-resistant compo-
measured. Therefore, the results are valid only for the fire test sition at 25 mm intervals starting 38 mm from the open end.
exposure conditions described in this procedure. The device is inserted over the bottom U-shaped frame. See
Fig. 4 and Fig. 5.
6. Apparatus 6.1.6 Timing Device—A timer accurate to the nearest 0.1 s.
6.1 The apparatus shall be as shown in Figs. 1-6 and shall 6.1.7 Measuring Device—A rule accurate to the nearest 1.0
include the following: mm.

FIG. 1 Horizontal Flammability Chamber

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D5132 − 20

FIG. 2 Typical Specimen Holder Support

FIG. 3 Specimen Holder With Specimen Positioned in the Specimen Holder Support

FIG. 4 Typical Specimen Holder—Two Identical U-Shaped Frames

7. Hazards mm are prepared by cutting from the test material. If the test
7.1 During the course of combustion, gases or vapors, or material has a coating, covering, or construction that is
both, are evolved and have the potential to be hazardous. considered directional in nature, and it has a directional effect
Precautions shall be taken to protect the operator. on the burning rate, then specimens are produced by cutting
five specimens in both the transverse and longitudinal direc-
8. Test Specimens tions.
8.1 A minimum of five specimens 100 6 5 mm wide by a 8.2 Cut specimens from uniform density samples. The
minimum of 300 mm long by thickness up to a maximum of 13 maximum thickness of any specimen shall be 13 mm. If any

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D5132 − 20

FIG. 5 Bottom U-Frame

FIG. 6 Burner Position Inside Cabinet

material to be tested exceeds this, it shall be cut to the above posite materials, all the layers within a depth of 13 mm from
thickness by a mechanical process applied to the side which the surface facing towards the occupant compartment shall be
does not face the occupant compartment, so that the specimen tested individually, as shown at the Fig. 7. Any material that
shall include the primary surface of the part. In case of does not adhere to other materials at every point of contact
materials made of different composition which are not com- shall be tested separately. Any material that adheres to other

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D5132 − 20

NOTE 1—Material A has a non-adhering interface with material B and is tested separately. Part of material B is within 13.0 mm of the occupant
compartment air space, and materials B and C adhere at every point of contact; therefore B and C are tested as a composite. The cut is in material C as
shown, to make a specimen 13.0 mm thick.
FIG. 7 Specimen Preparation (Illustrative Example)

materials at every point of contact shall be tested as a 10.2 Place samples with napped or tufted surface on a flat
composite with other material(s). Record the information on surface and comb twice against the nap using the metal comb
specimen preparation in the test report. at least 110 mm in length, with seven to eight teeth per 25 mm.
8.3 Where it is not possible to obtain a flat specimen 10.3 Place the test specimen between the two matching
because of the component configuration, cut the specimen to U-shaped frames so that the frames hold both long sides and
the maximum thickness of 13 mm at any point, from the area one end of the specimen.
with the least curvature, and in such a manner as to include the
face side. 10.4 Place the burner remote from the specimen, ignite, and
8.4 The minimum width and length of the specimen shall be adjust it to produce a blue flame 38 6 2 mm high. Adjust the
95 and 300 mm, respectively. Use the maximum available gas supply and the air ports of the burner until a yellow-tipped
length or width of a specimen (as described in 8.1) where either blue flame is produced and then increase the air supply until the
dimension is less than the specified values. yellow tip just disappears. Measure the height of the flame,
and, if necessary, readjust to obtain a flame 38 mm high.
8.5 For composites, laminates, or surface-treated samples,
the side nearest to the compartment occupant shall be placed 10.5 Place the burner inside the open end of the test
facing down during testing. chamber and position the burner to ensure that the center of the
8.6 If the material’s grain pattern or construction is such that burner top is 19 6 1 mm below the center of the bottom edge
it has a directional effect on the burning rate, conduct the of the specimen at the open end of the specimen holder when
testing in both the transverse and longitudinal directions, as the specimen is in the specimen testing position.
described in 8.1. Test five specimens in each direction. 10.6 Place the mounted specimen in the horizontal testing
position in the specimen holder support inside the test chamber.
9. Conditioning
10.7 Turn on the exhaust hood.
9.1 Unless otherwise agreed upon, materials shall be con-
ditioned for at least 24 h at 23 6 2°C and 50 6 10 % relative 10.8 Move the flame into contact with the specimen for a
humidity prior to testing. period of 15 s, then extinguish the exposure flame by turning
9.2 All specimens shall be tested in a laboratory atmosphere off the gas supply or by removing the flame from under the
of 15 to 35°C and 40 to 75 % relative humidity. For specimen.
convenience, the specimens can be stored up to 1 h in closed 10.9 Observe the leading edge of the flame front, starting
polyethylene bags after conditioning and prior to testing. the timer when the scribed mark 38 mm from the open end of
the sample holder is reached.
10. Procedure
10.1 Place the test chamber inside a laboratory exhaust 10.10 Measure the time it takes the leading edge of the
hood. flame front to progress to the line scribed 292 mm from the
open end of the top or bottom U-shaped frame. If the flame
NOTE 4—The proper control of the hood is necessary to ensure the does not reach this specified end point, time its progress to the
proper draft. Adjust the baffles or the exhaust motor speed, or both, so that
the face velocity of the hood shall be constant in the range of 0.1 m/s [75
furthest distance reached. If the specimen stops burning before
ft/min]. It is possible that the effectiveness of the hood will change when it has burned for 60 s and has not burned more than 50 mm past
the door to the lab is opened and closed. the 38 mm scribed line, no burn rate is calculated.

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D5132 − 20
11. Calculation tories tested ten different materials. Eight laboratories per-
11.1 Calculate the burning rate from the following formula: formed the test method without a drip tray, three laboratories
performed the test method with a drip tray. Every “test result”
B 5 D/T 3 60 (1) represents one individual determination. Laboratories submit-
where: ted test results from a single operator for each material, four
B = burning rate, mm/min, laboratories submitted five replicate test results, one laboratory
D = length the flame traveled, starting from the first scribed submitted four replicate test results. Practice E691 was fol-
line, mm, and lowed for the design and analysis of data, the details are given
T = time for the flame to travel distance D, s in ASTM Research Report No. D20-1238.
13.2 Warning—The data in Table 1 shall not be rigorously
12. Report
12.1 Report the following information:
12.1.1 Complete identification of the material tested, includ-
ing generic description, manufacturer, commercial designation, TABLE 1 Test Method D5132 without drip tray, Burn Rate (mm/
and lot number, color and other information as requested. min.)
12.1.2 Directionality of the specimens, if pertinent. See 8.1 Material
Values, s
and 8.5. Average SrA SRB rC RD
ABS 60.3 7.5 11.7 21.1 32.7
12.1.3 The thickness and type of specimens tested, that is, PVC 37.2 10.3 24.5 29.0 68.5
composite, laminate, finished section, cellular foam, etc. TPO 65.8 4.1 29.0 11.5 81.1
12.1.4 Conditioning treatment. Polystyrene 80.5 7.8 10.1 21.7 28.2
Foam/Fabric 1A 66.3 12.3 26.5 34.5 74.2
12.1.5 Any prior treatment before testing, other than Foam/Fabric 1B 74.0 7.9 25.1 22.1 70.4
cutting, trimming and conditioning. Foam/Fabric 2A 51.4 10.8 18.4 30.2 51.5
12.1.6 Number of specimens tested. Foam/Fabric 2B 53.2 12.6 17.2 35.4 48.3
Foam/PVC 5.9 11.2 14.8 31.4 41.5
12.1.7 Burnt distance in mm, and burning time, in seconds. Polyurethane 6.8 6.1 22.1 17.0 61.8
12.1.8 All calculated single values of burning rate, in mm / A
Sr = within-laboratory standard deviation of the average.
min. B
SR = between-laboratories standard deviation of the avergage.
C
12.1.9 Average burning rate in millimetres per minute when r = 2.83Sr.
D
R = 2.83SR.
the flame reaches the specific end point. Report D and T
separately for each specimen when the flame propagation stops
before reaching the end point.
12.1.10 Describe observations of burning characteristics
such as warping, melting, dripping, charring, etc. applied to acceptance or rejection of material, as those data are
12.2 The report shall contain the following statement: “In specific to the interlaboratory study and are not necessarily
this procedure, the specimens are subjected to one or more representative of other lots, conditions, materials, or laborato-
specific laboratory test conditions. If different test conditions ries. Users of this test method shall apply the principles
are substituted or the end-use conditions are changed, it is not outlined in Practice E691 to generate data specific to their
always possible by or from this test to predict changes in the laboratory and materials, or between specific laboratories.
fire-test-response characteristics measured. Therefore, the re- 13.3 Equivalence testing on numerical data from two
sults are valid only for the fire test exposure conditions sources shall be conducted in accordance with Practice E2935.
described in this procedure.”
13.4 Bias—There are no recognized standards by which to
13. Precision and Bias6 estimate bias of this test method.
13.1 Precision—The precision of this test method is based
on an interlaboratory study conducted in 2002. Eleven labora- 14. Keywords
14.1 burning rate; flame; flexible cellular materials; heat;
6
Supporting data have been filed at ASTM International Headquarters and are motor vehicles; occupant compartments; polymeric materials;
obtainable by requesting Research Report RR:D20-1238. rubber

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D5132 − 20
ANNEX

(Mandatory Information)

A1. ROUND ROBIN RESULTS

A1.1 An interlaboratory study of the Federal Motor Vehicle A1.2 Warning—The data in Table A1.1 shall not be rigor-
Safety Standard (FMVSS) 302 was conducted in 2002. Eleven ously applied to acceptance or rejection of material, as those
laboratories tested ten different materials. Every “test result” data are specific to the interlaboratory study and are not
represents one individual determination. Laboratories submit- necessarily representative of other lots, conditions, materials,
ted test results from a single operator for each material, six or laboratories. Users of this test method shall apply the
laboratories submitted five replicate test results, three labora- principles outlined in Practice E691 to generate data specific to
tories submitted four replicate test results, and one laboratory their laboratory and materials, or between specific laboratories.
submitted three replicate test results. Practice E691 was fol-
lowed for the design and analysis of data.

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D5132 − 20
TABLE A1.1 Burn Rate (mm/min)
Values, s
Material
Average SrA SRB rC RD
ABS 60.7 5.9 12.5 16.5 35.1
PVC 31.4 8.5 20.0 23.8 56.1
TPO 65.5 4.9 27.8 13.8 77.7
Polystyrene 73.6 11.8 20.2 33.1 56.6
Foam/Fabric 1A 68.0 6.7 28.6 18.7 80.2
Foam/Fabric 1B 73.9 5.3 27.5 14.8 76.9
Foam/Fabric 2A 51.6 15.0 25.4 42.0 71.0
Foam/Fabric 2B 53.0 14.0 19.3 39.2 54.2
Foam/PVC 5.0 10.9 14.0 30.4 39.1
Polyurethane 1.1 6.0 6.4 16.9 18.0
A
Sr = within-laboratory standard deviation of the average.
B
SR = between-laboratories standard deviation of the average.
C
r = 2.83Sr.
D
R = 2.83SR.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5132-19)
that may impact the use of this standard. (February 1, 2020)

(1) Revised 3.1.


(2) Added reference to ASTM D883, ASTM E456 and to ISO
13943.

Committee D20 has identified the location of selected changes to this standard since the last issue (D5132-17)
that may impact the use of this standard. (December 1, 2019)

(1) Added D883, E456, and E2935 to Referenced Documents, (5) Deleted Note 6 reference and note as the information
2.1. contained in the note is now included in 13.1.
(2) Added document titles to Referenced Documents, 2.1. (6) Revised Annex A1 to conform to D20 Guidance 4/2/19
(3) Revised 3.1—Definitions—to include reference to E456 for removing statements regarding equivalence of test results
definitions of terms relating to precision and bias and associ- based on repeatability or reproducibility values.
ated issues.
(4) Revised Section 13—Precision and Bias—to conform to
D20 Guidance 4/2/19 removing statements regarding equiva-
lence of test results based on repeatability or reproducibility
values.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5138 − 16

Standard Classification System and Basis for Specification for


Liquid Crystal Polymers Molding and Extrusion Materials
(LCP)1
This standard is issued under the fixed designation D5138; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* health practices and determine the applicability of regulatory


1.1 This classification system covers liquid crystal poly- limitations prior to use.
meric (LCP) materials suitable for injection molding and NOTE 1—There is no known ISO equivalent to this standard.
extrusion. This classification system allows the use of liquid
crystal polymers that are recycled, reconstituted, recycled- 2. Referenced Documents
regrind, recovered, or reprocessed, or a combination thereof, 2.1 ASTM Standards:2
provided that the requirements as stated in this classification D256 Test Methods for Determining the Izod Pendulum
system are met. It is the responsibility of the supplier and the Impact Resistance of Plastics
buyer of liquid crystal polymers that are recycled, D618 Practice for Conditioning Plastics for Testing
reconstituted, recycled-regrind, recovered, or reprocessed, or a D638 Test Method for Tensile Properties of Plastics
combination thereof, to ensure compliance. D648 Test Method for Deflection Temperature of Plastics
1.2 The properties included in this classification system are Under Flexural Load in the Edgewise Position
those required to identify the compositions covered. Other D790 Test Methods for Flexural Properties of Unreinforced
requirements necessary to identify particular characteristics and Reinforced Plastics and Electrical Insulating Materi-
important to specialized applications are allowed. These shall als
be agreed upon between the user and the supplier, by using D883 Terminology Relating to Plastics
suffixes as given in Section 5. D1238 Test Method for Melt Flow Rates of Thermoplastics
by Extrusion Plastometer
1.3 This classification system and subsequent line callout D1600 Terminology for Abbreviated Terms Relating to Plas-
(specification) are intended to be a means of calling out plastic tics
materials used in the fabrication of end-use items or parts. It is D3418 Test Method for Transition Temperatures and En-
not intended for the selection of materials. Material selection thalpies of Fusion and Crystallization of Polymers by
can be made by those having expertise in the plastics field after Differential Scanning Calorimetry
careful consideration of the design and the performance D3641 Practice for Injection Molding Test Specimens of
required of the part, the environment to which it will be Thermoplastic Molding and Extrusion Materials
exposed, the fabrication process to be employed, the costs D3835 Test Method for Determination of Properties of
involved, and the inherent properties of the material other than Polymeric Materials by Means of a Capillary Rheometer
those covered by this classification system. D3892 Practice for Packaging/Packing of Plastics
1.4 The values stated in SI units are to be regarded as D4000 Classification System for Specifying Plastic Materi-
standard. als
1.5 The following precautionary caveat pertains only to the D5630 Test Method for Ash Content in Plastics
test method portion, Section 11, of this classification system: D7209 Guide for Waste Reduction, Resource Recovery, and
This standard does not purport to address all of the safety Use of Recycled Polymeric Materials and Products (With-
concerns, if any, associated with its use. It is the responsibility drawn 2015)3
of the user of this standard to establish appropriate safety and E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications

1 2
This classification system is under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Materials. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2016. Published April 2016. Originally the ASTM website.
3
approved in 1990. Last previous edition approved in 2011 as D5138 - 11. DOI: The last approved version of this historical standard is referenced on
10.1520/D5138-16. www.astm.org.

*A Summary of Changes section appears at the end of this standard


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D5138 − 16
2.2 IEC and ISO Standards:4 ISO 11443 Plastics—Determination of the Fluidity of Plas-
IEC 112 Recommended Method for Determining the Com- tics Using Capillary and Slit-Die Rheometers
parative Tracking Index of Solid Insulation Materials ISO 20753 Plastics—Test Specimens
IEC 243 Recommended Methods of Test for Electrical 2.3 Military Standard:5
Strength of Solid Insulating Materials at Power Frequen- MIL-M-24519 Molding Plastics—Electrical Thermoplastics
cies
ISO 62 Plastics—Determination of Water Absorption 2.4 Underwriters Laboratories (UL):6
ISO 75-1 Determination of Temperature of Deflection Un- UL 94 Test for Flammability of Plastic Materials for Parts in
der Load—General Test Method Devices and Appliances
ISO 75-2 Determination of Temperature of Deflection Under 2.5 National Technical Information Service (NTIS):7
Load—Plastics and Ebonite AD297457 Procedure and Analytical Method for Determin-
ISO 178 Plastics—Determination of Flexural Properties of ing Toxic Gases Produced by Synthetic Compounds
Rigid Materials
ISO 180 Plastics—Determination of Izod Impact Strength of 3. Terminology
Rigid Materials
ISO 294-1 Plastics—Injection Moulding of Test Specimens 3.1 Definitions—Except for the terms defined below, the
of Thermoplastic Materials—General Principles for Injec- terminology used in this classification system is in accordance
tion Molding with Terminologies D883 and D1600.
ISO 527-1 Plastics—Determination of Tensile Properties— 3.2 Definitions of Terms Specific to This Standard:
General Principles 3.2.1 liquid crystal polymer (LCP)—A family of thermo-
ISO 527-2 Plastics—Determination of Tensile Properties— plastic polymers which upon heating to the processing
Test Conditions for Moulding and Extrusion of Plastics temperature, exhibit ordered structure and under shear, highly
ISO 604 Plastics—Determination of Compressive Properties aligned chains that are retained in the solid state. Liquid crystal
ISO 3451-1 Plastics—Determination of Ash Content—Part polymers are polymers that in the molten state exhibit birefrin-
1: General Methods gence in polarized light.
ISO 11357-1 Plastics—Differential Scanning Calorimetry
(DSC)—Part 1: General Principles
ISO 11357-3 Plastics—Differential Scanning Calorimetry
5
(DSC)—Part 3: Determination of Temperature and En- Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
thalpy of Melting and Crystallization dodssp.daps.dla.mil.
6
Available from Underwriters Laboratories (UL), 2600 N.W. Lake Rd., Camas,
WA 98607-8542, http://www.ul.com.
7
Available from National Technical Information Service (NTIS), 5301 Shawnee
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., Rd., Alexandria, VA 22312, http://www.ntis.gov.
4th Floor, New York, NY 10036, http://www.ansi.org.

TABLE LCP Liquid Crystal Polymers—Classification


Group Description Class Description GradeA Description
01 unsubstituted or methyl substituted, wholly aromatic 1 high temperature 0
copolyester, polyether, or polyester amide DTULB >260°C
2 medium temperature 0
DTUL = 220–260°C
3 general purpose 0
DTUL <220°C
02 mixed aromatic/aliphatic copolyesters, polyethers, or 1 high temperature 0
polyester amides DTUL >260°C
2 medium temperature 0
DTUL = 220–260°C
3 general purpose 0
DTUL <220°C
03 aromatic copolyesters, polyethers, or polyesteramides 1 high temperature 0
with aliphatic sidechain DTUL >260°C
2 medium temperature 0
DTUL = 220–260°C
3 general purpose 0
DTUL <220°C
04 blends 1 high temperature 0
DTUL >260°C
2 medium temperature 0
DTUL = 220–260°C
3 general purpose 0
DTUL <220°C
00 other 0 other 0
A
Description unspecified.
B
DTUL is deflection temperature under load measured at 1.8 MPa and is determined in accordance with Table A or Table B.

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D5138 − 16
4. Classification 4.2.2.1 Although the values listed are necessary to include
the range of properties available in existing materials, this does
4.1 The LCP materials are classified into groups according
not imply that every possible combination of properties exists
to their chemical composition. These groups are subdivided,
or can be obtained.
whether reinforced or not, into classes based on thermal
performance as shown in Table LCP. 4.2.3 When the grade or class of the basic material is not
known or is not important, the “0” classification shall be used.
NOTE 2—An example of this classification system is as follows: The
specification LCP0120 indicates the following LCP = liquid crystal poly- NOTE 6—An example of this classification for specifying a reinforced
mer as found in Terminology D1600: LCP material is given as follows: The specification LCP0120G30A22450
01 = Unsubstituted, or methyl substituted, wholly aromatic would indicate the following material requirements:
copolyester, polyether, or polyester amide (group) LCP = Liquid Crystal Polymer as found in Terminology D1600
2 = Medium temperature, DTUL = 220-260°C (class) 01— = Unsubstituted or methyl substituted, wholly aromatic
0 = Other (grade) copolyester, polyether, or polyester amide (group),
2 = medium temperature (class)
4.1.1 To facilitate the incorporation of future or special 0 = unspecified (grade)
materials, the “other” category for Group (00), Class (0), and G30 = Glass reinforced at 30 % nominal level
Grade (0) is shown in Table LCP. A = Table A property requirements
2 = Tensile strength, min, 100 MPa
4.2 Reinforced, filled, and lubricated versions of LCP ma- 2 = Flexural modulus, min, 8 GPa
terials are classified in accordance with Tables LCP and Table 4 = Notched izod impact, min, 15 kJ/m
5 = Deflection temperature under load, min, 260°C at 1.8 MPa,
A. Table LCP is used to specify the group or the group and 0 = Unspecified
class of LCP and Table A is used to specify the property If no properties are specified, the specification would be
requirements. LCP0120G30A00000.

NOTE 3—Test specimens shall be prepared in accordance with


ISO 20753, Specimen Type A1 or Practice D3641 accordingly.
5. Suffixes Requirements
NOTE 4—A similar callout can be developed using Table B. 5.1 When additional requirements are needed that are not
4.2.1 Reinforced, filled, and lubricated variations of the covered by the basic requirements or cell-table requirements,
basic materials are identified by a single letter that indicates the they shall be indicated through the use of suffixes.
filler, or reinforcement used, or both, and two digits that 5.2 A list of suffixes is found in Classification System
indicate the nominal quantity in percent by weight. The D4000 (Table 3) and are used for additional requirements as
reinforcement letter designations and associated tolerance appropriate.
levels are shown in Table 4. 5.2.1 Additional suffixes will be added to that standard as
NOTE 5—This part of the system uses the percent of reinforcements or
test methods and requirements are developed and requested.
additives, or both, in the callout of the modified basic material. The types
and percentages of reinforcements and additives are shown on the 6. General Requirements
suppliers’ technical data sheet unless they are proprietary in nature. If
necessary, additional callout of these reinforcements and additives can be 6.1 The composition of the specified material shall be
accomplished by the use of the suffix part of the system (see Section 5). uniform and shall conform to the requirements specified
4.2.2 Specific requirements shall be shown by a six- herein.
character specification. The specification will consist of the 6.2 The basic requirements from the property tables or cell
letter A and the five digits comprising the cell numbers for the tables are always in effect unless superseded by specific suffix
property requirements in the order as they appear in Table A. requirements, which always take precedence.

TABLE A Property Requirements for Liquid Crystal Polymer Based on ISO Test Methods
0 1 2 3 4 5 6 7 8 9
1 Tensile ISO 527 unspecified 70 100 120 140 160 180 200 220 specify
strength, value
min, MPa
2 Flexural ISO 178 unspecified 4 8 12 16 20 24 28 32 specify
modulus, value
min, GPa
3 Notched ISO 180 unspecified 5 9 12 15 18 25 37 50 specify
izod value
impact,
min, kJ/m2
4 DTULA at ISO 75/A unspecified 140 180 220 240 260 300 340 380 specify
1.8 MPa, value
min,° C
5 To be unspecified specify
determined value
A
DTUL = Deflection temperature under load tested flatwise on 80 by 10 by 4-mm specimen.

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D5138 − 16

TABLE B (Formerly Table A in D5138 – 90) Property Requirements for LCP Based on ASTM Test Methods
0 1 2 3 4 5 6 7 8 9
Tensile strength, MPa, min,A unspecified 70 100 120 140 160 180 200 220 specify value
(D638)
Flex modulus, GPa, min,B unspecified 4 8 12 16 20 24 28 32 specify value
(D790)
Notched Izod unspecified 40 75 100 125 150 200 300 400 specify value
impact, min,
J/m, (D256)C
Deflection temperature, min, unspecified 140 180 220 240 260 300 340 380 specify value
°C at 1.8 MPa, (D648)D
To be determined unspecified specify value
A
Type 1 tensile bar, 3.2 mm thick tested at 5 mm/min ± 25 % (minimum length 200 mm).
B
127 by 12.7 by 3.2-mm bar tested at 1.3 mm/min.
C
Bar thickness 3.2 mm.
D
Test Method D648, Method A.

TABLE 4 Reinforcement-FillerA SymbolsB and Tolerances fied in Table 5 are guidelines only. Since mechanical properties
Symbol Material
Tolerance can vary depending on the molding conditions, contact the
(Based on Total MassA )
manufacturer of the grade for molding conditions appropriate
C carbon and graphite fiber ±2 % for specification purposes.
G glass ±2 %
L lubricants (for example PTFE, depends upon material and 9.3 Because of the shear sensitivity of LCP materials,
graphite, silicone, and process—to be specified occasionally a gate smaller than the gate specified by the
molybdenum disulfide) molding practice or method is required to fill the part ad-
M mineral ±2 %
R combinations of reinforcements ±3 % for the total equately. When reporting data in accordance with a specifica-
or fillers, or both tion (line callout), the gate design shall be reported if different
A
Ash content of filled, or reinforced material, or both, is determined using either than the applicable molding practice ro method requirement.
Test Method D5630 or ISO 3451-1 where applicable.
B
Additional symbols will be added to this table as required. 10. Conditioning
10.1 Test specimens shall be conditioned in the standard
laboratory atmosphere for a minimum of 12 h (condition
7. Detail Requirements 12/23/50 of Practice D618).
7.1 The material shall conform to the requirements pre-
scribed in Tables LCP and A (or B), and the suffix requirements 11. Test Methods
as they apply. 11.1 Determine the properties enumerated in this classifica-
7.2 For the purposes of determining conformance with this tion system by means of the test methods referenced in Section
classification system, all specified limits for a specification 2.
(line callout) based on this classification system are absolute
limits, as defined in Practice E29. 12. Certification and Inspection

7.3 With the absolute method, an observed value or a 12.1 Inspection and certification of the material supplied
calculated value is not rounded, but is to be compared directly with reference to a specification based on this classification
with the limiting value. Conformance or nonconformance is system shall be for conformance to the requirements specified
based on this comparison. herein.
12.2 Lot-acceptance inspection shall be the basis on which
8. Sampling acceptance or rejection of the lot is made. The lot-acceptance
8.1 Sampling shall be statistically adequate to satisfy the inspection shall consist of filler or reinforcement content (if
requirements of 12.4. any).
8.2 A batch or lot shall be constituted as a unit of manufac-
ture as prepared for shipment. A batch or lot is allowed to TABLE 5 Processing Guidelines for Liquid Crystal Polymers for
consist of a blend of two or more production runs. Preparation of Test SpecimensA
Melt Average Mold
9. Specimen Preparation Material Temperature, Cycle Time, s Injection Temperature,
°C Velocity, mm/s °C
9.1 The moisture content of the molding material for the Liquid crystal B
30 ± 5 150–600 90 ± 5
preparation of test specimens shall not exceed 0.01 %. Material polymer
having a moisture content above these limits shall be dried in A
Contact the manufacturer of the grade for more specific molding conditions when
conducting tests for comparison with the requirements of this classification system.
accordance with the instructions of the manufacturer. B
Target melt temperature shall be ±20°C around the melt point. Actual melt
9.2 The test specimens shall be prepared by an injection temperature shall be held at ±3°C of the target. The melt point is defined as the
nominal melt transition temperature as measured by differential scanning
molding process as specified in ISO 294-1 for Table A or calorimetry.
Practice D3641 for Table B. The processing conditions speci-

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D5138 − 16
12.3 Periodic check inspection with a reference to a speci- 12.5 A report of the test results shall be furnished when
fication based on this classification system shall consist of the requested. The report shall consist of the results of the
tests for all requirements of the material under the specifica- lot-acceptance inspections for the shipment, the percent by
tion. Inspection frequency shall be adequate to ensure the weight of recycled plastic as defined in Guide D7209, if
material is certifiable in accordance with 12.4. requested, and the results of the most recent periodic check
12.4 Certification shall be that the material was manufac- inspections.
tured by a process in statistical control, sampled, tested, and
inspected in accordance with this classification system and that 13. Packaging and Package Marking
the average values for the lot meet the requirements of the 13.1 The provisions of Practice D3892 apply to packaging,
specification (line callout). packing, and marking of containers for plastic materials.
NOTE 7—The ASTM publication Manual on Presentation of Data and
Control Chart Analysis, 8th Edition,8 provides detailed information about 14. Keywords
statistical process control. 14.1 aromatic polyester (ARP); classification system; extru-
sion materials; injection molding materials; line call out; liquid
8
Available from ASTM International. Order stock number: MNL7-8TH-EB. crystal polymers (LCP); recycled plastics

SUPPLEMENTARY REQUIREMENTS

The following supplementary requirements shall apply only when specified by the inquiry, contract,
or order for agencies of the U.S. Government.

S1. Special End Uses TABLE S2.1 Property Values for Initial Physical and Electrical
Qualification Testing
S1.1 Unless otherwise specified in the contract or purchase Value Required for Each Type
order, the supplier is responsible for the performance of all of Compound
Type Type
testing and inspections. Except as otherwise specified, the Property Units
GLCP-30F GLCP-50F
supplier is allowed to utilize his own facilities or any commer- Flammability — V-0 V-0
cial laboratory acceptable to the Government. The Government Water absorption %, max 0.08 0.08
Compressive strength MPa 75 75
reserves the right to perform any of the testing or inspections Dielectric strength
set forth in the specification requirements. This testing ensures Short-Time Test 1 kV/mm 18.8 18.8
Short-Time Test 2 kV/mm 18.8 18.8
qualification on a one-time basis unless the manufacturer Tracking index V 120 140
makes a significant change in formulation, raw material, or
process. S3. Quality Assurance
S3.1 Acceptance Criteria—Failure to conform to require-
S2. Physical Requirements ments in Table S2.1 shall result in rejection of the material.
S3.2 Sample Size—The minimum number of test specimens
S2.1 The physical and electrical property requirements for to be tested shall be as specified in Table S3.1.
initial material qualification are given in Table S2.1 and the test S3.3 Test Method—Testing shall be in accordance with the
methods in Table S3.1. Unless otherwise stated, the values are methods specified in Table S3.1.
minimum requirements. S3.4 Conditioning—Standard test specimens shall be con-
ditioned before testing as specified in Table S3.1 and as
described in Section 4.
TABLE S3.1 Sampling and Conditioning for Initial Qualification Testing
Test Method Number
Property to Be Tested Test Method Specimens Conditioning Units
Modified per Tested
Flammability UL 94 125 by 13 mm 10 per UL 94 per UL 94
by thickness
Compressive strength ISO 604 25 by 10 by 4 mm 5 E-48/50+C-96/23/50 MPa
(minimum average)
Water absorption ISO 62 50-mm disk, 3 E-24/100+des+D-48/50 Percent
3 mm thick (maximum average)
Dielectric Strength: IEC 243 S5.1 60 by 60 by 2-mm kV/mm
Short-time test plaque 3 E-48/50+C-96/23/50 (minimum average)
Short-time test 3 E-48/50+D-48/50
Tracking index IEC 112 80 by 10 by 4 mm 4 A V

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D5138 − 16
S4. Conditioning shall be denoted by use of a plus (+) sign between successive conditions.
Examples: C-96/23/50 — Humidity condition; 96 h at 23°C
S4.1 Nomenclature: and 50 % R.H.
S4.1.1 Condition A—As received. D-48/50 — Immersion condition; 48 h at 50°C.
S4.1.2 Condition C—Humidity conditioning. E-48/50 — Temperature condition; 48 h at 50°C.
S4.1.3 Condition D—Immersion conditioning in distilled
S5. Test Method Modification
water.
S4.1.4 Condition E—Temperature conditioning. S5.1 Dielectric Strength:
S4.1.5 Condition des—Dessication condition, cooling over S5.1.1 The test shall be performed under oil at a frequency
silica gel or calcium chloride in a desiccator at 23°C for 16 to not exceeding 100 Hz at the temperature of the final condi-
20 h after temperature conditioning. tioning.
S4.2 Designation— Conditioning procedures shall be des- S5.1.2 Short-Time Test—The voltage shall be increased
ignated as follows: uniformly at the rate of 500 V/s.
S4.2.1 A capital letter indicating the general conditioning.
S4.2.2 A number indicating, in hours, the duration of S6. Toxicity Requirements
conditioning. S6.1 Thermoplastic molding compounds shall be tested for
S4.2.3 A number indicating, in °C, the conditioning tem- toxicity in accordance with NTIS AD297457. Specimens shall
perature. meet the requirements in Table S6.1, expressed as the maxi-
S4.2.4 A number indicating the relative humidity when it is mum level permissible.
controlled. TABLE S6.1 Toxicity When Heated
S4.3 Tolerances: Compounds Units GLCP-30F GLCP-50F
S4.3.1 Relative Humidity—Standard tolerance shall be Carbon dioxide ppm 15 000 15 000
Carbon monoxide ppm 1 000 1 000
610 %. Ammonia ppm 500 500
S4.3.2 Temperature—Standard tolerance shall be 62°C. Aldehydes as HCHO ppm 50 50
For water immersion the standard tolerance shall be 61°C. Cyanide as HCN ppm 50 50
NOTE S4.1—The numbers shall be separated from each other by slant (/) Oxides of nitrogen as NO2 ppm 100 100
Hydrogen chloride ppm 50 50
marks, and from the capital letter by a dash (-). A sequence of conditions

APPENDIXES

(Nonmandatory Information)

X1. MELT VISCOSITY TESTING

X1.1 Determine melt viscosity using a capillary rheometer X1.1.4 Shear Rates—Report at 1000 s–1. Alternatively, run
in accordance with Test Method ISO 11443 or Test Method at constant shear rate of 400 s−1 for 15 min. Interpolate and
D3835 at the following conditions: report viscosities at 5 and 10-min residence time.
X1.1.1 Drying—Minimum 11⁄2 h (maximum 72 h) at 150 6 NOTE X1.1—The test method for flow rates of thermoplastic materials
10°C in a vacuum oven (minimum reduction of 0.05 MPa from by extrusion plastometer (Test Method D1238) is not recommended as a
atmospheric pressure) under N2 bleed. test method for describing liquid crystal polymers because of the
X1.1.2 Temperature—0-20°C above the nominal melt tran- morphological nature of the material. The LCPs maintain a crystalline
structure even at their processing temperatures. They are highly shear
sition peak as determined in accordance with Test Method
sensitive, and are difficult to process under the low shear rate of the flow
ISO 11357-3 or Test Method D3418 differential scanning rate test. Repeatability of flow rate value is poor. Melt viscosity by
calorimetry using second melting curve at 20°C/min. capillary rheology at appropriate shear rate(s) should be used to describe
X1.1.3 Capillary Die—1-mm diameter, 20:1 L/D, 180° full the flow properties of these materials.
entrance angle.

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D5138 − 16

X2. MILITARY SPECIFICATION M-24519

X2.1 The following Specification D5138 call outs describe


the LCP materials referenced in Military Specification MIL-
M-24519 under the appropriate MIL SPEC callout:
Specification D5138 MIL-M-24519

LCP0120G30A43430 EA300ED035EE200EF140 GLCP-30F


LCP0120G50A44230 EA300ED042EE200EF180 GLCP-50F

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5138 - 11)
that may impact the use of this standard. (April 1, 2016)

(1) Replaced ISO 3167 reference with ISO 20753. (3) Added Note 7 added.
(2) Replaced Specimen 1A with specimen A1 in Note 3. (4) Added title to Table 1 and footnotes.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

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United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5155 − 19

Standard Test Methods for


Polyurethane Raw Materials: Determination of the
Isocyanate Content of Aromatic Isocyanates1
This standard is issued under the fixed designation D5155; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* mendations issued by the World Trade Organization Technical


1.1 These test methods are used to measure the isocyanate Barriers to Trade (TBT) Committee.
content of aromatic isocyanates used as polyurethane raw 2. Referenced Documents
materials.
1.1.1 Test Method A—Unheated toluene-dibutylamine deter- 2.1 ASTM Standards:2
mines the toluene diisocyanate content, the amine equivalent D883 Terminology Relating to Plastics
and the isocyanate content of refined toluene-2,4-diisocyanate D1193 Specification for Reagent Water
and toluene-2,6-diisocyanate, or mixtures of the two. Other E180 Practice for Determining the Precision of ASTM
isomers, if present, will be included in the determination. This Methods for Analysis and Testing of Industrial and Spe-
test method is also applicable to other isocyanates of suitable cialty Chemicals (Withdrawn 2009)3
reactivity and solubility. E456 Terminology Relating to Quality and Statistics
1.1.2 Test Method B—Heated toluene-dibutylamine deter- E691 Practice for Conducting an Interlaboratory Study to
mines the amine equivalent and the isocyanate content of crude Determine the Precision of a Test Method
or modified isocyanates derived from toluene diisocyanate, E2935 Practice for Conducting Equivalence Testing in
methylene di-(4-phenylisocyanate) and polymeric (methylene Laboratory Applications
phenylisocyanate). 2.2 ISO Standard:
1.1.3 Test Method C—Unheated trichlorobenzene-toluene- ISO 14896 Polyurethane Raw Materials-Determination of
dibutylamine determines the amine equivalent and the isocya- Isocyanate Content
nate content of crude or modified isocyanates derived from 3. Terminology
toluene diisocyanate, methylene-di-(4-phenylisocyanate) and
polymeric (methylene phenylisocyanate). 3.1 Definitions—Terms used in this standard are defined in
accordance with Terminology D883, unless otherwise speci-
1.2 The values stated in SI units are to be regarded as fied. For terms relating to precision and bias and associated
standard. No other units of measurement are included in this issues, the terms used in this standard are defined in accordance
standard. with Terminology E456.
1.3 This standard does not purport to address all of the 3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the 3.2.1 amine equivalent—the weight of sample that will
responsibility of the user of this standard to establish appro- combine with 1.0-g equivalent weight of dibutylamine.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3.2.2 assay—the percent by weight of toluene diisocyanate
present in the sample.
NOTE 1—Method C of this test method is equivalent to Method B of
ISO 14896.
3.2.3 isocyanate (NCO) content—the percent by weight of
NCO groups present in the sample.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard- 4. Summary of Test Methods
ization established in the Decision on Principles for the 4.1 In all three test methods, the isocyanate sample is
Development of International Standards, Guides and Recom- reacted with an excess amount of dibutylamine to form the

1 2
These test methods are under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Materials - Plastics and Elastomers. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Aug. 1, 2019. Published August 2019. Originally the ASTM website.
approved in 1991. Last previous edition approved in 2014 as D5155 - 14ɛ1. DOI: 3
The last approved version of this historical standard is referenced on
10.1520/D5155-19. www.astm.org.

*A Summary of Changes section appears at the end of this standard


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D5155 − 19
corresponding urea. The NCO content is determined from the tion of the sample with insoluble urea. Therefore, blanket the
amount of dibutylamine consumed in the reaction. The test sample with dry air or nitrogen at all times. (Warning—
methods differ in the reaction conditions, or solvents used, or Diisocyanates are eye, skin and respiratory irritants at concen-
both. trations above the occupational exposure limit (TLV or PEL).
4.1.1 Test Method A—The sample is added to an excess Diisocyanates can cause skin and respiratory sensitization
amount of dibutylamine in toluene and allowed to stand at (asthma) in some people. Once sensitized, further exposure to
room temperature for 15 min. The reaction mixture is diluted diisocyanates should be eliminated. A combination of engi-
with isopropyl alcohol, and the excess dibutylamine is back- neering controls and personal protective equipment, including
titrated with hydrochloric acid. respiratory, skin and eye protection, may be used to prevent
4.1.2 Test Method B—The sample is added to an excess over-exposure to diisocyanates. Consult the product suppliers’
amount of dibutylamine in toluene and stirred for 20 min. The Safety Data Sheet (SDS) for more detailed information about
resulting solution is then heated rapidly to 100°C, removed potential health effects and other specific safety and handling
from the heat, and allowed to stand for 30 min. The reaction instructions for the product.)
mixture is diluted with isopropyl alcohol, and the excess
dibutylamine is back-titrated with hydrochloric acid. 9. Test Conditions
4.1.3 Test Method C—The sample is added to an excess 9.1 Since isocyanates react with moisture, keep the labora-
amount of dibutylamine in toluene and trichlorobenzene. The tory humidity low, preferably below 50 % relative humidity.
resulting solution is allowed to stand until it has cooled to room
temperature. The reaction mixture is diluted with methanol and TEST METHOD A—UNHEATED TOLUENE-
back-titrated with hydrochloric acid. DIBUTYLAMINE

5. Significance and Use 10. Apparatus


5.1 These test methods are to be used for research or for 10.1 Any weighing device that weighs a liquid by difference
quality control to characterize isocyanates used in polyurethane to the nearest 0.001 g.
products. 10.2 Cooling Bath—Any container approximately 50 mm
deep filled with ice and water.
6. Interferences
10.3 Pipet capable of reproducibly delivering 50 6 .05 mL.
6.1 Phosgene, the carbamyl chloride of the isocyanate,
hydrogen chloride, and any other acidic or basic compounds 10.4 Buret capable of dispensing 0.05 mL at a time.
will interfere. In refined isocyanates, these impurities are
11. Reagents
usually present in such low amounts that they do not affect the
determination. While some crude or modified isocyanates 11.1 Bromocresol Green Indicator Solution—Using 1.5 mL
contain acidities of up to approximately 0.05 %, the NCO of 0.1 N sodium hydroxide, extract the bromocresol green from
content is not normally corrected. 0.100 g of bromocresol green indicator-grade powder, stirring
vigorously until the amount of insoluble residue remains
7. Reagents and Materials constant. Decant the aqueous portion into a 100-mL volumetric
7.1 Purity of Reagents—Reagent grade chemicals shall be flask and dilute to the mark with water.
used in all tests. Unless otherwise indicated, it is intended that 11.2 Dibutylamine Solution (260 g/L)—Dilute 260 g of dry
all reagents shall conform to the specifications of the Commit- dibutylamine to 1 L with dry toluene. Dry the solution with a
tee on Analytical Reagents of the American Chemical Society, drying agent.5
where such specifications are available.4 Other grades are
11.3 Hydrochloric Acid (1 N)—Prepare 1 N HCl (hydro-
allowed, provided it is first ascertained that the reagent is of
chloric acid) and standardize frequently enough to detect
sufficiently high purity to permit its use without lessening the
changes of 0.001 N.
accuracy of the determination.
11.4 Isopropyl Alcohol.
7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water as defined 11.5 Toluene, dry with a drying agent.5
by Types I through IV of Specification D1193.
12. Procedure
8. Sampling 12.1 Run sample and blank determinations side by side.
8.1 Since organic isocyanates react with atmospheric Run the blank determination exactly as described in 12.2 –
moisture, take special precautions in sampling. Usual sampling 12.4, but without adding the sample.
methods, even when conducted rapidly, can cause contamina- 12.2 Add a magnetic stirring bar and 40 mL of dry toluene
to a 500-mL Erlenmeyer flask that has been rinsed successively
4
Reagent Chemicals, American Chemical Society Specifications, American with water, alcohol, and high-purity acetone, dried at 100°C,
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
5
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia The 4A Molecular Sieve, or its equivalent, has been found suitable. The 4A
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, Molecular Sieve is available from VWR International,Inc., 1310 Goshen Parkway,
MD. West Chester, PA 19380.

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D5155 − 19
and allowed to cool in a desiccator. Accurately add, by pipet or N = normality of the HCl, meq/mL,
buret,6 50 mL of dibutylamine solution and mix carefully. W = sample used, g,
12.3 While stirring the contents of the flask, slowly add 6.5 87.08 = equivalent weight of TDI, mg/meq,
to 7.0 g of the sample weighed to the nearest 0.001 g (Note 2). 1000 = conversion from g to mg, and
100 = conversion to percent.
Wash down the sides of the flask with 10 mL of dry toluene,
then stopper the flask loosely and allow it to stand at room
14. Precision and Bias8
temperature for 15 min.
14.1 Attempts to develop a precision and bias statement for
NOTE 2—If spattering is anticipated, cool the flask and contents in the
this test method have not been successful due to the limited
cooling bath before adding the sample and continue to cool until the heat
of reaction is dissipated. Add 10 mL of dry toluene, stopper the flask number of laboratories participating in round-robin tests. Data
loosely, and allow the contents to come to room temperature. on precision and bias are not given for this reason. Anyone
12.4 Add 225 mL of isopropyl alcohol and 0.8 mL of wishing to participate in the development of precision and bias
bromocresol green indicator solution. Titrate with 1 N HCl data are to contact the Chairman, Subcommittee D20.22
solution in a 50 or 100-mL buret7 while stirring the flask (Section D20.22.01), ASTM, 100 Barr Harbor Drive, West
contents with the magnetic stirring bar. Near the end point, Conshohocken, PA 19428.
slowly add the HCl dropwise. The end point is reached when 14.2 A limited round robin was conducted.
the blue color disappears and a yellow color appears that 14.2.1 It has been estimated that the maximum expected
persists for at least 15 s (Note 3). difference between two test results for the same material,
obtained by the same operator using the same equipment on the
NOTE 3—Alternatively, the end point is determined using a potentio-
metric titrator and electrodes. When using this apparatus, it occasionally is same day in the same laboratory due solely to the method is
necessary to transfer the solution to a 600-mL beaker prior to titration. 0.4 % TDI.
After transfer, rinse the Erlenmeyer flask with 25 mL of isopropyl alcohol 14.2.2 It has been estimated that the maximum expected
and add the rinse to the 600-mL beaker. To titrate, immerse the calomel difference between two test results for the same material,
and glass electrodes or a combination electrode of the pH meter
(standardized with pH 4.0 and pH 7.0 standard buffers) and titrate the
obtained by different operators using different equipment in
sample to the break that occurs at approximately pH 4.2 to 4.5 with 1.0 N different laboratories due solely to the method is 0.8 % TDI.
HCl while stirring the solution with a stirring bar. 14.3 There are no recognized standards by which to esti-
13. Calculation mate the bias of this test method.
13.1 Calculate the assay as follows: 14.4 For information on equivalence, refer to Test Methods
E2935.
~ B 2 S !~ N !~ 87.08!~ 100!
%TDI 5 (1)
1000~ W ! TEST METHOD B—HEATED TOLUENE-
DIBUTYLAMINE
When constants are combined, this equation reduces to:
~ B 2 S !~ N !~ 8.708! 15. Apparatus
%TDI 5 (2)
~W! 15.1 Potentiometric Titrator, or pH meter.
13.2 Calculate the amine equivalent as follows:
15.2 Combination pH Electrode.
1000~ W !
Amine Equivalent 5 (3) 15.3 Any weighing device suitable for weighing a liquid
N~B 2 S!
sample by difference to the nearest 0.001 g.
13.3 Calculate the percent NCO as follows:
15.4 Magnetic Stirrer.
42.02~ B 2 S !~ N !~ 100!
%NCO 5 (4) 15.5 Thermometer, from − 10 to 100°C range.
1000~ W !
15.6 Pipet or buret capable of reproducibly delivering 25 6
When constants are combined, this equation reduces to: 0.025 mL.
4.202~ B 2 S !~ N !
%NCO 5 (5) 16. Reagents
~W!
where: 16.1 Dibutylamine Solution (260 g/L)—Dilute 260 g dry
B = HCl required for titration of the blank, mL, dibutylamine to 1 L with dry toluene.
S = HCl required for titration of the sample, mL, 16.2 Hydrochloric Acid (1 N)—Prepare 1 N hydrochloric
acid (HCl) and standardize frequently enough to detect changes
of 0.001 N.
6
Pipets and burets shall conform to National Institute of Standards and
Technology tolerances, as given in Peffer, E. L., and Mulligan, G. C., “Testing of
16.3 Isopropyl Alcohol, 99 % minimum purity.
Glass Volumetric Apparatus,” NIST Circular C434, 1941, available from the 16.4 Toluene, dry, dried with a drying agent.5
Superintendent of Documents, U.S. Government Printing Office, Washington, DC
20025.
7
If an isocyanate monomer other than TDI is used, substitute the equivalent
8
weight of the material being analyzed. The calculated assay result will be percent by Supporting data are available from ASTM Headquarters. Request RR:D20-
weight of the monomer used. 1089.

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D5155 − 19
17. Procedure on precision and bias are not given for this reason. Anyone
17.1 Add 50 mL of dry toluene to a dry 600-mL beaker. wishing to participate in the development of precision and bias
Pipet 256 mL of the dibutylamine solution into the beaker. data are to contact the Chairman, Subcommittee D20.22
Swirl the beaker to mix the contents. (Section D20.22.01), ASTM International, 100 Barr Harbor
Drive, West Conshohocken, PA 19428.
17.2 Transfer to the beaker 0.02 to 0.03 equivalents of the
sample weighed to the nearest 0.001 g. The amount of sample 19.2 A limited round robin was conducted.
needed is calculated from the following equation: 19.2.1 It has been estimated that the maximum expected
105 difference between two test results for the same material,
weight of sample ~ g ! 5 (6) obtained by the same operator using the same equipment on the
expected % NCO
same day in the same laboratory due solely to the method is
Start the magnetic stirrer carefully and rinse the sides of the 0.80 amine equivalents (0.2 % at 30.0 % NCO).
beaker with an additional 10 mL of dry toluene. Cover the 19.2.2 It has been estimated that the maximum expected
beaker and continue mixing for an additional 20 min. difference between two test results for the same material,
17.3 Place the beaker on a hot plate with the −10 to 100°C obtained by different operators using different equipment in
thermometer in the sample. Heat the sample mixture rapidly different laboratories due solely to the method is 2.0 amine
with stirring, so that the solution reaches a temperature of 95 to equivalents (0.4 % at 30 % NCO).
100°C in 31⁄2 to 41⁄2 min. Do not overheat. Quickly remove the
19.3 There are no recognized standards by which to esti-
beaker from the hot plate, cover it with a watchglass, and allow
mate the bias of this test method.
it to stand for 30 min.
17.4 Cool the beaker and contents to room temperature and 19.4 For more information on equivalence, refer to Test
add 225 mL of isopropyl alcohol. Methods E2935.
17.5 Titrate potentiometrically with 1.0 N HCl to the break TEST METHOD C—UNHEATED
that occurs at apparent pH approximately 4.2 to 4.5 (for manual TRICHLOROBENZENE-TOLUENE-DIBUTYLAMINE
titration see Note 4, below).
17.6 Prepare and titrate a blank exactly as described in 17.1 20. Apparatus
– 17.5, but without adding the sample. 20.1 Potentiometric Titrator, or pH meter (Note 4).
18. Calculation 20.2 Calomel Reference Electrode and Indicator Electrode
or a Combination pH electrode.
18.1 Calculate the amine equivalent as follows:
1000~ W ! 20.3 Any weighing device suitable for weighing a liquid
Amine Equivalent 5
N~B 2 S!
(7) sample by difference to the nearest 0.001 g.
18.2 Calculate the percent NCO as follows: 20.4 Magnetic Stirrer.
42.02 ~ B 2 S ! ~ N ! ~ 100! 20.5 Pipet or buret capable of reproducibly delivering
% NCO 5 (8)
1000~ W ! 20 6 0.02 mL.
When constants are combined, this equation reduces to: NOTE 4—If a potentiometric titrator is not available; the titration is
performed using a conventional 50-mL buret and bromophenol blue
4.202 ~ B 2 S ! N indicator (0.04 % aqueous bromophenol blue, sodium salt, reagent grade).
% NCO 5 (9) Titrate the blank and the sample solutions to the first appearance of a
~W!
stable yellow color. (The solution will change from a blue color at the start
B = HCl required for titration of blank, mL, of the titration, to a bluish-green intermediate color, to a yellow color at
S = HCl required for titration of sample, mL, the end point. Recognition of the end point is a matter of experience, but
better defined color changes are obtained when the acid is titrated rapidly
N = normality of HCl, meq/mL, into the solution until the first flash of yellow color is observed. This flash
W = sample used, g, and of color normally appears within a few tenths of a millilitre of the end
4.202 = constant combining the equivalent weight of NCO point.)
(42.02) mg/meq, conversion of g to 1000 mg, and
conversion to 100 % 21. Reagents
19. Precision and Bias9 21.1 Dibutylamine.
19.1 Attempts to develop a precision and bias statement for 21.2 Methanol.
this test method have not been successful due to the limited
21.3 Toluene, dry, dried with a drying agent.5
number of laboratories participating in round-robin tests. Data
21.4 Trichlorobenzene-1,2,4 (TCB) —Dry over Type 4A
9
Supporting data are available from ASTM Headquarters. Request RR:D20-
molecular sieves.
1040. The precision estimates are based on an interlaboratory study performed in
21.5 Dibutylamine Solution (2 N)—Dilute 260 g of dibu-
1989 on one sample each of Lupranate M20S (BASF), PAPI 20 and Isonate 143L
(Dow), Mondur PF (Bayer), and Rubinate HF185 (Rubicon). Eleven industrial tylamine to 1 L with dry toluene and dry over Type 4A
laboratories participated in the test method evaluation. molecular sieves.

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21.6 Methanolic Hydrochloric Acid (1 N)—Prepare 1 N conditions during operation also are to be reported, such as any
hydrochloric acid from methanol and concentrated HCl. Stan- heating required to effect solution before titration, or end point
dardize frequently enough to detect changes of 0.001 N (Note identified different from that described in 22.5.
5).
25. Precision and Bias9
NOTE 5—In order to have homogenous titrations, it is recommended
that methanolic HCl be used in this procedure. If desired, aqueous HCl is 25.1 Table 1 is based on a round robin involving nine
used. However, turbidity will be encountered in some titrations. It is laboratories and conducted in 1991 in accordance with Practice
recommended that 200 to 250 mL of methanol be added to the reacted E180. All labs used potentiometric titration for the generation
product to minimize the formation of two layers. Experience has shown
that if the mixtures are agitated vigorously, inhomogeneity is tolerated of the data used in this study. Except for MDI and TDI, all the
without adversely affecting the results. samples were prepared at one source, but the individual
specimens were prepared at the laboratories that tested them.
22. Procedure The MDI and TDI samples were freshly produced material at
22.1 Add 25 mL of TCB to a dry 250-mL wide-mouth the laboratory site. Each test result was the average of two
Erlenmeyer flask. Pipet 20 mL of the dibutylamine solution individual determinations. (Warning—The following explana-
into the flask. Swirl to mix the contents. tions of r and R (25.2.1 – 25.2.3) are intended only to present
a meaningful way of considering the approximate precision of
22.2 Transfer the approximate amount of sample required
this test method. The data in Table 1 are not to be rigorously
weighed to the nearest 0.001 g to the flask. The approximate
applied to the acceptance or rejection of material, as those data
amount of sample required is calculated from the following
are specific to the round robin and not necessarily representa-
equation:
tive of other lots, conditions, materials, or laboratories. Users
84 of this test method are to apply the principles outlined in
weight of sample, g 5 (10)
expected % NCO Practice E180 or E691 to generate data specific to their
22.3 Cover the flask and swirl the contents until the solution laboratory and materials or between specific laboratories. The
is homogeneous. The reaction mixture will warm to approxi- principles of 25.2.1 – 25.2.3 then would be valid for such data.)
mately 40°C. 25.2 Precision
22.4 Let the sample stand until the reaction mixture reaches 25.2.1 Repeatability, (r)—It has been determined that the
room temperature (20 to 25 min) and add 100 mL of methanol maximum expected difference between two test results for the
to the flask (see Note 4). same material, obtained by the same operator using the
equipment on the same day in the same laboratory due solely
22.5 Titrate potentiometrically with 1.0 N HCl to the break
to the method is r.
that occurs at apparent pH approximately 4.2 to 4.0.
25.2.2 Reproducibility, (R)—It has been estimated that the
22.6 Prepare and titrate a blank exactly as described in 22.1 maximum expected difference between two test results for the
– 22.5, but without adding the sample. same material, obtained by different operators using different
equipment in different laboratories due solely to the method is
23. Calculation R.
23.1 Calculate the amine equivalent as follows: 25.2.3 There are insufficient degrees of freedom to make a
1000~ W ! statistically acceptable determination for TDI. The data in
Amine Equivalent 5 (11) Table 1 are provided for information only. The precision for
N~B 2 S!
TDI isomers is expected to be similar to results obtained for
23.2 Calculate the percent NCO as follows: MDI.
42.02 ~ B 2 S ! ~ N ! ~ 100!
% NCO 5 (12) 25.3 There are no recognized standards by which to esti-
1000 ~ W !
mate the bias of this test method.
When constants are combined, this equation reduces to:
4.202 ~ B 2 S ! N
% NCO 5 (13) TABLE 1 Round-Robin Percent NCO Data In Accordance with
~W!
PracticeE180A
where: Average Sr B SR C rD RE dfF
B = HCl required for titration of blank, mL, Lupranate M20S 31.30 0.082 0.206 0.230 0.577 9
Rubinate 1850 30.78 0.082 0.194 0.230 0.543 9
S = HCl required for titration of sample, mL, PAPI 20 29.57 0.080 0.172 0.224 0.482 8
N = normality of HCl, meq/mL, Isonate 143L 28.83 0.126 0.230 0.353 0.644 9
W = sample used, g, and Mondur PF 22.63 0.048 0.120 0.134 0.336 9
4.202 = constant combining the equivalent weight of NCO MDI 33.53 0.011 0.080 0.031 0.224 6
TDI (see 25.2.3) 48.18 0.078 0.126 0.218 0.353 2
(42.02) mg/meq, conversion of g to 1000 mg, and
A
Values in units of percent NCO.
conversion to 100 %. B
Sr = within-laboratory standard deviation of the replicates.
C
SR = between-laboratories standard deviation of the average.
24. Report D
r = within-laboratory repeatability limit = 2.8·Sr.
E
R = between-laboratories reproducibility limit = 2.8·SR.
24.1 The result is reported as the average of duplicates, F
df = degrees of freedom in the data.
expressed as percent NCO, to the nearest 0.01 %. Any unusual

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D5155 − 19
25.4 For information on equivalence, refer to Test Methods
E2935.
26. Keywords
26.1 isocyanates; isocyanates aromatic; methylene-bis-(4-
phenylisocyanate); polymethylene polyphenylisocyanate;
polyurethane; raw materials; test method; titration; toluene
diisocyanate

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5155 –
14ɛ1) that may impact the use of this standard. (August 1, 2019)

(1) Removed non-mandatory language and corrected grammar (3) Removed definitions and statements of equivalency from
throughout. Precision and Bias sections (14, 19, and 25).
(2) Added references to E456 and E2935

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5204 − 19

Standard Classification System and Basis for Specification for


Polyamide-Imide (PAI) Molding and Extrusion Materials1
This standard is issued under the fixed designation D5204; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* ization established in the Decision on Principles for the


1.1 This classification system covers polyamide-imide ma- Development of International Standards, Guides and Recom-
terials suitable for injection molding and extrusion. mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.2 The properties included in this classification system are
those required to identify the compositions covered. It is 2. Referenced Documents
possible that other requirements are necessary to identify
particular characteristics important to specialized applications. 2.1 ASTM Standards:2
The use of suffixes as shown in Section 5 is one way of D149 Test Method for Dielectric Breakdown Voltage and
specifying these requirements. Dielectric Strength of Solid Electrical Insulating Materials
at Commercial Power Frequencies
1.3 This standard allows for the use of recycled materials D150 Test Methods for AC Loss Characteristics and Permit-
provided that specification requirements based upon this clas- tivity (Dielectric Constant) of Solid Electrical Insulation
sification system are met. D256 Test Methods for Determining the Izod Pendulum
1.4 This classification system and subsequent line call-out Impact Resistance of Plastics
(specification) is intended to be a means of calling out plastics D257 Test Methods for DC Resistance or Conductance of
materials used in the fabrication of end items or parts. It is not Insulating Materials
intended for the selection of materials. Material selection needs D618 Practice for Conditioning Plastics for Testing
to be made by those having expertise in the plastics field after D790 Test Methods for Flexural Properties of Unreinforced
careful consideration of the design and the performance and Reinforced Plastics and Electrical Insulating Materi-
required of the part, the environment to which it will be als
exposed, the fabrication process to be employed, the inherent D792 Test Methods for Density and Specific Gravity (Rela-
properties of the material other than those covered by this tive Density) of Plastics by Displacement
classification, and the economics. D883 Terminology Relating to Plastics
1.5 The values stated in SI units are to be regarded as the D1525 Test Method for Vicat Softening Temperature of
standard. (Reporting in inch-pound units is acceptable.) Plastics
D1600 Terminology for Abbreviated Terms Relating to Plas-
1.6 The following precautionary caveat pertains only to the tics
test methods portion, Section 11, of this classification system: D1708 Test Method for Tensile Properties of Plastics by Use
This standard does not purport to address all of the safety of Microtensile Specimens
concerns, if any, associated with its use. It is the responsibility D2863 Test Method for Measuring the Minimum Oxygen
of the user of this standard to establish appropriate safety, Concentration to Support Candle-Like Combustion of
health, and environmental practices and determine the appli- Plastics (Oxygen Index)
cability of regulatory limitations prior to use. D3641 Practice for Injection Molding Test Specimens of
NOTE 1—There is no known ISO equivalent to this standard. Thermoplastic Molding and Extrusion Materials
1.7 This international standard was developed in accor- D3892 Practice for Packaging/Packing of Plastics
dance with internationally recognized principles on standard- D4000 Classification System for Specifying Plastic Materi-
als
1
This classification system is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic
2
Materials. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Aug. 1, 2019. Published August 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1991. Last previous edition approved in 2017 as D5204 - 17. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5204-19. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D5204 − 19
E29 Practice for Using Significant Digits in Test Data to 4.3 Use Table A to specify physical property requirements
Determine Conformance with Specifications for other PAI materials. These properties are shown by a
IEEE/ASTM SI-10 Standard for Use of the International six-character designation. The designation consists of the letter
System of Units (SI): The Modern Metric System A and the five digits comprising the cell numbers for the
2.2 Military and Federal Specifications and Standards:3 property requirements in the order as they appear in Table A.
MIL-P-46179A Plastic Molding and Extrusion Materials, 4.3.1 Although the values listed are necessary to include the
Polyamide-Imide (PAI) range of properties available in existing materials, not every
possible combination of the properties exists or can be ob-
NOTE 2—MIL-P-46179A property requirements are the basis of Clas-
sification System D5204. The Department of Defense adopted Classifica- tained.
tion System D5204 on July 27, 1994, and canceled MIL-P-46179A. 4.3.2 A single letter is used to identify the grade and indicate
2.3 SAE Specifications:4 the major reinforcement or combinations, or both, along with
AMS 3670B Polyamide-Imide Bar, Rod, and Shapes two digits that indicate the percentage of additive(s) by total
Molded or Extruded mass. The reinforcement and additive letter designations and
AMS 3670/1B Unfilled Polyamide-Imide Bar, Rod and associated tolerance levels are shown in Table 1.
TABLE 1 Reinforcement-Filler Symbols and Tolerances
Shapes
AMS 3670/2B Polyamide-Imide Bar, Rod and Shapes 20- Category Material Tolerance

Graphite-3-Polytetrafluoroethylene Filled C Carbon or graphite fiber reinforced ±3 percentage points


AMS 3670/3B Polyamide-Imide Bar, Rod and Shapes 12- G Glass fiber reinforced ±3 percentage points
Graphite-3-Polytetrafluoroethylene Filled L Lubricants ±3 percentage points
M Minerals ±3 percentage points
AMS 3670/4C Polyamide-Imide Bar, Rod and Shapes 30 R Combinations of reinforcements or ±5 percentage points
Glass Fiber fillers, or both
AMS 3670/5C Polyamide-Imide Bar, Rod and Shapes 30 4.3.3 This part of the classification system uses the type and
Carbon Graphite Fiber percentage of additive to designate the modification of the
basic material. To facilitate this designation, the type and
3. Terminology
percentage of additive is frequently shown on the supplier’s
3.1 The terminology used in this classification system is in technical data sheet. If necessary, additional requirements are
accordance with Terminology D883 and D1600. indicated by use of the suffix part of the system, as given in
3.2 Definitions of Terms Specific to This Standard: Section 5.
3.2.1 polyamide-imide (PAI), n—a polymer that is com- 4.3.4 Reinforced, filled, and lubricated versions of PAI
posed of linkages of all random, or all block, or all alternating, materials that are not in Table PAI are classified in accordance
or any combination thereof, amide and imide units in the with Tables PAI and A. Table PAI is used to specify the Group
structural backbone. or group and class of PAI and Table A is used to specify the
property requirements. An example of this classification sys-
4. Classification tem for a polyamide-imide material containing 40 % glass is as
4.1 The polyamide-imide materials are designated PAI, as follows:
specified in Terminology D1600. The designation PAI0130G40A61550
PAI0130 = polyamide-imide from Table PAI,
4.2 Polyamide-imide materials are classified into groups G40 = glass reinforced at 40 % nominal level,
that are subdivided into classes and grades as shown in Table A = Table A physical-property requirements,
6 = tensile strength, 172 MPa, min,
PAI. 1 = elongation, 4 %, min,
4.2.1 An example of this classification system is as follows: 5 = flexural strength, 269 MPa, min,
5 = flexural modulus, 11700 MPa, min, and
The designation PAI012L23 would indicate from Table PAI:
0 = unspecified property.
PAI = Polyamide-imide as found in Terminology D1600,
If no properties are specified, the designation would be PAI0130G40A00000.
01 (Group) = Injection molding material,
2 (Class) = Wear resistance PAI, and
L23 (Grade) = Nominal 20 % graphite and 3 % PTFE with the require- 5. Suffixes
ments given in Table PAI.
5.1 When additional requirements are needed, based on
4.2.2 To facilitate the incorporation of special materials not application, that are not covered by the basic requirements
covered in Table PAI, the “other” category (0) for group, class, (Table PAI) or cell-table requirements (Table A), they are
and grade is shown on the table with the basic properties to be indicated through the use of suffixes.
obtained from Table A.
5.2 Use the suffixes found in Classification System D4000
(Table 3) for additional requirements as appropriate. Additional
3
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, suffixes will be added to Classification System D4000 as test
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
methods and requirements are developed and requested.
dodssp.daps.dla.mil.
4
Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale, 5.2.1 An example of this classification system using a suffix
PA 15096-0001, http://www.sae.org. is as follows:

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D5204 − 19

The designation PAI013G30CBXXX 10. Conditioning


PAI013G30 = polyamide-imide material as described in Table PAI,
C = melting point / softening point from Classification System 10.1 Postcure all test specimens in accordance with the
D4000 manufacturer’s instructions.
B = Test Method D1525, Rate A (Vicat), and
XXX = three digit number indicating minimum value, °C. 10.2 Condition all test specimens for a minimum of 40 h at
23°C and 50 % relative humidity in accordance with 3.1.2 of
5.3 Suffixes for electrical properties, if required, are found Practice D618 after postcuring and before testing.
in Table SE in the Supplementary Requirements section of this
standard. 11. Test Methods
11.1 Determine the properties enumerated in this classifica-
6. General Requirements tion system in accordance with the relevant methods as they
6.1 Basic requirements from Table A, as they apply, are apply.
always in effect unless these requirements are superseded by 11.2 Specify methods for reinforcement and additive con-
specific suffix requirements, which always take precedence. centration.
6.1.1 The material composition shall be uniform and shall
conform to the requirements specified herein. 12. Certification and Inspection
12.1 Inspection and certification of the material supplied
7. Detail Requirements
with reference to a specification based on this classification
7.1 Test specimens for the various materials shall conform system shall be for conformance to the requirements specified
to the requirements prescribed in Table A and the suffix herein.
requirements as they apply.
12.2 Lot acceptance inspection shall be the basis on which
7.2 For the purpose of determining conformance, all speci- acceptance or rejection of the lot is made and shall consist of
fied limits in this specification (line callout) based on this the tests listed, as they apply, as follows: tensile strength at
classification system, are absolute limits, as defined in Practice break, tensile elongation at break, and specific gravity.
E29.
12.3 Periodic check inspection shall consist of the tests
7.2.1 With the absolute method, an observed value or a
specified for all requirements of the material under this
calculated value is not rounded, but is to be compared directly
classification system. Inspection frequency shall be adequate to
with the limiting value. Conformance or nonconformance with
ensure that the material is certifiable in accordance with 12.4
a specification based on this classification system is based on
this comparison. NOTE 4—If any failure occurs, it is acceptable to retest the material to
establish conformity.
8. Sampling 12.4 Certification shall state that the material was manufac-
8.1 Sampling shall be statistically adequate to satisfy re- tured by a process in statistical control, sampled, tested, and
quirements of 12.2. A batch or lot of material is defined as inspected in accordance with this classification system, and
material produced in a single compound blend. that the average values meet the requirements of the specifi-
cation (line call-out).
9. Test Specimen
12.5 A report of the test results shall be furnished when
9.1 Dry pellets before molding test specimens. Pellets dried requested. The report shall consist of the lot-acceptance inspec-
on trays at 149°C (300°F) in a desiccant air drier for a tion for the shipment. The results of the most recent periodic-
minimum of 24 h have been found to be satisfactory for check inspection shall also be furnished when requested by the
injection molding. purchaser.
9.2 Unless otherwise specified, prepare injection and extru- 13. Packaging and Package Marking
sion resins test specimens by injection molding in accordance
with Practice D3641. 13.1 For packing, packaging, and package marking, the
provisions of Practice D3892 shall apply.
NOTE 3—Typical conditions for molding are melt temperature of 315 to
370°C (600 to 700°F) and mold temperature of 195 to 215°C (380 to 14. Keywords
420°F), depending on the product. Because of the equipment requirements
and difficulty associated with molding PAI, the manufacturer normally 14.1 extrusion material; line call-out; molding material;
does all molding of parts. polyamide-imide

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D5204 − 19
TABLE PAI Requirements for Polyamide-Imide Plastics
Tensile Strength,
Test Method Tensile Elongation,
D1708, Test Method Specific Gravity,
Group Description Class Description Grade Description MPa (psi), min D1708, %, min Test Method D792

01 Injection Molding 1 general purpose M00 0 % mineral 158 (23 000) 9 1.36 to 1.39
M03 3 % mineral 158 (23 000) 9 1.39 to 1.43
0 other
2 wear resistance L15 12 % graphite, 3 % PTFE 124 (18 000) 5 1.44 to 1.48
L23 20 % graphite, 3 % PTFE 124 (18 000) 5 1.48 to 1.53
L20 12 % graphite, 8 % PTFE 97 (14 000) 4 1.48 to 1.52
R30 30 % filled 69 (10 000) 4 1.52 to 1.59
R35 35 % filled 110 (16 000) 3 1.56 to 1.60
R45 45 % filled 96 (14 000) 3 1.53 to 1.58
0 other
3 high strength G30 30 % glass fiber 200 (29 000) 4 1.59 to 1.63
C30 30 % carbon fiber 163 (23 600) 4 1.46 to 1.50
0 other
02 Extrusion 1 general purpose M00 0 % mineral 158 (23 000) 9 1.36 to 1.39
M03 3 % mineral 158 (23 000) 9 1.39 to 1.43
0 other
2 wear resistance L15 12 % graphite, 3 % PTFE 124 (18 000) 5 1.44 to 1.48
L23 20 % graphite, 3 % PTFE 124 (18 000) 5 1.48 to 1.53
R30 30 % filled 69 (10 000) 4 1.52 to 1.59
R35 35 % filled 110 (16 000) 3 1.56 to 1.60
R45 45 % filled 96 (14 000) 3 1.53 to 1.58
0 other
3 high strength G30 30 % glass fiber 200 (29 000) 4 1.59 to 1.63
C30 30 % carbon fiber 163 (23 600) 4 1.46 to 1.50
0 other
00 Other 0 other 0 other

TABLE A Detailed Requirements for Special Polyamide-Imides


Designation
Order PropertyA 0 1 2 3 4 5 6 9B

1 Tensile strength,C unspecified 97 114 124 138 159 172 specify value
MPaD (psi), min (14 000) (16 500) (18 000) (20 000) (23 000) (25 000)
2 Elongation,C % , min unspecified 4 5 6 7 8 9 specify value
3 Flexural strength,E unspecified 152 165 193 228 269 290 specify value
MPaD (psi), min (22 000) (24 000) (28 000) (33 000) (39 000) (42 000)
4 Flexural modulus,E unspecified 3860 5030 5520 9660 11 700 15 900 specify value
MPaD (psi), min (560 000) (730 000) (800 000) (1 400 000) (1 700 000) (2 300 000)
5 Izod ImpactF , J/mG unspecified 37 53 64 80 101 117 specify value
(ft · lb ⁄in.), min (0.7) (1.0) (1.2) (1.5) (1.9) (2.2)
A
Physical property data were determined using injection molded and postcured specimens.
B
If a specific value is required it must be shown in the call-out.
C
See Test Method D1708, Speed B, using 3.175 ± 0.05 mm (0.125 in.) thick specimens.
D
MPa X 145 = psi.
E
See Test Method D790, Method 1, Procedure A.
F
See Test Method D256, Method A, using the center portion of a D638, Type I specimen.
G
J/m × 0.01873 = ft · lb ⁄in.

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D5204 − 19
SUPPLEMENTARY REQUIREMENTS

FOR SPECIAL END USES

The following supplementary requirements apply only when specified by the inquiry, contract or
order for agencies of the U.S. Government.

S1. Special End Uses S2. Physical Requirements


S1.1 Unless otherwise specified in the contract or purchase S2.1 Material properties, in addition to those in Tables PAI
order, the supplier is responsible for the performance of and A, are sometimes required for initial material qualifications
acceptance testing per 12.2 of this standard. Except as other- (such as those described in MIL-P-46179A) are given in Table
wise specified, the supplier is permitted to utilize its own S2.1.
facilities or any commercial laboratory acceptable to the
Government. The Government reserves the right to perform S2.2 Electrical requirements for initial material qualifica-
any of the testing or inspections set forth in the specification tions are given in Table SE.
requirements.
TABLE S2.1 Property Values for Initial Qualification Testing
Physical and ASTM Methods Type I Type II Type II Type II Type III Type III Type IV
Thermal Class 1 Class 2 Class 3 Class 1 Class 2
Properties
Flexural Strength, D790 193 165 158 152 290 269 297
min. (Procedure A) (28 000) (24 000) (23 000) (22 000) (42 000) (39 000) (43 000)
MPa (psi)A
Flexural Modulus, D790 3860 5860 5520 5030 9660 11,700 15,900
min. (Procedure A) (560 000) (850 000) (800 000) (730 000) (1 400 000) (1 700 000) (2 300 000)
MPa (psi)
Compressive D695 165 145 124 103 199 248 203
Strength, min. (24 000) (21 000) (18 000) (15 000) (28 900) (36 000) (29 500)
MPa (psi)
Shear Strength, D732 103 89 62 63 110 124 97
min. (15 000) (12 900) (9000) (9200) (16 000) (18 000) (14 000)
MPa (psi)
Deflection Temp. D648 260 260 260 260 260 260 260
at 1820 kPa (264 (500) (500) (500) (500) (500) (500) (500)
psi),
°C (°F), min.
Coefficient of D696 27–36 22–29 22–29 23–31 12–22 9–17 9–27
Linear Thermal (15–20) (12–16) (12–16) (13–17) (7–12) (5–9) (5–15)
Expansion,
10—6 cm/cm/°C
(10—6 in./in./°F)
Thermal C177 0.21–0.28 0.50–0.58 ... ... 0.32–0.40 ... 0.43–0.57
Conductivity (1.5–2.0) (3.5–4.0) ... ... (2.25–2.75) ... (3.0–4.0)
W/m-K
(Btu-in./h-ft2 - °F)B
UL Rating D3801 V0 V0 V0 V0 V0 V0 V0
(UL94)
Smoke Density F814 9 ... ... ... 4 ... 5
Smoldering 220 ... ... ... 50 ... 90
(Dmax)C
Flaming (Dmax)
Oxygen Index, D2863 41 42 42 40 46 45 47
min.D
Water Absorption D570 0.5 0.5 0.5 0.5 0.5 0.5 0.5
wt. %, max.E
Glass Transition D3418 272 ± 2 272 ± 2 272 ± 2 272 ± 2 272 ± 2 272 ± 2 272 ± 2
Temp., Tg °C (°F), (522 ± 5) (522 ± 5) (522 ± 5) (522 ± 5) (522 ± 5) (522 ± 5) (522 ± 5)
min.F
A
MPa × 145 = psi
B
1 W/m = 6.933 Btu-in./h - ft2 - °F
C
Dmax = Maximum specific optical density; specimens are 3 in. × 3 in. by thickness supplied.
D
Type A, self-supporting samples, approximately 4.0 in. × 1⁄2 in. × 1⁄8 in. Test specimens sometimes glow after flaming combustion.
E
24 h immersion
F
Glass transition temperature shall be determined on dry, fully cured specimens.

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D5204 − 19
S3. Quality Assurance S3.3 Test Methods— Testing shall be in accordance with the
S3.1 Acceptance Criteria— Lot acceptance testing shall be methods specified in Table PAI and Table S2.1.
in accordance with 12.2 of this standard. S3.4 Conditioning— Test specimens shall be conditioned as
S3.2 Sample Size— The minimum number of test specimens described in Section 10.110.2.
to be tested shall conform to the requirements of the respective S3.5 Lot Certification— Lot certification shall be in accor-
test method or, if different, by agreement with the customer. dance with 12.4 of this standard.

TABLE SE Electrical Property Requirements


Property 1 2 3 4 5 6
Dielectric constant, max:A
1 kHz 4.6 6.6 8.0 7.5 4.8 4.7
1 MHz 4.3 5.9 7.3 6.6 4.6 5.1
Dissipation factor, max:A
1 kHz 0.033 0.046 0.074 0.046 0.028 0.050
1 MHz 0.039 0.053 0.079 0.089 0.064 0.055
Volume resistivity, min:B
Ω-cm 10 × 1015 5 × 1014 5 × 1014 5 × 1014 7.6 × 1015 2.5 × 1015
(Ω-in.) (4 × 1015) (2 × 1014) (2 × 1014) (2 × 1014) (3 × 1015) (1 × 1015)
Surface resistivity, min,B Ω 1 × 1016 1 × 1015 8 × 1015 2 × 1015 2 × 1015 2 × 1015
Dielectric strength, min:C
kV/mm 19.3 28.0 16.1
(V/mil) (490) (710) (410)
A
See Test Method D150.
B
See Test Method D257.
C
See Test Method D149.

APPENDIXES

(Nonmandatory Information)

X1. CROSS REFERENCE FROM MIL-P-46179A AND CLASSIFICATION SYSTEM D5204

X1.1 This classification system contains pertinent specifica- X1.3 Appropriate additional suffixes can be used as
tion items from MIL-P-46179A, for molding and extrusion required.
materials, polyamide-imide (PAI).
X1.2 The cross-reference designations are listed in Table
X1.1.

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TABLE X1.1 Cross Reference Designations for MIL-P-46179A and Revisions of Classification System D5204
MIL-P-46179A DOD D5204 – 99 D5204 – 01
D5204 Adoption Notice
Dated 27 July 1994
(Based on D5204 – 91)
Type I PAI000R03A56316E11FB41 PAI011M03 or PAI021M03 PAI000R03A56316E11FB41 or
PAI011M03 or PAI021M03
Type II Class 1 PAI000L15A32232E12FB42 PAI012L15 or PAI022L15 PAI000L15A32232E12FB42 or
PAI012L15 or PAI022L15
Type II Class 2 PAI000L23A22133E13FB42 PAI012L23 PAI000L23A22133E13FB42 or
PAI012L23
Type II Class 3 PAI000L20A11122E14FB40 PAI0121L20 PAI000L20A11122E14FB40
Type III Class 1 PAI000G30A61643E15FB46 PAI013G30 or PAI023G30 PAI000G30A61643E15FB46 or
PAI013G30 or PAI023G30
Type III Class 2 PAI000G40A61553E16FB45 Not Manufactured Not Manufactured
Type IV PAI000C30A51661FB47 PAI013C30 PAI000C30A51661FB47 or
PAI013C30
Explanation of Call-Outs for Table X1.1
An example of specifying Type III Class 1 material using property Table A in this standard and Table 3 in D4000 is as follows:
The designation PAI000G30A61643E15FB46 would indicate:
PAI000 = unspecified polyamide-imide material,
G30 = glass reinforced at 30 % nominal level,
A = Table A physical properties,
6 = tensile strength, min 172 MPa,
1 = elongation, min 4 %,
6 = flexural strength, min 290 MPa,
4 = flexural modulus, min 9660 MPa,
3 = Izod impact of 64 J/m,
E = Table SE electrical property requirements,
1 = electrical tests as specified in the footnotes of Table SE,
5 = electrical properties as given in column 5 of Table SE,
FB = Table 3 (suffix symbols and requirements) in D4000, and
46 = oxygen index, max 46 %
An example of specifying Type III Class 1 material using only Table PAI is as follows:
The designation PAI013G30 would indicate from Table PAI:
PAI = polyamide-imide as found in Terminology D1600,
01 (Group) = injection molding material,
3 (Class) = high strength PAI, and
G30 (Grade) = glass reinforced at the 30 % nominal level with the require-
ments given in Table PAI.

X2. CROSS REFERENCE DESIGNATIONS FROM THE SOCIETY OF AUTOMOTIVE ENGINEERS AMS 3670B AND CLASSI-
FICATION SYSTEM D5204

X2.1 This classification system contains pertinent specifica- X2.2 The cross reference designations are listed in Table
tion items from the SAE AMS 3670B. X2.1.

TABLE X2.1 Cross Reference Designations for SAE AMS 3670B


and Classification System D5204
AMS 3670B Designation ASTM D5204 CALL-OUT
3670/1B PAI011M03 or PAI021M03
3670/2B PAI012L23 or PAI022L23
3670/3B PAI012L15 or PAI022L15
3670/4C PAI013G30 or PAI023G30
3670/5C PAI013C30 or PAI023C30

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D5204 − 19
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5204 - 17)
that may impact the use of this standard. (August 1, 2019)

(1) The specific gravity range for 012L23 and 022L23 materi-
als in Table PAI was changed from 1.48 – 1.52 to 1.48 – 1.53,
respectively.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5205 − 16

Standard Classification System and Basis for Specification for


Polyetherimide (PEI) Materials1
This standard is issued under the fixed designation D5205; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* 2. Referenced Documents


1.1 This classification system covers unfilled, filled, and 2.1 ASTM Standards:2
reinforced polyetherimide materials suitable for injection D149 Test Method for Dielectric Breakdown Voltage and
molding and extrusion. Dielectric Strength of Solid Electrical Insulating Materials
1.2 This classification system is not intended for the selec- at Commercial Power Frequencies
tion of materials, but only as a means to call out plastic D150 Test Methods for AC Loss Characteristics and Permit-
materials to be used for the manufacture of parts. The selection tivity (Dielectric Constant) of Solid Electrical Insulation
of these materials is to be made by personnel with expertise in D257 Test Methods for DC Resistance or Conductance of
the plastics field where the environment, inherent properties of Insulating Materials
the materials, performance of the parts, part design, manufac- D618 Practice for Conditioning Plastics for Testing
turing process, and economics are considered. D638 Test Method for Tensile Properties of Plastics
D648 Test Method for Deflection Temperature of Plastics
1.3 The properties included in this classification system are Under Flexural Load in the Edgewise Position
those required to identify the compositions covered. Other D790 Test Methods for Flexural Properties of Unreinforced
requirements necessary to identify particular characteristics and Reinforced Plastics and Electrical Insulating Materi-
important to specialized applications are to be specified by als
using suffixes as given in Section 5. D792 Test Methods for Density and Specific Gravity (Rela-
1.4 Polyetherimide materials, being thermoplastic, are re- tive Density) of Plastics by Displacement
processable and recyclable. This classification system allows D883 Terminology Relating to Plastics
for the use of those polyetherimide materials, provided that all D1238 Test Method for Melt Flow Rates of Thermoplastics
specific requirements of this classification system are met. by Extrusion Plastometer
1.5 The values stated in SI units are to be regarded as D1600 Terminology for Abbreviated Terms Relating to Plas-
standard. No other units of measurement are included in this tics
standard. D2863 Test Method for Measuring the Minimum Oxygen
Concentration to Support Candle-Like Combustion of
1.6 The following precautionary caveat pertains only to the Plastics (Oxygen Index)
test methods portion, Section 12, of this classification system: D3641 Practice for Injection Molding Test Specimens of
This standard does not purport to address all of the safety Thermoplastic Molding and Extrusion Materials
concerns, if any, associated with its use. It is the responsibility D3892 Practice for Packaging/Packing of Plastics
of the user of this standard to establish appropriate safety and D4000 Classification System for Specifying Plastic Materi-
health practices and determine the applicability of regulatory als
limitations prior to use. Specific precautionary statements are D5630 Test Method for Ash Content in Plastics
given at the end of 5.4. D5740 Guide for Writing Material Standards in the Classi-
NOTE 1—There is no known ISO equivalent to this standard. fication Format
D7209 Guide for Waste Reduction, Resource Recovery, and
1
This classification system is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic
2
Materials. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2016. Published September 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1991. Last previous edition approved in 2010 as D5205 – 10. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5205-16. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D5205 − 16
Use of Recycled Polymeric Materials and Products (With- Category Material Tolerance
drawn 2015)3 (Based on the Total Mass)
C Carbon and graphite fiber- ±2 percentage points
E29 Practice for Using Significant Digits in Test Data to reinforced
Determine Conformance with Specifications G Glass-reinforced
E662 Test Method for Specific Optical Density of Smoke < 15 % glass content ±2 percentage points
> 15 % glass content ±3 percentage points
Generated by Solid Materials L Lubricants (such as PTFE, Depends upon material and
2.2 Military Standards:4 graphite, silicone, and process—to be specified
MIL-P-46184 Plastic Molding and Extrusion Materials, molybdenum disulfide)
M Mineral-reinforced ±2 percentage points
Polyetherimide (PEI). R Reinforced-combination/ ±3 percentage points based on
MIL-M-24519 Molding Plastics, Electrical, Thermoplastic mixtures of reinforcements or the total reinforcement
2.3 Underwriters Laboratories Standards:5 other fillers/reinforcements

UL 94 Tests for Flammability of Plastic Materials for Parts NOTE 3—If necessary, additional requirements are specified using
in Devices and Appliances suffixes as described in Section 5. Any special tolerances, when levels are
below 5 %, are to be specified. Ash content of filled or reinforced
3. Terminology materials are determined using Test Method D5630 where applicable.

3.1 Definitions—The terminology used in this classification 4.2.2 Specific requirements for reinforced, filled, or lubri-
system is in accordance with Terminologies D883 and D1600. cated polyetherimide materials shall be shown by a six-
character designation. The designation will consist of the letter
3.2 Abbreviation—The polyetherimide materials will be “A” or “B” and the five digits comprising the cell numbers for
designated “PEI” as specified in Terminology D1600. the property requirements in the order as they appear in Tables
4. Classification A or B.
4.2.2.1 Although the values listed are necessary to include
4.1 Unfilled polyetherimide materials are classified into the range of properties available in existing materials, this does
groups according to their composition. These groups are not imply that every possible combination of the properties
subdivided into classes and grades as shown in Table PEI. exists or can be obtained.
NOTE 2—An example of this classification system is given as follows. 4.2.3 When the grade of the basic materials is not shown, or
The designation ASTM D5205 PEI 0114 indicates the following: is not important, the use of “O”-grade classification shall be
PEI = polyetherimide as found in Terminology D1600, used for reinforced materials in this system.
01 = polyetherimide (group),
1 = general purpose (class), and NOTE 4—An example of this classification for a polyetherimide
4 = requirements given in Table PEI (grade). material is given as follows. The designation ASTM D5205
PEI0110G10A48266 would indicate the following material requirements:
4.1.1 To facilitate incorporation of future or special materi-
PEI 0110 = general-purpose polyetherimide from Table PEI,
als the “other” category (0) for group, class, and grade is shown G10 = glass reinforced at nominal 10 % level,
in Table PEI. The basic properties of these materials can be A = Table A property requirements,
obtained from Tables A or B as they apply. 4 = 110-MPa tensile strength, min,
8 = 13790-MPa flexural modulus, min,
4.2 Reinforced, pigmented, filled, and lubricated versions of 2 = 4 g/10 min; melt flow, min,
polyetherimide materials are classified in accordance with 6 = 205-MPa flexural strength, min, and
6 = 230°C deflection temperature, min.
Tables PEI and A or B. Table PEI is used to specify the
unreinforced material and Table A or B is used to specify the If no properties are specified, the designation would be
property requirements after the addition of reinforcements, ASTM D5205 PEI0110G10A00000.
pigments, fillers, or lubricants at the nominal level indicated 5. Suffixes
(see 4.2.1).
5.1 When additional requirements are needed that are not
4.2.1 A single letter shall be used to indicate the major
covered by the basic requirements or cell-table requirements,
category of the reinforcement, along with two numbers that
they shall be indicated through the use of suffixes.
indicate the percentage of additive(s) by mass, with the
tolerances as tabulated as follows: 5.2 A list of suffixes can be found in Classification System
D4000 (Table 3) and are to be used for additional requirements
3
as appropriate. Additional suffixes will be added to that
The last approved version of this historical standard is referenced on
www.astm.org.
standard as test methods and requirements are developed and
4
Available from Standardization Documents Order Desk, Bldg. 4 Section D, requested.
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
5.3 Electrical requirements are designated by a suffix which
5
Available from Underwriters Laboratories (UL), 2600 N.W. Lake Rd., Camas, uses the letter E followed by two digits. These digits refer to
WA 98607-8542, http://www.ul.com. use of Table 1.

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D5205 − 16
TABLE 1 Electrical Detail Requirements
NOTE 1—Resin samples should be dried 4 h at 160°C in an air-circulating oven before molding specimens to be used in these tests.
Property ConditionA Units A B C D E
Dielectric constant,B max 48/50 + D24 ⁄23
1 KHz, 50 % RH, 23°C ... 3.2 3.7 3.7 3.8 ...
1 MHz ... ... ... ... ... 3.5
Dissipation factor,B max 48/50 + D24 ⁄23
1 KHz, 50 % RH, 23°C ... 0.0015 0.0016 0.0017 0.0017 ...
2450 MH, 50 % RH, 23°C ... 0.003 ... ... ... ...
1 MH, 50 % RH, 23°C ... ... ... ... ... 0.007
Volume resistivity,C min 24/23/50 ohm-cm 1016 1016 1016 1016 ...
Dielectric strength,D min (1.6-mm thickness, in 48/ KV/mm 23.6 23.0 22.0 21.0 17.0
oil, S/T) 50 + 96 ⁄23 ⁄50 (V/mil)
Specific gravityE ... ... 1.27 1.34 1.42 1.51 ...
A
In accordance with Practice D618.
B
See Test Methods D150.
C
See Test Methods D257.
D
See Test Methods D149.
E
See Test Method D792 (tolerance ± 0.02).

First Digit First Digit


0 = specimen to be specified by user 0 = to be specified by user,
1 = specimens as appropriate for test methods as defined in Table 1 1 = product is tested according to UL94 at 3.05-mm minimum thickness,
Second Digit 2 = product is tested according to UL94 at 1.47-mm minimum thickness,
0 = to be specified by user 3 = product is tested according to UL94 at 0.71-mm minimum thickness,
1 = meets requirements of Table 1, Column A 4 = product is tested according to Test Method D2863,
2 = meets requirements of Table 1, Column B 5 = product is tested according to Test Method E662.
3 = meets requirements of Table 1, Column C Second Digit
4 = meets requirements of Table 1, Column D 0 = To be specified by user
5 = meets requirements of Table 1, Column E 1 = 94V-0 flammability class
2 = 94V-1 flammability class
5.4 Flammability requirements are designated by a suffix 3 = 94V-2 flammability class
that uses the letter F followed by two digits. (Warning—By 4 = 94-5V flammability class
5 = Oxygen index 44 % minimum
publication of this classification system and its use of flamma- 6 = Specific optical density, flaming mode, D4 # 2, D max # 50.
bility ratings, ASTM does not intend that their use in any way
6. General Requirements
reflects hazards presented under actual fire conditions.)
6.1 The plastic compositions shall be uniform and shall
conform to the requirements specified herein.

TABLE PEI Polyetherimide Materials Detail Requirements

NOTE 1—The values listed were developed for “natural colors.” Pigments or other additives, or both, can alter these properties.
DeflectionC FlexuralE
Flow-Rate,B Specific Temperature TensileD Strength, FlexuralE Modulus, Test
Test Method Gravity, Test (DTUL), min, Test Method Strength, Test
Group Description Class Description Grade DescriptionA Methods
D1238, Method Test Method D638, Methods D790, D790,
g/10, min D792 D648, MPa, min MPa, min MPa, min
°C, min

01 Polyetheri- 1 General- 1 <2 1.25–1.30 194 103 152 3030


Purpose
mide 2 2–8 1.25–1.30 194 103 152 3030
3 6–12 1.25–1.30 194 103 152 3030
4 10–16 1.25–1.30 194 103 152 3030
5 15–22 1.25–1.30 194 103 152 3030
6 20–30 1.25–1.30 192 90 138 2900
7 > 30 1.25–1.30 190 83 138 2900
0 Other ... ... ... ... ... ...
2 Impact- 1 <2 1.22–1.28 180 83 117 2410
Modified
2 2–8 1.22–1.28 180 83 117 2410
3 6–12 1.22–1.28 180 83 117 2410
4 10–16 1.22–1.28 180 83 117 2410
5 15–22 1.22–1.28 180 83 117 2410
6 20–30 1.22–1.28 180 69 103 2280
7 > 30 1.22–1.28 180 69 103 2280
0 Other ... ... ... ... ... ...
0 Other 0 Other ... ... ... ... ... ...

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DeflectionC FlexuralE
Flow-Rate,B Specific Temperature TensileD Strength, FlexuralE Modulus, Test
Group Description Class Description Grade DescriptionA Test Method Gravity, Test (DTUL), min, Test Method Strength, Test Methods
D1238, Method Test Method D638, Methods D790, D790,
g/10, min D792 D648, MPa, min MPa, min MPa, min
°C, min

02 PEI Chemical 1 General- 1 <2 1.25–1.30 198 93 128 2760


Purpose
Resistant 2 2–8 1.25–1.30 198 93 128 2760
3 6–12 1.25–1.30 198 93 128 2760
4 10–16 1.25–1.30 198 93 128 2760
5 15–22 1.25–1.30 198 93 128 2760
6 20–30 1.25–1.30 196 90 124 2760
7 > 30 1.25–1.30 196 90 124 2760
0 Other ... ... ... ... ... ...
2 Impact- 1 <2 1.22–1.28 184 69 90 2070
Modified
2 2–8 1.22–1.28 184 69 90 2070
3 6–12 1.22–1.28 184 69 90 2070
4 10–16 1.22–1.28 184 69 90 2070
5 15–22 1.22–1.28 184 69 90 2070
6 20–30 1.22–1.28 184 69 90 2070
7 > 30 1.22–1.28 184 69 90 2070
0 Other ... ... ... ... ... ...
3 High-Heat 1 <2 1.27–1.32 215 97 145 2760
Resistant 2 2–8 1.27–1.32 215 97 145 2760
3 6–12 1.27–1.32 215 97 145 2760
4 10–16 1.27–1.32 215 97 145 2760
5 15–22 1.27–1.32 215 97 145 2760
6 20–30 1.27–1.32 215 97 145 2760
7 > 30 1.27–1.32 215 97 145 2760
0 Other ... ... ... ... ... ...
4 High-Heat 1 <2 1.23–1.30 200 69 103 2070
Impact- 2 2–8 1.23–1.30 200 69 103 2070
Modified
3 6–12 1.23–1.30 200 69 103 2070
4 10–16 1.23–1.30 200 69 103 2070
5 15–22 1.23–1.30 200 69 103 2070
6 20–30 1.23–1.30 200 69 103 2070
7 > 30 1.23–1.30 200 69 103 2070
0 Other 0 Other ... ... ... ... ... ...
03 PEI Heat- 1 General- 1 <2 1.27–1.31 210 103 145 2760
Purpose
Resistant 2 2–8 1.27–1.31 210 103 145 2760
3 6–12 1.27–1.31 210 103 145 2760
4 10–16 1.27–1.31 210 103 145 2760
5 15–22 1.27–1.31 210 103 145 2760
6 20–30 1.27–1.31 210 90 131 2760
7 > 30 1.27–1.31 210 90 131 2760
0 Other ... ... ... ... ... ...
2 Impact- 1 <2 1.22–1.28 196 69 110 2070
Modified
2 2–8 1.22–1.28 196 69 110 2070
3 6–12 1.22–1.28 196 69 110 2070
4 10–16 1.22–1.28 196 69 110 2070
5 15–22 1.22–1.28 196 69 110 2070
6 20–30 1.22–1.28 196 69 110 2070
7 > 30 1.22–1.28 196 69 110 2070
0 Other ... ... ... ... ... ...
3 High-Heat 1 <2 1.28–1.32 225 103 138 2760
2 2–8 1.28–1.32 225 103 138 2760
3 6–12 1.28–1.32 225 103 138 2760
4 10–16 1.28–1.32 225 103 138 2760
5 15–22 1.28–1.32 225 103 138 2760
6 20–30 1.28–1.32 225 103 138 2760
7 > 30 1.28–1.32 225 103 138 2760
0 Other ... ... ... ... ... ...
4 High-Heat 1 <2 1.24–1.28 210 69 97 2070
Impact- 2 2–8 1.24–1.28 210 69 97 2070
Modified
3 6–12 1.24–1.28 210 69 97 2070
4 10–16 1.24–1.28 210 69 97 2070
5 15–22 1.24–1.28 210 69 97 2070
6 20–30 1.24–1.28 210 69 97 2070
7 > 30 1.24–1.28 210 69 97 2070
0 Other ... ... ... ... ... ...
0 Other 0 Other ... ... ... ... ... ...

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DeflectionC FlexuralE
Flow-Rate,B Specific Temperature TensileD Strength, FlexuralE Modulus, Test
Group Description Class Description Grade DescriptionA Test Method Gravity, Test (DTUL), min, Test Method Strength, Test Methods
D1238, Method Test Method D638, Methods D790, D790,
g/10, min D792 D648, MPa, min MPa, min MPa, min
°C, min

04 PEI—Flexible 1 General- 1 <2 1.16–1.20 N/AF 34 52 690


Purpose
Resistant 2 2–8 1.16–1.20 N/AF 34 52 690
3 6–12 1.16–1.20 N/AF 34 52 690
4 10–16 1.16–1.20 N/AF 34 52 690
5 15–22 1.16–1.20 N/AF 34 52 690
6 20–30 1.16–1.20 N/AF 34 52 690
7 > 30 1.16–1.20 N/AF 34 52 690
0 Other ... ... ... ... ... ...
2 Semirigid 1 <2 1.16–1.20 N/AF 21 14 69
2 2–8 1.16–1.20 N/AF 21 14 69
3 6–12 1.16–1.20 N/AF 21 14 69
4 10–16 1.16–1.20 N/AF 21 14 69
5 15–22 1.16–1.20 N/AF 21 14 69
6 20–30 1.16–1.20 N/AF 21 14 69
7 > 30 1.16–1.20 N/AF 21 14 69
0 Other ... ... ... ... ... ...
3 Nonrigid 1 <2 1.10–1.20 N/AF 7 7 <69
2 2–8 1.10–1.20 N/AF 7 7 <69
3 6–12 1.10–1.20 N/AF 7 7 <69
4 10–16 1.10–1.20 N/AF 7 7 <69
5 15–22 1.10–1.20 N/AF 7 7 <69
6 20–30 1.10–1.20 N/AF 7 7 <69
7 > 30 1.10–1.20 N/AF 7 7 <69
0 Other ... ... ... ... ... ...
0 Other 0 Other ... ... ... ... ... ...
A
No descriptions are listed unless needed to describe a special grade under the class. All other grades are listed by requirements.
B
Conditions—Method A, 6.7 kg, 2.0955-mm inside diameter orifice:
Group-Class Test Temperatures, °C
011, 012, 021, 022 337
023, 024, 031, 032, 033, 034 367
041, 042, 043 295
C
Specimens 6.4 mm tested at 1.82 MPa.
D
Type 1 bar, speed 5.1 mm/min.
E
Method I, Procedure A, speed = 2.5 mm ⁄min, span-to-depth ratio 16/1 (tangent modulus).
F
“N/A” indicates the particular data so designated is considered “Not Applicable” to the product being considered.

TABLE A Detail Requirements Filled or Reinforced PEI, or Both


NOTE 1—Resin samples should be dried 4 h at 160°C in an air-circulating oven before molding specimens to be used in these tests and before
determining melt-flow rate.
Designa-
Property/ASTM Test
tion Units 0 1 2 3 4 5 6 7 8 9
Method
Order
1 Tensile strength, min, D638,A Type I MPa B
25 55 80 110 135 165 190 220 C

bar, 0.2 in./min


2 Flexural modulus, min, D790D MPa B
690 1720 3450 5170 6900 8620 10340 13790 C

3 Flow Rate, min, D1238E g/10 min B


1 4 7 10 13 16 20 24 C

4 Flexural strength, min, D790D MPa B


30 65 100 135 170 205 240 275 C

5 Deflection Temperature, min, D648F °C B


180 190 200 210 220 230 240 250 C

A
Type I bar, speed = 5.1 mm/min.
B
Unspecified.
C
Specify value. If a specific value is required, it must appear on the drawing or contract, or both.
D
Method 1, Procedure A; speed = 2.55 mm ⁄min.
E
Conditions—Method A, 6.7 kg, 2.0955-mm inside diameter orifice:
Group-Class Test Temperatures, °C
011, 012, 021, 022 337
023, 024, 031, 032, 033, 034 367
041, 042, 043 295
F
6.4-mm thick specimen tested at 1.82 MPa.

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D5205 − 16
TABLE B Detail Requirements Unreinforced/Unfilled PEI
NOTE 1—Resin samples should be dried 4 h at 160°C in an air-circulating oven before molding specimens to be used in these tests and before
determining melt-flow rate.
Designa-
Property/ASTM Test
tion Units 0 1 2 3 4 5 6 7 8 9
Method
Order
1 Tensile strength, min, D638A MPa B
14 25 40 55 65 80 95 110 C

2 Flexural modulus, min, D790D MPa B


7 30 65 340 690 1380 2070 2760 C

3 Flow Rate, min, D1238E g/10 min B


2 6 10 14 18 22 26 30 C

4 Flexural strength, min, D790D MPa B


7 30 65 90 110 130 150 170 C

5 Deflecting Temperature, min, D648FG °C B


170 180 190 200 210 220 230 240 C

A
Type I bar, speed = 5.1 mm ⁄min.
B
Unspecified.
C
Specify value. If a specific value is required, it must appear on the drawing or contract, or both.
D
Method 1, Procedure A; speed = 2.55 mm ⁄min.
E
Conditions—Method A, 6.7 kg, 2.0955-mm inside diameter orifice:
Group-Class Test Temperatures, °C
011, 012, 021, 022 337
023, 024, 031, 032, 033, 034 367
041, 042, 043 295
F
6.4-mm thick specimen tested at 1.82 MPa.

7. Detail Requirements 13. Inspection and Certification


7.1 The various materials shall conform to the requirements 13.1 Inspection and certification of the material supplied
prescribed in the tables and suffix requirements as they apply. with reference to a specification based on this classification
7.2 For the purpose of determining conformance, all speci- system shall be for conformance to the requirements specified
fied limits for a specification (line callout) based on this herein.
classification system are absolute limits, as defined in Practice 13.2 Lot-acceptance inspection shall be the basis on which
E29. acceptance or rejection of the lot is made. The lot-acceptance
7.2.1 With the absolute method, an observed value or a shall consist of: flow rate.
calculated value is not rounded, but is to be compared directly
with the specified limiting value. Conformance or nonconfor- 13.3 Periodic check inspection shall consist of the tests
mance is based on this comparison. specified for all requirements of the material under this
classification system. Inspection frequency shall be adequate to
8. Sampling ensure the material is certifiable in accordance with 13.4.
8.1 Sampling shall be statistically adequate to satisfy re- 13.4 Certification shall be that the material was manufac-
quirements of 13.4. A batch or lot is contrued as a unit of tured by a process in statistical control, sampled, tested, and
manufacture as prepared for shipment and can consist of a inspected in accordance with this classification system, and
blend of two or more “production runs.” that the average values meet the requirements of the specifi-
9. Number of Tests cation (line callout).
9.1 The number of tests shall be consistent with the require- NOTE 5—The ASTM publication Manual on Presentation of Data and
ments of 13.4. Control Chart Analysis, 8th Edition,6, provides detailed information about
statistical process control.
10. Specimen Preparation
13.5 A report of the test results shall be furnished when
10.1 Unless otherwise specified, test specimens shall be requested. The report shall consist of results of the lot
prepared by injection molding in accordance with Practice acceptance inspection for the shipment and the results of the
D3641 employing the following conditions: most recent periodic check inspection.
Minimum Minimum
Mold Stock
Temperature, Temperature,
14. Packing, Packaging, and Package Marking
°C °C
Unfilled and unreinforced 120 360
14.1 Provisions of Practice D3892 apply for packing,
Filled or reinforced, or both 150 390 packaging, and marking of containers for plastic materials.
11. Conditioning
15. Keywords
11.1 Condition test specimens at least 40 h at 23°C and
50 % relative humidity as defined in 3.1.2 of Practice D618. 15.1 classification; line-call-out; polyetherimide resins

12. Test Methods


12.1 Determine the properties enumerated in this classifica- 6
Available from ASTM International Headquarters. Order Catalog Number:
tion system using the referenced test methods. MNL-8TH-EB.

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D5205 − 16

APPENDIX

(Nonmandatory Information)

X1. CROSS REFERENCES

X1.1 The following cross references between government


specifications and Classification System D5205 are provided
for information purposes only.
TABLE X1.1 Cross References Designations for Classification System D5205 and Government Specifications
Government Specification Classification System D5205
MIL-P-46184
Type I (unfilled) PEI0113 E01 F05 F06
Type II Class 1 (glass reinforced) PEI0110 G10 A49203 E02 ZU 434OMPa
Class 2 (glass reinforced) PEI0110 G20 A99103 E03 ZU 5800MPa
Class 3 (glass reinforced) PEI0110 G30 A99103 E04 ZK 159MPa ZU 7600MPa
MIL-M-24519B
Type: GLT-10F (glass reinforced) PEI0110 G10 A00290 E05 EF085 ZN180
GLT-20F (glass reinforced) PEI0110 G20 A00190 E05 EF085 ZN195
GLT-30F (glass reinforced) PEI0110 G30 A00190 E05 EF085 ZN215

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D5205 – 10) that may impact the use of this standard. (September 1, 2016)

(1) Added statement allowing recycled material to Scope. (6) Corrected placement of footnote A in Table PEI and applied
(2) In 2.1, added reference to D5740, Standard Guide for footnote F to all appropriate cells.
Writing Material Standards in the Classification D4000 For- (7) Eliminated footnote B as unnecessary on all tables.
mat. (8) Rewrote footnote D on Tables A and B.
(3) In 2.1, added reference to D7209, Guide for Waste (9) Rewrote 8.1 and 8.2 to correct reference and to use wording
Reduction, Resource Recovery, and Use of Recycled Poly- of D5740 in 8.1.
meric Materials and Products. (10) In 11.1, eliminated tolerances in order to avoid possible
(4) Revised Note 3 for clarity of intent. misinterpretation of the requirements.
(5) Rewrote Section 5 to improve consistency with wording of (11) Revised 13.2 to use wording of D5740.
D5740, Standard Guide for Writing Material Standards in the (12) Revised 13.4 to reflect current practice and added Note 8.
Classification D4000 Format. (13) Revised 13.5 to accommodate use of recycled material.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5206 − 19 An American National Standard

Standard Test Method for


Windload Resistance of Rigid Plastic Siding1
This standard is issued under the fixed designation D5206; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope D1600 Terminology for Abbreviated Terms Relating to Plas-


1.1 This test method describes methods for testing and tics
evaluating windload resistance of rigid plastic siding when D4756 Practice for Installation of Rigid Poly(Vinyl Chlo-
fastened in accordance with Practice D4756, specific product ride) (PVC) Siding and Soffit
standard specifications, or in accordance with manufacturer’s E631 Terminology of Building Constructions
installation instructions. 2.2 ASCE Standard:3
ASCE 7-10 Minimum Design Loads for Buildings and Other
1.2 The proper use of this test method requires a knowledge Structures
of the principles of pressure measurement. 2.3 International Code Council:4
1.3 This test method describes the apparatus and the proce- International Building Code
dures to be used to determine an average maximum sustained International Residential Code
static test pressure, or ultimate test pressure values, or both,
with static pressure applied uniformly to a specimen. 3. Terminology
NOTE 1—There is no known ISO equivalent to this test method. 3.1 General—Definitions are in accordance with Terminolo-
gies D883 and E631 and abbreviations are in accordance with
1.4 The values expressed in inch-pound units are to be Terminology D1600 unless otherwise indicated.
regarded as the standard. The SI equivalents in parentheses are
for information only. 3.2 Definitions of Terms Specific to This Standard:
3.2.1 maximum sustained static test pressure—the greatest
1.5 This standard does not purport to address all of the
difference in static air pressure (negative or positive) that a test
safety concerns, if any, associated with its use. It is the
specimen withstands without failure, expressed as force per
responsibility of the user of this standard to establish appro-
square foot (or pascals).
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3.2.2 nail hem thickness—the average thickness of the nail
For specific precautionary statements, see Section 7. hem as measured between the nail slots.
1.6 This international standard was developed in accor- 3.2.3 specimen—the entire assembled siding panel as de-
dance with internationally recognized principles on standard- scribed in Section 8.
ization established in the Decision on Principles for the 3.2.4 static test pressure—the specific difference in static air
Development of International Standards, Guides and Recom- pressure (positive or negative) for which the specimen is to be
mendations issued by the World Trade Organization Technical tested expressed as force per square foot (or pascals).
Barriers to Trade (TBT) Committee.
3.2.5 ultimate test pressure—the difference in static air
2. Referenced Documents pressure (positive or negative) at which failure occurs ex-
pressed as force per square foot (or pascals).
2.1 ASTM Standards:2
D883 Terminology Relating to Plastics 4. Summary of Test Method
4.1 This method can be used to determine either the
maximum sustained static test pressure or the ultimate
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics pressure, or both, for the siding specimen. The procedure
and is the direct responsibility of Subcommittee D20.24 on Plastic Building
Products.
consists of sealing the test specimen with or against one face of
Current edition approved Nov. 15, 2019. Published January 2020. Originally a test chamber, supplying air to or exhausting air from the
approved in 1991. Last previous edition approved in 2013 as D5602 – 13. DOI:
10.1520/D5206-19.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from American Society of Civil Engineers (ASCE), 1801 Alexander
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Bell Dr., Reston, VA 20191, http://www.asce.org.
4
Standards volume information, refer to the standard’s Document Summary page on Available from International Code Council (ICC), 500 New Jersey Ave., NW,
the ASTM website. 6th Floor, Washington, DC 20001, http://www.iccsafe.org.

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D5206 − 19
chamber at a rate required to maintain a specific static air 6. Apparatus
pressure across the specimen for a specific time period. 6.1 The description of theapparatus is general in nature; any
Pressure is applied in increments and the sample observed for equipment capable of performing the test procedure within the
failure at each stage, to determine the maximum sustained allowable tolerances is permitted.
static test pressure, the ultimate test pressure, or both.
6.2 Major Components (See Fig. 1):
5. Significance and Use 6.2.1 Test Chamber—A test chamber or box with an
5.1 This test method is a standard procedure for determining opening, a removable mounting panel, or one open side in
windload resistance of rigid plastic siding under specified which or against which the specimen is installed. Either the
uniform static pressure difference. This typically is intended to positive test chamber configuration or the negative test cham-
represent the effects of wind loads on exterior building sur- ber configuration shall be used to perform this test. (See Fig.
faces. The actual loading on building surfaces is quite complex, 1.) At least one static pressure tap shall be provided to measure
varying with wind direction, time, height above ground, the chamber pressure and shall be so located that the reading is
building shape, terrain, surrounding structures, and other fac- unaffected by the velocity of the air supply to or from the
tors. chamber or any other air movement. The air supply opening
into the chamber shall be arranged so that the air does not
5.2 Design wind pressure is derived for specific geographi- impinge directly on the test specimen with any significant
cal locations from wind velocity maps prepared by various velocity. A means of access into the chamber to facilitate
agencies and found in references such as ASCE 7, the adjustments, observations, and measurements after the speci-
International Residential Code, International Building Code or men has been installed is permitted.
other sources. For additional detailed information relating to
the use of this test method for evaluation of wind load NOTE 3—The test chamber or the specimen mounting frame, or both,
must not deflect under the test load in such a manner that the performance
resistance, refer to Annex A1 of the standard specification of the specimen will be affected.
appropriate for the type of polymeric siding.
6.2.2 Air System—A controllable blower, a compressed air
NOTE 2—In applying the results of this test method, note that the supply, an exhaust system, or reversible controllable blower
performance of rigid PVC siding is a function of installation, and the designed to provide the required maximum air pressure differ-
specimen may or may not truly represent the actual application. In service,
performance will also depend on the rigidity of supporting construction, ence across the specimen. The system shall provide an essen-
and on the resistance of other components to deterioration by various tially constant air pressure difference for the required test
causes, to thermal expansion and contraction, etc. period.

FIG. 1 Test Chamber

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D5206 − 19
6.2.3 Pressure Measuring Apparatus—A device to measure siding face will depend upon whether a positive or negative
the test pressure difference within a tolerance of 62 %. chamber configuration is used. The test configuration shall
create a load on the siding in the direction that would tend to
7. Safety Precautions pull the siding off the wall.
7.1 Take proper precautions to protect the observers in the 9.2 Install a filler panel in the test chamber of box opening
event of any failure. At the pressures used in this test method, not covered by the specimen frame.
considerable energy and hazard are involved. In cases of
failure, the hazard to personnel is less with a negative pressure 9.3 Seal all seams in the equipment and test chamber which
configuration, as the specimen will tend to blow into the test could permit pressure leakage during the test.
chamber rather than out. Do not permit personnel in such 9.4 Failure of siding specimen has occurred when any of the
chambers during tests and lock out chambers during tests. following criteria are present:
8. Test Specimens 9.4.1 Siding nail tab is torn or disengaged from fastener.
9.4.2 Permanent buckling of siding.
8.1 Sampling—Siding samples for test specimens shall be
selected at random from production stock. 9.4.3 Fastener withdrawal from frame.
9.4.4 Permanent disengagement of locks.
8.2 Prepare a test specimen frame to simulate construction
methods that will be expected in the field. The frame shall be 9.5 Procedure—This procedure determines the maximum
sized to accommodate a minimum of three stud spaces wide sustained static test pressure, the ultimate test pressure for
and a minimum of four siding panels high. Measure the nail failure, or both, for the siding.
hem thickness at a minimum of 5 locations along the nail hem 9.5.1 Check the specimen for proper adjustment and lock
prior to mounting the panel. out the chamber if human entry is possible.
8.2.1 Stud spacing shall have either 16 or 24-in. (406 or 609 9.5.2 Apply a preload of 5 lbf/ft2 (239.4 Pa) to the test
mm) centers in accordance with the manufacturer’s fastening specimen and hold for 30 s. Release pressure difference across
instructions. the specimen, and allow a 1-min recovery period.
8.2.2 The overall height of the test specimen frame shall be
9.5.3 Apply a pressure difference across the specimen in
adjusted for siding panels of varying height to keep the
increments of 5 lbf/ft2 (239.4 Pa), holding for 30 s before
distance between the frame and the siding at the top and bottom
increasing the next 5 lbf/ft2 (239.4 Pa). Continue test until
to a minimum and yet provide clearance between siding and
failure occurs. Record the pressure at failure, which is the
frame. (See Fig. 1.)
ultimate pressure, as well as the mode of failure. Record the
8.3 Apply 2-mil (0.0508 mm) maximum thickness plastic highest pressure that was sustained for 30 s without failure,
film between the siding and the studs or sheathing and seal it which is the maximum sustained static test pressure.
to the perimeter of the test frame. If sheathing is applied to the 9.5.4 Test two additional specimens for failure pressure
exterior of the studs, 2-in. (50.8 mm) minimum diameter holes difference as detailed in 9.5.1 to 9.5.3. For each sample, record
centered horizontally and vertically between studs shall be cut the pressure at failure, which is the ultimate test pressure, and
through the sheathing to allow pressure application to the the failure mode. Record the highest pressure that was sus-
plastic film. tained for 30 s without failure, which is the maximum
8.3.1 Film application must permit full pressure load trans- sustained static test pressure.
fer to the siding test specimen and must not prevent movement
9.5.5 Average the pressure at failure for each of the three
or failure of the specimen. Apply film loosely with extra folds
specimens and report this value as the average ultimate test
of material at each corner and at all offsets and recesses. When
pressure of the siding product. Average the highest pressure
load is applied, there shall be no fillet caused by tightness of
that was sustained for 30 s without failure for each of the three
the plastic film.
specimens and report this value as the average maximum
8.4 Apply a starter strip and at least four siding panels to the sustained static test pressure.
test specimen frame as specified in the section on application of 9.5.6 For the test results to be considered valid, the ultimate
horizontal siding in Practice D4756 (9.1), the standard speci- test pressure and the maximum sustained static test pressure for
fication appropriate for the type of siding, or manufacturer’s each of the three specimens must fall within the following
installation instructions. required range:
8.5 In cases where siding is not designed or configured for (1) For average test pressure less than 33.33 lbf/ft2, the
use as horizontal panels, the test structure shall be modified to result for each of the three specimens is not greater than 5 psf
provide a test exposure similar to that described in the above above or below the average of the three specimens.
sections, with the siding installed in accordance with the (2) For average test pressure greater than or equal to 33.33
manufacturer’s instructions. lbf/ft2 (1596 Pa), the result for each of the three specimens is
not greater than 15 percent above or below the average of the
9. Procedure three pressures.
9.1 Position a test specimen frame vertically or horizontally 9.5.6.1 If the result for any of the three specimens falls
over the opening in the test chamber (box) so as to subject the outside the required range, a test with a fourth specimen is to
entire test specimen to the pressure load. The orientation of the be conducted. The average of all four tests is reported.

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D5206 − 19
10. Report 10.1.8 As appropriate, the ultimate test pressure, the aver-
10.1 Report the following information: age maximum sustained static test pressure, or both.
10.1.1 Date of the test and the report. 10.1.9 A statement that the tests were conducted in accor-
10.1.2 Identification of the siding (manufacturer, trademark, dance with this test method, or a full description of any
or code, lot number, source of supply, dimensions, model type, deviations from this test method.
material) and other related information. 10.1.10 Author of the report.
10.1.3 Specific details of test parameters including siding 10.1.11 Testing agency which conducted the tests and re-
nominal and measured thickness, siding style, fasteners used, quester of tests, including addresses.
number of siding spans used, stud spacing, nail slot edge 10.1.12 Ambient conditions including temperature, before
distance, average nail hem thickness, type and thickness of and during tests.
sheathing material, and other pertinent information. If a double 10.1.13 Signatures of persons responsible for supervision of
nail hem is used, the thickness of both nail hem walls shall be the tests and a list of official observers.
reported. Any deviation from the test procedure in Sections 8 10.1.14 Append to the report any data not required herein,
and 9 shall be reported. but useful to a better understanding of the test results,
10.1.4 Detailed drawings of the test specimen, showing conclusions, or recommendations.
dimensioned section profiles and any other pertinent details. 11. Precision and Bias
Any deviation from the drawings or any modifications made to
the specimen to obtain the reported values shall be noted on the 11.1 Precision—Due to the subjective nature of the tests
drawing and in the report. (pass/fail mode), the many variable styles of siding under test,
10.1.5 Any deviation from the manufacturer’s installation the variable installation practice depending on the manufactur-
instructions or any modifications made to the test specimen to er’s instructions, the variable sheathing or stud backing to
obtain the reported values shall be noted on the installation which the siding is installed, and the variable modes of failure,
instructions and the test report. the precision of this test method has not been measured.
10.1.6 A record of visual observations made during the 11.2 Bias—It is not possible to measure bias in this test
application of pressure and during the examination for failure method since there is no reference value.
criteria.
10.1.7 A tabulation of test pressure difference applied to 12. Keywords
each specimen, specimen orientation, duration of pressure 12.1 PVC siding; plastic siding; siding failure modes; test
application, and failure mode for each test performed. methods; windload resistance

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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Downloaded/printed by
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5207 − 14

Standard Practice for


Confirmation of 20–mm (50–W) and 125–mm (500–W) Test
Flames for Small-Scale Burning Tests on Plastic Materials1
This standard is issued under the fixed designation D5207; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D5025 Specification for Laboratory Burner Used for Small-


1.1 This practice covers the confirmation of test flames for Scale Burning Tests on Plastic Materials
small-scale burning tests on plastic materials using the labora- E176 Terminology of Fire Standards
tory burner described in Specification D5025. Back pressures E220 Test Method for Calibration of Thermocouples By
and flow rates for methane, propane, and butane supply gases Comparison Techniques
are given for specific test flames. This practice describes a E230 Specification and Temperature-Electromotive Force
procedure to confirm the heat evolution of the test flame. (EMF) Tables for Standardized Thermocouples
E608 Specification for Mineral-Insulated, Metal-Sheathed
1.2 The values stated in SI units are to be regarded as the Base Metal Thermocouples
standard. 2.2 IEC Standards:3
1.3 This standard is used to measure and describe the IEC/TS 60695-11-3 Ed. 1: Fire Hazard Testing-Part 11: Test
response of materials, products, or assemblies to heat and Flames-Section 3: 500 W Flames: Apparatus and Confir-
flame under controlled conditions, but does not by itself mational Test Methods
incorporate all factors required for fire hazard or fire risk IEC/TS 60695-11-4 Ed. 2: Fire Hazard Testing-Part 11: Test
assessment of the materials, products, or assemblies under Flames-Section 4: 50 W Flame: Apparatus and Confirma-
actual fire conditions. tional Test Methods
NOTE 1—There is no similar ISO standard. This practice is equivalent
in technical content to, but not fully corresponding in presentation with,
3. Terminology
the confirmatory procedures of IEC/TS 60695-11-3, Method A and IEC/ 3.1 Definitions of Terms:
TS 60695-11-4, Method A. 3.1.1 For definitions of terms related to plastics used in this
1.4 Fire testing is inherently hazardous. Adequate safe- test method, refer to Terminology D883. For definitions of
guards for personnel and property shall be employed in terms related to fire used in this test method, refer to Termi-
conducting these tests. nology E176.
1.5 This standard does not purport to address all of the
4. Summary of Practice
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4.1 A test flame of specified height and color is obtained
priate safety and health practices and determine the applica- with gas supplied at a suggested back pressure and flow rate. A
bility of regulatory limitations prior to use. thermal sensor is then positioned over the flame, and the time
for the temperature of the sensor to increase from 100 to 700°C
2. Referenced Documents is determined. The time is used to confirm the heat-evolution
2.1 ASTM Standards:2 profile of the test flame.
D883 Terminology Relating to Plastics 5. Significance and Use
D3195 Practice for Rotameter Calibration
5.1 The flame height and color (indicative of air-to-gas
ratio) for a test flame have traditionally been specified in the
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and individual test method. The energy content of the flame has
is the direct responsibility of Subcommittee D20.30 on Thermal Properties. also been addressed by reference to a specific supply gas. It has
Current edition approved May 1, 2014. Published May 2014. Originally been determined that the supply-gas back pressure and flow
approved in 1991. Last previous edition approved in 2009 as D5207 – 09. DOI:
10.1520/D5207-14. rate can be varied without affecting the height and color of the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.

*A Summary of Changes section appears at the end of this standard


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D5207 − 14
flame. However, the energy content of the flame is affected. the 20-mm (50–W) flame, and a 10.0 6 0.05-g slug is used for
This practice provides the back pressure and flow rate of the the 125-mm (500–W) flame. A Type K thermocouple with a
supply gas for a 20-mm (50–W) and a 125-mm (500–W) test 0.5-mm diameter stainless steel sheath constructed in accor-
flame, and a procedure for confirming the heat-evolution dance with Specification E608 shall be peened into the top of
profile of the test flame. the slug.
5.2 Information is provided for test flames using methane, 6.6 Temperature Indicator—A potentiometer or temperature
propane, or butane. Using this information, these supply gases indicator for Type K thermocouples capable of reading to
can be used interchangeably with a standardized burner to 800°C. Calibrate the combination thermal sensor and tempera-
produce essentially the same test flame. ture indicator in accordance with the general procedures
outlined in Method E220. The initial calibration tolerance is
6. Apparatus defined in Tables E230.
6.1 Test Chamber, enclosure or laboratory hood, free of 6.7 Ring Stand, with a clamp or equivalent device, adjust-
induced or forced draft, having an internal volume of at least able for positioning of the thermal sensor.
0.5 m3 for the 20–mm (50–W) flame or 0.75 m3 for the
125–mm (500–W) flame. 6.8 Timer, stop watch or other suitable timing device
capable of timing to the nearest 0.1 s.
6.2 Laboratory Burner, constructed in accordance with
Specification D5025. 6.9 Gas Supply—A supply of methane, propane, or butane,
with suitable regulator and meter for uniform gas flow.
6.3 Manometer/Pressure Gauge, capable of measuring to
800 mm of water, with increments of 5 mm. 6.9.1 Methane, Technical grade, 98 % minimum purity,
having a heating value of 37 6 1 MJ ⁄m3 at 25°C. Natural gas
6.4 Flow Meter—A rotameter calibrated in accordance with with a certified heating value of 37 6 1 MJ/m3 will likely
Practice D3195, with correlation curves appropriate for the gas, provide similar results.
or a mass flow meter with at least 2 % accuracy. 6.9.2 Propane, Technical grade, 98 % minimum purity,
6.5 Thermal Sensor (Copper Slug and Thermocouple)—A having a heating value of 94 6 2 MJ ⁄m3 at 25°C.
slug constructed of high conductivity (electrolytic) copper with 6.9.3 Butane, CP grade, 99 % minimum purity, having a
dimensions as shown in Fig. 1. A 1.76 6 0.01-g slug is used for heating value of 120 6 3 MJ/m3 at 25°C.

FIG. 1 Copper Slug for Thermal Sensor

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7. Confirmation Procedure
7.1 Locate the burner in a draft-free enclosure or hood.
Connect the burner to the gas supply, in line with a control
valve, flowmeter and manometer. See Fig. 2.
7.2 Connect the leads of the Type K thermocouple to the
temperature indicator. Clamp the thermocouple sheath above
the burner, along its central axis, so that the copper slug is
suspended 75 mm minimum from the clamp. See Fig. 3.
7.2.1 20-mm (50–W) Test Flame—Position the slug 10 6 1
mm from the top of the burner.
7.2.2 125-mm (500–W) Test Flame—Position the slug
55 6 1 mm from the top of the burner.
7.3 Move the burner away from the copper slug to ensure no
influence of the flame on the slug during the preliminary
adjustment of the test flame.
7.4 If the copper slug has not been used before, conduct a
preliminary run to condition the surface of the slug. Discard
this first result. The slug shall not be polished or cleaned for
subsequent use. The presence or absence of an oxide coating
affects the thermal response of the slug to the flame. It is
recommended that laboratories maintain a standard reference
slug and a working slug to compare their thermal response
working and verify that the oxide coating is not affecting the
working slug’s thermal response.
7.5 Start with the needle valve on the burner completely
open, and the air-inlet openings closed or reduced to the
smallest setting. Set the gas-flow rate and back pressure for the FIG. 3 Confirmatory Test Arrangement
type of flame and gas supply. Ignite the flame.
7.5.1 20-mm (50–W) Test Flame—Set the gas flow rate as TABLE 1 20-mm (50–W) Test Flame
shown in Table 1. Adjust the needle valve so that the back
Gas Type Methane
pressure is also as shown in Table 1. Adjust the barrel air
Flow rate mL/min 105 ± 5
supply so that a blue flame with no inner cone and an overall Back pressure mm water <10
height of 20 6 1 mm is produced, when viewed in subdued
light.
TABLE 2 125-mm (500–W) Test Flame
NOTE 2—If alternate fuel gases such as propane or butane are used,
ensure that a stable flame is obtained and the heat-evolution profile Gas Type Methane Propane Butane
complies with 7.10.1. It is possible the yellow tip will not disappear when Flow rate mL/min 965 ± 30 380 ± 15 300 ± 10
using propane or butane. Back mm water 125 ± 25 550 ± 100 600 ± 125
pressure
7.5.2 125-mm (500–W) Test Flame—Set the gas flow rate as
shown in Table 2. Adjust the needle valve so that the back
pressure is also as shown in Table 2. Adjust the barrel air
supply so that a flame having an inner blue cone of 40 6 2 mm 7.6 Extinguish the flame and reposition the copper slug, if
and an overall height of 125 6 10 mm is produced, when necessary.
viewed in subdued light. 7.7 Reignite the flame and allow the burner to operate for 5
min to stabilize the working temperature.
7.8 The initial temperature of the slug shall be less than
50°C.
7.9 Reposition the burner under the slug. Start the timer
when the temperature of the slug reaches 100 6 2°C. Stop the
timer when the temperature of the slug reaches 700 6 3°C.
Record this time. Remove the burner and allow the slug to cool
in air to less than 50°C between determinations.
NOTE 3—It is optional to use a small fan to reduce the time to cool the
slug.
NOTE 4—To avoid damage to the thermocouple, immediately remove or
FIG. 2 Burner Supply Arrangement extinguish the flame once the slug has reached 700°C.

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D5207 − 14
7.10 Report the individual determinations.
7.10.1 20-mm (50–W) Test Flame—The time for the tem-
perature to rise from 100 6 2 to 700 6 3°C shall be 44 6 2 s.
7.10.2 125-mm (500–W) Test Flame—The time for the
temperature to rise from 100 6 2 to 700 6 3°C shall be 54 6 2
s.
7.11 If the temperature-rise time falls outside the specified
range, adjust the gas-flow rate and repeat the calibration
procedure from 7.5. If the temperature-rise time is within the
specified range, repeat the heating procedure (see 7.7) two
additional times to confirm the heat-evolution profile of the test
flame.
7.12 An example of a typical temperature response is shown
in Fig. 4.

8. Keywords
8.1 confirmation; flammability; laboratory burner; small-
FIG. 4 Typical Temperature Response
scale burning tests; test flames

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5207 - 09)
that may impact the use of this standard. (May 1, 2014)

(1) Added standard edition number to IEC/TS60695-11-3 (4) Added the replacement criteria for copper slug to minimize
(2.2). variation in results (7.4).
(2) Revised 3.1.
(3) Revised the term “heat flux” to “heat evolution” (5.1) to
align with 1.1, 4.1, and 7.11.

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of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
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Designation: D5208 − 14

Standard Practice for


Fluorescent Ultraviolet (UV) Exposure of Photodegradable
Plastics1
This standard is issued under the fixed designation D5208; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* G141 Guide for Addressing Variability in Exposure Testing


1.1 This practice covers the specific procedures applicable of Nonmetallic Materials
for fluorescent Ultraviolet (UV) exposure of photodegradable G147 Practice for Conditioning and Handling of Nonmetal-
plastics conducted in accordance with Practices G151 and lic Materials for Natural and Artificial Weathering Tests
G154. This practice also covers the preparation of test speci- G151 Practice for Exposing Nonmetallic Materials in Accel-
mens and the evaluation of test results. erated Test Devices that Use Laboratory Light Sources
G154 Practice for Operating Fluorescent Ultraviolet (UV)
1.2 Practice D4329 covers fluorescent UV exposures of Lamp Apparatus for Exposure of Nonmetallic Materials
plastics intended for long term use in outdoor applications. G169 Guide for Application of Basic Statistical Methods to
1.3 The values stated in SI units are to be regarded as Weathering Tests
standard. The values given in parentheses are for information
only. 3. Terminology
1.4 This standard does not purport to address all of the 3.1 The definitions given in Terminology G113 are appli-
safety problems, if any, associated with its use. It is the cable to this practice.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4. Significance and Use
bility of regulatory limitations prior to use. 4.1 Materials made from photodegradable plastics are in-
tended to show relatively rapid deterioration of chemical,
NOTE 1—There is no known ISO equivalent to this standard.
physical, and mechanical properties when exposed to light,
2. Referenced Documents heat, and water after fulfilling their intended purpose. This
practice is intended to induce property changes associated with
2.1 ASTM Standards:2 conditions that might be experienced when the material is
D3826 Practice for Determining Degradation End Point in discarded as litter, including the effects of sunlight, moisture,
Degradable Polyethylene and Polypropylene Using a Ten- and heat. The exposure used in this practice is not intended to
sile Test simulate the deterioration caused by localized weather phe-
D4329 Practice for Fluorescent Ultraviolet (UV) Lamp Ap- nomena such as atmospheric pollution, biological attack, and
paratus Exposure of Plastics salt water exposure.
D5870 Practice for Calculating Property Retention Index of
Plastics 4.2 Cautions—Variation in results can be expected when
E691 Practice for Conducting an Interlaboratory Study to operating conditions are varied within the accepted limits of
Determine the Precision of a Test Method this practice. Therefore, no reference to the use of this practice
G113 Terminology Relating to Natural and Artificial Weath- shall be made unless accompanied by a report prepared in
ering Tests of Nonmetallic Materials accordance with Section 9 that describes the specific operating
conditions used. Refer to Practice G151 for detailed informa-
tion on the caveats applicable to use of results obtained in
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and accordance with this practice.
is the direct responsibility of Subcommittee D20.96 on Environmentally Degradable
NOTE 2—Additional information on sources of variability and on
Plastics and Biobased Products.
strategies for addressing variability in the design, execution and data
Current edition approved April 1, 2014. Published April 2014. Originally
approved in 1991. Last previous edition approved in 2009 as D5208 - 09. DOI:
analysis of laboratory accelerated exposure tests is found in Guide G141.
10.1520/D5208-14.
2
4.3 Exposure of a similar material of known performance (a
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
control) at the same time as the test specimens provides a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on standard for comparative purposes. Use of a control to rank the
the ASTM website. stability of test materials greatly improves agreement between

*A Summary of Changes section appears at the end of this standard


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D5208 − 14
different laboratories.3,4 It is recommended that at least three mens to prevent loss of water vapor. Attach porous specimens
replicates of each material evaluated be exposed to allow for to a solid backing such as aluminum that can act as a vapor
statistical evaluation of results. barrier.
4.4 Test results will depend upon the care that is taken to 6.5 Unless otherwise specified, expose at least three repli-
operate the equipment in accordance with Practice G154. cate specimens of each test and control material.
Significant factors include regulation of line voltage, tempera-
6.6 Follow the procedures described in Practice G147 for
ture of the room in which the device operates, temperature
identification and conditioning and handling of specimens of
control, and condition and age of the lamps, if exposure is
test, control, and reference materials prior to, during, and after
conducted in a device without irradiance control.
exposure.
5. Apparatus 6.7 Do not mask the face of a specimen for the purpose of
5.1 Use of fluorescent UV apparatus that conform to the showing on one panel the effects of various exposure times.
requirements defined in Practices G151 and G154 is required to Misleading results can be obtained by this method, since the
conform to this practice. masked portion of the specimen is still exposed to temperature
and humidity cycles that, in many cases, will affect results.
5.2 The spectral power distribution of the fluorescent UV
lamp shall conform to the requirements in Practice G154 for a 6.8 Since the thickness of a specimen can markedly affect
UVA 340 lamp. the results, thickness of test and control specimens shall be
within 610 % of the nominal dimensions.
5.3 Test Chamber Location:
5.3.1 Locate the apparatus in an area maintained between 18 NOTE 3—This is especially important when mechanical properties are
and 27°C (65 and 80°F). Control of ambient temperature is being investigated.
particularly critical when one apparatus is stacked above 6.9 Retain a supply of unexposed file specimens of all
another, because the heat generated from the lower unit can materials tested.
interfere with the operation of the units above. 6.10 Specimens shall not be removed from the exposure
5.3.2 Place the apparatus at least 300 mm from walls or apparatus for more than 24 h and then returned for additional
other apparatus. Do not place the apparatus near a heat source tests, since this will not produce the same results on all
such as an oven. materials as tests run without this type of interruption. Report
5.3.3 Ventilate the room in which the apparatus is located to any elapsed time as noted under Section 9.
remove heat and moisture.
NOTE 4—Since the stability of the file specimen can also be time-
6. Test Specimens dependent, users are cautioned that over prolonged exposure periods, or
where small differences in the order of acceptable limits are anticipated,
6.1 The size and shape of specimens to be exposed will be comparison of exposed specimens with the file specimen are not neces-
determined by the specifications of the particular test method sarily valid. Instrumental measurements are recommended whenever
used to evaluate the effects of the exposure on the specimens; possible.
the test method shall be determined by the parties concerned.
Where practical, it is recommended that specimens be sized to 7. Procedure
fit specimen holders and racks supplied with the exposure 7.1 When the test and control specimens do not completely
apparatus. Unless supplied with a specific backing as an fill the specimen racks, fill all empty spaces with blank panels
integral part of the test, specimens shall be mounted so that to maintain the test conditions within the chamber.
only the minimum specimen area required for support by the
holder shall be covered. This unexposed surface must not be 7.2 Unless otherwise specified, control irradiance at 0.89
used as part of the test area. W/(m2 · nm) at 340 nm.
6.2 For specimens of insulating materials, such as foams, NOTE 5—In devices without irradiance control operated at 50 6 3°C
uninsulated black panel temperature the typical irradiance at 340 nm is
maximum specimen thickness is 20 mm in order to allow for 0.89 W/(m2 · nm). (See Note 1 of Table X2.1 in Practice G154 for a full
adequate heat transfer for condensation. explanation of the current default irradiance.)
6.3 To provide rigidity, attach flexible specimens to a 7.2.1 During equilibrium operation, the allowed deviation
backing panel made of aluminum, 0.635 mm (0.025 mm) thick. from the 340 nm set point is 60.02 W/(m2 • nm). If the
Suggested aluminum alloys are 5052, 6061, or 3003. indicated irradiance is outside the tolerance, stop the test and
6.4 Seal any holes in specimens larger than two mm and any correct the problem before continuing.
openings larger than one mm around irregularly shaped speci- 7.3 Unless otherwise specified, program the device to one of
the following test cycles.
3
Fischer, R., “Results of Round Robin Studies of Light- and Water-Exposure
7.3.1 Cycle A—20 h UV (light only) with uninsulated black
Standard Practices,” Accelerated and Outdoor Durability Testing of Organic panel temperature controlled at 50°C.
Materials, ASTM STP 1202, Warren D. Ketola and Douglas Grossman, Eds., 4 h Dark/condensation with uninsulated black
American Society for Testing and Materials, Philadelphia, 1993. panel temperature controlled at 40°C.
4
Ketola, W., and Fischer, R., “Characterization and Use of Reference Materials
in Accelerated Durability Tests,” VAMAS Technical Report No. 30. Available from Repeat this 24-hour cycle continuously until the desired total
NIST, Gaithersburg, MD. exposure is reached.

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D5208 − 14
experiments run to determine the test reproducibility from the
exposure and property measurement procedures. Conduct these
round-robins in accordance with Practice E691 and include a
statistically representative sample of all laboratories or orga-
nizations who would normally conduct the exposure and
property measurement. The precision and bias section contains
results from such a round-robin.
8.1.1 If a standard or specification for use between two or
three parties requires a definite property level after a specific
FIG. 1 Sample Rotation time or radiant exposure in an exposure test conducted in
accordance with this practice, base the specified property level
on two independent experiments run in each laboratory to
7.3.2 Cycle B—4 h UV (light only) with uninsulated black determine the reproducibility for the exposure and property
panel temperature controlled at 50°C. measurement process. The reproducibility of the exposure/
4 h Dark/condensation with uninsulated black property measurement process is then used to determine the
panel temperature controlled at 40°C. minimum level of property after the exposure that is mutually
Repeat this 8-hour cycle continuously until the desired total agreeable to all parties.
exposure is reached.
8.2 When reproducibility in results from an exposure test
7.3.3 Cycle C—continuous UV with uninsulated black panel
conducted in accordance with this practice have not been
temperature controlled at 50°C. Operate continuously until the
established through round-robin testing, specify performance
desired total exposure is reached.
requirements for materials in terms of comparison (ranked) to
7.3.4 During equilibrium operation, the maximum allow-
a control material. The control specimens shall be exposed
able deviation from the uninsulated black panel temperature set
simultaneously with the test specimen(s) in the same device.
point is 63°C. If the indicated temperature of the uninsulated
All concerned parties must agree on the specific control
black panel is outside these limits, stop the test and correct the
material used.
problem before continuing.
8.2.1 Conduct analysis of variance to determine whether
NOTE 6—The set points and tolerances for 7.2 and Cycles A, B, and C any differences between test materials and control materials are
represent an operational control point for equilibrium conditions at a
statistically significant. Expose replicates of the test specimen
single location in the cabinet, which does not necessarily represent the
uniformity of those conditions throughout the cabinet. ASTM Committee and the control specimen so that statistically significant per-
G03 is working to refine these tolerances and address the uniformity issue. formance differences can be determined.
7.3.5 Use Cycle C for materials that will be used for toxicity NOTE 7—Fischer illustrates use of rank comparison between test and
testing after exposure. This is essential because cycles that use control materials in specifications.5
condensation can wash away by-products of photochemical NOTE 8—Guide G169 includes examples showing use of analysis of
degradation. variance to compare materials.

7.4 Unless otherwise specified, reposition specimens as 8.3 In most cases, periodic evaluation of test and control
follows in order to minimize any effects from temperature or materials is necessary to determine the variation in magnitude
UV light variation. Figure 1 shows a diagram of the specimen and direction of property change as a function of exposure time
repositioning. or radiant exposure.
7.4.1 Reposition the specimens horizontally at least every 8.4 The time or radiant exposure necessary to produce a
third day by (1) moving the two extreme right hand holders to defined change in a material property can be used to evaluate
the far left of the exposure area, and (2) sliding the remaining or rank the stability of materials. This method is preferred over
holders to the right. evaluating materials after an arbitrary exposure time or radiant
7.4.2 Reposition the specimens vertically so that each speci- exposure.
men spends the same amount of exposure time in each vertical 8.4.1 Exposure to an arbitrary time or radiant exposure can
position within the specimen holder. For instance, if two be used for the purpose of a specific test if agreed upon by the
specimens are stacked vertically in each holder, then the top parties concerned. When a single exposure period is used,
and bottom specimens shall switch places halfway through the select a time or radiant exposure that will produce the largest
test. If four specimens are stacked vertically, then reposition performance differences between the test materials or between
the specimens vertically three times during the test. the test material and the control material.
7.5 Identification of any control specimen used shall accom- 8.5 Evaluate or rate changes in exposed test specimens in
pany the report. accordance with applicable ASTM test methods.
8. Periods of Exposure and Evaluation of Test Results
8.1 If a standard or specification for general use requires a 5
Fischer, R., Ketola, W., “Impact of Research on Development of ASTM
definite property level after a specific time or radiant exposure
Durability Testing Standards,” Durability Testing of Non-Metallic Materials, ASTM
in an exposure test conducted in accordance with this practice, STP 1294, Robert Herling, Editor, American Society for Testing and Materials,
base the specified property level on results from round-robin Philadelphia, 1995.

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D5208 − 14
TABLE 1 Results from Round-Robin Test
Tensile Elongation Determined in Accordance with Practice D3826
Material Average Repeatability Reproducibility Repeatability Reproducibility
Tested Standard Standard Limit, r Limit, R
Deviation, sf Deviation, sR
ECOA , unexposed 187.0 67.7 185.5 189.6 519.5
ECO, exposed 240 hB 1.7 0.8 1.1 2.3 3.0
white LLC , exposed 24 hB 364.7 64.5 110.0 180.6 308.1
white LL, exposed 240 hB 4.0 2.1 4.6 5.8 12.8
clear LL, exposed 24 hB 531.3 110.2 110.2 308.5 308.5
clear LL, exposed 240 hB 75.1 26.7 152.7 74.8 427.5
A
ECO material is ethylene/carbon monoxide copolymer which is known to degrade under UV exposure.
B
The exposure used for this round-robin was Cycle A of this standard.
C
LLDPE and white LLDPE are blown film low density polyethylene with an additive to promote degradation by solar radiation. Clear LLDPE was natural in color, while
white LLDPE had some TiO2 added to provide the white color.

8.5.1 When testing degradable polyethylene and 9.1.7 Specimen repositioning procedure, if different from
polypropylene, conduct tensile tests in accordance with Prac- the procedure described in 7.3, and
tice D3826 to determine the degradation end point. 9.1.8 Type of property tests and results. Calculate retention
8.5.2 In accordance with EPA regulation 40 CFR Part 238, of characteristic property in accordance with Practice D5870
a polyethylene or polypropylene material cannot be considered when it is reported.
as photodegradable when tested in accordance with this prac-
10. Precision and Bias6
tice if an exposure of longer than 250 light hours using Cycle
A is needed to produce degradation end point determined in 10.1 Precision:
accordance with Practice D3826. 10.1.1 The repeatability and reproducibility of results ob-
tained in exposures conducted in accordance with this practice
NOTE 9—For some materials, changes can continue after the specimen
has been removed from the exposure apparatus. Make measurements
will vary with the materials being tested, the material property
(visual or instrumental) within a standardized time period or as agreed being measured, and the specific test conditions and cycles that
upon between interested parties. The standardized time period needs to are used. It is essential to determine reproducibility of the
consider conditioning prior to testing. exposure/property measurement process when using the results
from exposures conducted in accordance with this practice in
9. Report
product specifications.
9.1 Report the following information: 10.1.2 A round-robin conducted and analyzed in accordance
9.1.1 Type and model of exposure device. with Practice E691 for exposures of three degradable poly-
9.1.2 If exposure is conducted in a device without irradiance olefin polymers produced the repeatability and reproducibility
control, record the age of fluorescent lamps used at the start of results for tensile elongation shown in Table 1.
the exposure, and note whether any lamps were exchanged
NOTE 10—For this round-robin, six laboratories exposed three different
during the period of exposure. materials supplied by two laboratories. Each participating laboratory
9.1.3 If required, report irradiance measured at a single exposed five replicate specimens. After exposure, the specimens were
wavelength in W/(m2 · nm) and radiant energy measured at a returned to the originating laboratory for tensile testing.
single wavelength in J/(m2 · nm). For measurements made over 10.2 Bias:
a broad band, such as 300–400 nm, report irradiance in W/m2 10.2.1 Bias cannot be determined because no acceptable
and radiant exposure in J/m2, specifying the spectral region standard weathering reference materials are available.
measured.
9.1.3.1 Do not report spectral irradiance or radiant exposure 11. Keywords
unless direct measurement of spectral irradiance was made 11.1 degradation; exposure; fluorescent UV; light exposure;
during the exposure. ultraviolet
9.1.4 Elapsed exposure time,
9.1.5 Light and dark-moisture-condensation periods, 6
Supporting data have been filed at ASTM International Headquarters and may
9.1.6 Operating uninsulated black panel temperature, be obtained by requesting Research Report RR: RR:D20-1205.

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D5208 − 14
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5208 - 09)
that may impact the use of this standard. (April 1, 2014)

(1) Added “if exposure is conducted in a device without (5) Removed old 9.1.7 since it references humidity.
irradiance control” at the end of 4.4. (6) Removed reference to G53 from 2.1.
(2) Removed “6 0.02” from 7.2 as redundant to 7.2.1, and (7) Removed requirement to measure temperature within 6 in.
could be misinterpreted to mean can be set between 0.87 and of device in 5.3.1.
0.91. (8) Grammar corrected in 4.4.
(3) Minor revision to 9.1.2 for clarity. (9) Removed non-mandatory language.
(4) Removed humidity in 9.1.5 as it is not controlled in a
fluorescent UV device.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5224 − 12 (Reapproved 2019)

Standard Practice for


Compression Molding Test Specimens of Thermosetting
Molding Compounds1
This standard is issued under the fixed designation D5224; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 2.2 ISO Standard:


1.1 This practice covers the general principles to be fol- ISO 295 Plastics—Compression Molding Test Specimens
lowed when compression molding test specimens of thermo- of Thermosetting Materials3
setting molding compounds, such as phenolics, aminoplastics, ISO 3167 Plastics—Multipurpose—Test Specimens3
melamine phenolics, epoxies, and unsaturated polyesters.
3. Terminology
1.2 Molding conditions are given for amino, phenolic, and
allyl molding compounds. The exact molding conditions will 3.1 Definitions—For definitions of terms pertaining to plas-
vary from material to material, and, if not incorporated in the tics used in this practice, see Terminology D883.
material specification, shall be agreed upon between the 3.2 Definitions of Terms Specific to This Standard:
purchaser and the supplier or determined by previous experi- 3.2.1 breathe step, n—in plastics molding, the part of the
ence with the particular type of material being used molding cycle in which the mold halves are opened
1.3 The values stated in SI units are to be regarded as momentarily, prior to curing, to release volatiles from the
standard. The values in parentheses are given for information molded part.
only. 3.2.2 skin, n—in plastics molding, the thin resin-rich layer
1.4 This standard does not purport to address all of the (skin) on the surface of the molded part.
safety concerns, if any, associated with its use. It is the 3.2.3 skin effect, n—in plastics testing, the positive or
responsibility of the user of this standard to establish appro- negative effect on the results of some standard tests attributable
priate safety, health, and environmental practices and deter- to the skin.
mine the applicability of regulatory limitations prior to use.
4. Summary of Practice
NOTE 1—This standard and ISO 295 address the same subject matter,
but differ in technical content. 4.1 Compression molded test specimens are produced by
1.5 This international standard was developed in accor- loading a mold cavity with some form of the molding material,
dance with internationally recognized principles on standard- applying a specified pressure to the mating surface for a
ization established in the Decision on Principles for the specified time and at a specified temperature, and then remov-
Development of International Standards, Guides and Recom- ing the part from the cavity.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 5. Significance and Use
5.1 The conditions at which compounds are molded are
2. Referenced Documents
known to influence the properties of the specimens. The degree
2.1 ASTM Standards:2 of cure, elimination of knit-lines between particles, density of
D638 Test Method for Tensile Properties of Plastics the part, and degradation of the polymer are among those
D883 Terminology Relating to Plastics factors which will be affected by the molding conditions. Thus
it is important to conform to a standard set of conditions in
1
order to have a valid comparison of properties between
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and
different compounds and different batches of the same com-
is the direct responsibility of Subcommittee D20.09 on Specimen Preparation.
Current edition approved May 1, 2019. Published June 2019. Originally pound.
approved in 1992. Last previous edition approved in 2012 as D5224 - 12. DOI:
10.1520/D5224-12R19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM ISO Standards Handbook 21, Vol 2, Plastics, 2nd Ed., 1990, available from
Standards volume information, refer to the standard’s Document Summary page on American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York,
the ASTM website. NY 10036.

*A Summary of Changes section appears at the end of this standard


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D5224 − 12 (2019)

FIG. 1 Single-Cavity Positive-Compression Mold for Bar Test


Specimens

5.2 Molded specimens showing evidence of low-density


areas due to trapped gases shall be discarded. A breathe step
can be incorporated to eliminate this situation. If used, it is
critical that the breathe step be as brief as possible to avoid
precuring of the compound before full pressure is applied
FIG. 2 Compression Mold for Disk Test Specimens
leading to poorly “knitted” areas and lower strength in the
molded specimen.

6. Apparatus 6.1.4 A cavity draft angle not exceeding 3° can be used to


6.1 Molds: facilitate specimen removal.
6.1.1 The mold shall be made of steel, able to withstand the 6.1.5 The clearance between the vertical wall of the cavity
molding temperatures and pressures. The mold shall be de- and that of the force shall not exceed 0.1 mm (0.004 in.).
signed such that the compressive mold force is transferred to 6.1.6 Mold surfaces finished to a roughness of 0.4 to 0.8 µm
the molding material with no appreciable loss. The molds (SPI-SPE #2 or equivalent4) are preferred, unless it is known
shown in Figs. 1 and 2 are recommended for maintaining the that the particular test is not affected by a coarser surface finish.
maximum force on the material. They are of the three-plate Chrome plating is recommended but not necessary. Draw
design; consisting of a shell or floating plate, with upper and polishing of all cavity surfaces in the direction parallel to the
lower compression plates. Molds may be of single or multiple force will facilitate specimen removal.
cavity design. 6.1.7 If ejector pins are used, they shall not deform the
specimens and their placement shall be such that the pin marks
NOTE 2—Semi-positive molds can be used, and for materials such as are not in the area of test.
amino compounds, are preferred. 6.1.8 The mold shall have a loading chamber of sufficient
6.1.2 The majority of tests will use bars 12.7 mm (0.5 in.) in volume to allow the introduction of the entire charge of
width by 127 mm (5 in.) or 64 mm (2.5 in.) in length, discs 51 material in a single loading. Preforms can be used to decrease
mm (2 in.) or 102 mm (4 in.) in diameter or an appropriate the required loading volume of high bulk materials. The
tensile bar as described in Test Method D638 or the multi- conditions of such preforming shall be included in the report.
purpose design from ISO 3167. The mold shall be capable of 6.1.9 As the specimen surface facing the lower die is heated
molding thickness from 1.5 mm (0.06 in.) to 12.5 mm (0.5 in.). for a longer time and at a higher temperature in the time
Some procedures such as flame testing require thinner speci- interval between filling and compression, it is recommended
mens. In all cases the ASTM Standard Test Procedure to be that a mark be placed on one cavity face in such a position that
used shall be consulted for the dimensions of the required test it will not interfere with the testing. When reporting the results
specimens. of tests that affect the surfaces unequally, the tested surface
6.1.3 If at all possible, specimens shall be molded directly to shall be indicated.
dimension, rather than machined from a plaque to maintain the 6.2 Press—The hydraulic press shall have a range of pres-
integrity of any skin effect. sures sufficient to insure that the specified pressure is applied
6.1.3.1 If it is necessary for specimens to be machined from
plates or plaques, they shall not be taken from the edge of the
plaque and a minimum margin of 10 mm (0.5 in.) is recom- 4
Mold comparison kits are available from the D-M-E Company, 29111 Stephen-
mended. This shall be noted in the report. son Highway, Madison Heights, MI 48071.

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TABLE 1 Molding Conditions for Compression Molding of Thermoset Molding Compounds
Molding Condition A B C D E F G H
Charge powder preformA powder or preformB powder, pill, or granular powder or preformB powder powder preform
Preheating none electronic air oven air oven none air oven electronic
Preheat temperature 104 to 115°C 90°C 90°C 120°C 107°C
Preheat time 30 min 60 min 10 min 25 to 30 s
Molding temperatureC 170°C 170°C 170°C 150°C 150°C 160°C 160°C 160°C
Molding pressureD,E 17 MPaE 17 MPa 17 MPa 28 MPa 28 MPa 20 MPa 20 MPa 20 MPa
Molding time
3.2 mm thickness 5 min 3 min 5 min 4 min 5 min 5 min 3 min 3 min
6.4 mm thickness 5 min
12.7 mm thickness 5 min
Breathing allowed allowed allowed allowed allowed when necessary (keep brief)
A
A single preform, preferably approximating the molded shape, shall be used. If more than one preform is used, weld lines may affect the test value of the specimen.
B
When using preforms, the material should be preheated in powder form, then preformed and molded immediately.
C
Molding temperatures should be held to within 3°C of the specified level.
D
Molding pressure should be held to within 2 MPa of the specified level.
E
Highly plastic materials may flash excessively under the molding pressure specified. If that occurs, molding pressure may be reduced to a minimum of 10 MPa, in which
case the pressure used shall be reported.

and maintained during the entire molding operation, and of a maximum depth of 13 mm (0.5 in.). Dry in an air-circulating
maintaining that pressure within 61.5 MPa (6218 psi). oven for 30 min at 90 6 3°C. Mold the material immediately
6.2.1 In order to prevent precure, the press shall be capable after conditioning.
of closing within 15 s after the placement of the material in the 7.3 Referee Testing: Allyl Molding Compounds:
mold. A two-speed press is preferred for this purpose. The fast 7.3.1 For referee testing of all test specimens, place a
approach speed can be in the range of 200 to 400 mm/s (8 to sufficient quantity of material in an open tray to a depth of 25
16 in./s) while the slow closing speed of 5 mm/s (0.2 in./s) is mm (1 in.) for 72 h in a standard laboratory atmosphere (23 6
used to prevent gas entrapment. 1°C, 50 6 5 % relative humidity).
6.3 Heating System—Mold heating can be accomplished by 7.4 Electronic Preheating:
conduction from heated platens, heaters inserted into the mold 7.4.1 When electronic preheating is to be used (refer to
itself, by hot fluids circulated through passageways in the Molding Conditions, Table 1), the objective is to attain a
mold, or any suitable alternative. The heating system shall be particular temperature as rapidly as possible. Determine the
capable of controlling the mold temperature to 63°C (65°F) conditions necessary to attain that temperature with spare
from point-to-point on the mold and for the duration of the preforms which are then discarded. Do not use this type of
molding time. preheating when preparing electrical test specimens. The
6.3.1 If the mold is heated directly, it shall be insulated from material shall be transferred to the mold immediately after
the press platens with a sheet of insulating material. preheating to prevent cooling or premature curing.
NOTE 3—It is generally preferable to heat the mold electrically. 7.5 Preplastification:
6.4 Temperature-Measurement System: 7.5.1 Preplastification is permissible to insure thermal and
6.4.1 Mold Temperature—A surface pyrometer or equiva- mechanical homogenization of the material. The preplasticized
lent means is used to measure the temperature of the mold material shall be molded immediately after preplastification to
surface. prevent cooling or premature curing. Preplastification condi-
6.4.2 Preheated Compound Temperature—If the compound tions shall be the subject of an agreement between the
is to be preheated to a definite temperature, a needle-probe interested parties and shall be included in the molding report.
pyrometer or equivalent sensitive to 62°C shall be used.
8. Procedure
7. Conditioning
8.1 Unless directed otherwise in the material specification,
7.1 Except for referee testing and preparation of samples for mold test specimens under the conditions listed in Table 1.
electrical tests, prior conditioning of the material is not 8.1.1 The “breathe step,” if used, is done by slightly opening
required. the mold for a few seconds to release volatiles generated by the
7.2 Referee Testing: Phenolic and Amino Molding Com- curing process and is done after it has already been closed at
pounds: the molding temperature.
7.2.1 For the referee testing of all but electrical specimens, 8.1.2 Release agents are not normally needed as molding
place a sufficient quantity of material in an open tray to a compounds have internal lubricants to facilitate mold release.
maximum depth of 13 mm (0.5 in.) for 72 h in a standard If release agents are used it shall be shown that they have no
laboratory atmosphere (23 6 1°C, 50 6 5 % relative humid- influence on the test specimen properties. They shall be noted
ity). in the report.
7.2.2 For the preparation of electrical test specimens, place 8.1.3 Cooling fixtures can be used to prevent warpage upon
a sufficient sample of the molding material in an open tray to removal of the specimens from the mold.

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D5224 − 12 (2019)
8.2 Phenolic Molding Compounds: 9. Report
8.2.1 Use conditions A or B from Table 1 for impact, 9.1 Report the following information:
flexure, tension, water absorption, heat deflection, heat-aging 9.1.1 Type and description of material used,
tests. 9.1.2 Description of the mold,
8.2.2 Use Condition C from Table 1 for electrical test 9.1.3 State of material molded (as received or with “referee
specimens. test” conditioning),
8.3 Amino Molding Compounds: 9.1.4 Molding condition used (A, B, C, D, E, F, G, or H) and
any variations from the listed condition,
8.3.1 For urea-formaldehyde compounds use Condition D
9.1.5 Whether or not a “breathe step” was used during
from Table 1.
molding,
8.3.2 For melamine-formaldehyde compounds use Condi- 9.1.6 Whether any specimens were machined, and
tion E from Table 1. 9.1.7 Whether any release agents were used.
8.4 Allyl Molding Compounds—Use conditions F, G, or H NOTE 4—A report form (Fig. 3) identifying all pertinent information is
from Table 1. provided for reference.
8.5 Molding Pressures: 10. Precision and Bias
8.5.1 The molding pressures shown in Table 1 are recom-
10.1 Inasmuch as this practice does not generate a numeri-
mended and shall be used for all referee molding and testing.
cal result, a precision and bias estimate is not possible.
If other pressures are to be used, the oil pressure p0 in
However, the procedures used during molding of test speci-
megapascals (MPa), to be displayed on the pressure gauge in
mens will affect the numerical results from tests done on the
order to obtain the specified pressure p, in megapascals, is
specimens. Thus variabilities in the molding procedure will
given by the equation:
contribute to variability in the final test results.
p 0 5 ~ p 3 A 1 ! /A (1)
11. Keywords
where:
11.1 allyl molding compound; amino molding compound;
A = the area of the press piston head, m2, and compression molding; phenolic molding compound; plastics;
A1 = the total area of the cavities, m2.
thermoset

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FIG. 3 Compression Molding Report

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5225 − 17

Standard Test Method for


Measuring Solution Viscosity of Polymers with a Differential
Viscometer1
This standard is issued under the fixed designation D5225; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* mendations issued by the World Trade Organization Technical


1.1 This test method covers the determination of the solu- Barriers to Trade (TBT) Committee.
tion viscosity of polymers using a differential or the modified
2. Referenced Documents
differential viscometer. It is applicable to all polymers that
dissolve completely without chemical reaction or degradation 2.1 ASTM Standards:2
to form solutions that are stable with time and temperature. D1243 Test Method for Dilute Solution Viscosity of Vinyl
Results of the test are usually expressed as specific viscosity, Chloride Polymers
intrinsic viscosity (limiting viscosity number), inherent viscos- D2857 Practice for Dilute Solution Viscosity of Polymers
ity (logarithmic viscosity number), or relative viscosity (vis- E691 Practice for Conducting an Interlaboratory Study to
cosity ratio). Determine the Precision of a Test Method
E2935 Practice for Conducting Equivalence Testing in
1.2 Since there is more than one type of viscometer avail-
Laboratory Applications
able to measure a differential pressure, follow the manufactur-
er’s directions applicable to the equipment being used. 3. Terminology
1.3 The solution viscosity values are comparable with those 3.1 Definitions:
obtained using a glass capillary of Test Method D2857. This 3.1.1 inherent viscosity—the ratio of the natural logarithm
test method differs from the glass capillary in that the solvent of the relative viscosity to the concentration. The IUPAC term
and the solution are compared at the same time that a test is for inherent viscosity is logarithmic viscosity number.
run. With a glass capillary, each solution must be referenced
3.1.2 intrinsic viscosity—limit of the reduced and inherent
back to the solvent run in the same capillary at the same
viscosities as the concentration of the polymeric solute ap-
temperature.
proaches zero and represents the capacity of the polymer to
1.4 The values stated in SI units are to be regarded as increase viscosity. The IUPAC term for intrinsic viscosity is
standard. No other units of measurement are included in this limiting viscosity number.
standard. 3.1.3 reduced viscosity—the ratio of the specific viscosity to
1.5 This standard does not purport to address all of the the concentration. Reduced viscosity is a measure of the
safety concerns, if any, associated with its use. It is the specific capacity of the polymer to increase the relative
responsibility of the user of this standard to establish appro- viscosity. The IUPAC term for reduced viscosity is viscosity
priate safety, health, and environmental practices and deter- number.
mine the applicability of regulatory limitations prior to use. 3.1.4 relative viscosity—the ratio of the polymer solution
For specific hazard statements, see Section 8. pressure to the pressure of the solvent.
NOTE 1—There is no known ISO equivalent to this standard. 3.1.5 specific viscosity—the relative viscosity minus one.
1.6 This international standard was developed in accor- 3.1.6 viscosity constant, K—baseline reading when solvent
dance with internationally recognized principles on standard- is present in both capillaries.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 4. Summary of Test Method
4.1 Differential Viscometer (Fig. 1):

1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
2
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2017. Published January 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1992. Last previous edition approved in 2014 as D5225 - 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5225-17. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D5225 − 17
across the capillaries. A pump continuously supplies solvent
flow. The ratio of the pressures P2 and P1 is proportional to the
ratio of the viscosities of the fluid in capillary 2 to that in
capillary 1.
P2 η2
5K 5 K·Relative Viscosity (2)
P1 η1

4.2.1.1 K, the viscosity constant, is obtained from the


baseline reading when solvent is present in both capillaries, so
η2/η1 is unity.
4.2.1.2 With the valve in LOAD position, the sample is
flushed through the sample loop by the syringe pump. A
baseline reading is established and recorded by the computer
data acquisition system. When the valve is switched to the
INJECT position, solvent flowing from capillary 1 pushes the
sample into capillary 2. The differential pressure P2 will
increase due to the higher viscosity of the sample solution. The
steady state value of P2/P1 then yields the value of relative
NOTE 1—
R1, R2, R3, R4 = Matched SS Capillary Tubing viscosity of the sample.
A, B = Solution Holdup Reservoirs P2
SA, SB = Switching Valve Relative Viscosity 5 (3)
KP1
Pi = Solvent Inlet Pressure Transducer
∆P = Differential Pressure Transducer 4.2.1.3 Absolute viscosity of the sample may be calculated
FIG. 1 Differential Viscometer
from relative viscosity, RV, assuming the viscosity of the
solvent is known.
4.1.1 The viscosity measurement with the differential vis- η ~ sample! 5 RV·η ~ solvent! (4)
cometer is based on a fluid analog of the Wheatstone Bridge.
Pure solvent at constant inlet pressure Pi enters a balanced 5. Significance and Use
capillary network and flows through, producing a zero or
5.1 Solution viscosity values for polymers are related to the
baseline pressure on the differential pressure transducer. Solu-
average molecular size of that portion of the polymer which
tion is loaded into the sample reservoir A and then injected
dissolves in the solvent.
onstream by means of the switching valve SA. The differential
pressure begins to rise until it reaches a steady state value of
6. Apparatus
∆P proportional to the specific viscosity of the solution. The
differential pressure is monitored continuously on a strip chart 6.1 Differential Viscometer, or Relative Viscometer, Dilute
recorder or computer, providing a baseline where ∆P is Solution Viscosity (DSV) System,
measured. The equation relating ∆P to specific viscosity is: 6.2 Glass Vial, 25 mL,
4∆P 6.3 Screw Type Cap, open top, size 24-400,
η sp 5 (1)
P i 2 2∆P
6.4 Septa, aluminum foil (household grade) or acceptable
4.1.2 Derivation of the equation is in Annex A1. substitute,
4.2 Modified Differential Viscometer (Fig. 2): 6.5 Balance, capable of weighting to 0.0001 gms,
4.2.1 The modified differential viscometer has two stainless
6.6 Filter Funnel, and
steel capillaries connected in series with a sample loading/
injection valve before the second capillary. Two differential 6.7 Filter medium, coarse filter paper or metal screen of 140
pressure transducers, P1 and P2, are connected in parallel mesh or finer.

7. Reagents and Materials


7.1 Polymer Sample.
7.2 Solvent.
7.3 Compressed Gas Cylinder of nitrogen or helium.

8. Hazards
8.1 Flammable solvents are to be used in a hood or a well
ventilated area.
8.2 Solvents are to be dated and to be used on a first-in
FIG. 2 Relative Viscometer first-out basis.

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D5225 − 17
8.3 Stored solvents prone to develop peroxides should be data in Table 1 should not be rigorously applied to acceptance
tested on a regular schedule for peroxide development. or rejection of material, as those data are specific to the one
laboratory and may not be representative of other lots,
9. Procedure conditions, materials, or laboratories.)
9.1 Set viscometer oven temperature to maintain solution of
NOTE 2—Users of this test method should apply the principles outlined
the test polymer. in Practice E691 to generate data specific to their laboratory and materials,
9.2 Adjust inlet solvent pressure to obtain the pressure or between specific laboratories. The principles of 11.2.1 through 11.2.3
differential and test time desired. would then be valid for such data.

9.3 Prepare polymer solution. Weigh the polymer accurately 11.2 Concept of Ir and IR—If Sr and SR have been calculated
to the nearest 1.0 6 0.1 mg and record weight. from a large enough body of data, then the following applies:
9.4 Filter polymer solution into a 25-mL vial. Cover vial 11.2.1 Repeatability—The value below which the absolute
with an aluminum septa or equivalent and cap. difference between two individual test results obtained under
repeatability conditions is likely to be expected to occur with a
9.5 Program the instrument and processing parameters for probability of approximately 0.95 (95 %).
the desired viscosity calculations.
11.2.2 Reproducibility—The value below which the abso-
9.6 Initiate viscosity acquisition. lute difference between two test results obtained under repro-
9.7 After the last sample has been run, flush the sample lines ducibility conditions is likely to be expected to occur with a
and sample holder with fresh solvent. probability of approximately 0.95 (95 %).
9.8 Turn off viscometer, leaving the sample lines filled with 11.2.3 Equivalence testing on numerical data from two
solvent. sources shall be conducted in accordance Practice E2935 or
any known method for judging the equivalence of two means.
10. Report
NOTE 3—Example: A t-test.
10.1 Report viscosity data for each sample in the run queue.
11.3 Bias is systematic error which contributes to the
11. Precision and Bias difference between a test result and a true (or reference) value.
11.1 Table 1 is the precision data for eight polymers which There are no recognized standards on which to base an estimate
were measured using this test method. Each result is an average of bias for this test method.
of three or more independent tests made by a single laboratory.
(Warning—The following explanations of Ir and IR (11.2 thru 12. Keywords
11.2.3) are only intended to present a meaningful way of 12.1 differential solution viscosity; differential viscometer;
considering the approximate precision of this test method. The polymer solution viscosity

ANNEX

(Mandatory Information)

A1. CALCULATIONS FOR DIFFERENTIAL VISCOMETER

TABLE 1 Precision Data for the Solution Viscosities of Various PolymersA


Relative Viscosity Inherent Viscosity Intrinsic Viscosity
Polymer Solvent Concentration
Mean Sr Ir Mean Sr Ir Mean Sr Ir
poly(1-butene) decalin 0.1 g/100 mL 1.207 0.007 0.020 1.853 0.054 0.153 1.892 0.057 0.161

polycarbonate methylene chloride 0.5 g/100 mL ... ... ... 0.460 0.003 0.0085 0.472 0.003 0.0085
poly(ethylene) decalin 0.1 g/100 mL 1.124 0.005 0.014 1.166 0.044 0.125 1.181 0.045 0.127
poly(4-methyl-1-pentene) decalin 0.1 g/100 mL 1.280 0.007 0.018 2.294 0.051 0.144 2.361 0.054 0.153
poly(propylene) decalin 0.1 g/100 mL
resin “A” 1.170 0.005 0.014 1.557 0.042 0.112 1.585 0.044 0.125
resin “B” 1.182 0.005 0.014 1.664 0.045 0.127 1.695 0.047 0.133
resin “C” 1.254 0.008 0.021 2.240 0.060 0.170 2.299 0.063 0.178
resin “D” 1.289 0.007 0.018 2.516 0.052 0.147 2.593 0.056 0.158
resin “E” 1.415 0.003 0.008 3.452 0.021 0.059 3.604 0.022 0.062
poly(phenylene oxide) chloroform 0.1 g/100 mL 1.053 0.0005 0.001 0.500 0.003 0.0085 0.503 0.003 0.009
poly(styrene) toluene 0.1 g/100 mL 1.095 0.0006 0.002 0.726 0.0015 0.004 0.737 0.0025 0.007
poly(vinyl chloride) tetrahydrofuran 0.2 g/100 mL 1.225 0.0003 0.0009 1.015 0.001 0.003 1.039 0.001 0.003
A
This data was generated by a Viscotek Model 100-01 viscometer, Malvern Instruments, 117 Flanders Rd., Westborough, MA.

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D5225 − 17
A1.1 Assume R3 is filled with solution and R1, R2, R4 are Q 1 η o 1η o 2η o
5 5 (A1.4)
filled with solvent. The measured quantities are the inlet Q2 η o 1η η o 1η
pressure Pi and the differential pressure ∆P.
A1.5 Combining Eqs (A1.2), (A1.3), and (A1.4), we find
∆P P 1 2 P 2 the following:
5 (A1.1)
Pi Pi
∆P
Pi
5 1/2 F
η 2 ηo
η1η o G (A1.5)
P1 = pressure drop across R3 and
P2 = pressure drop across R4. A1.6 The definition of specific viscosity of a solution is as
follows:
A1.2 R2 and R4 have equal flow resistance, so Pi = 2P2,
giving the following: η 2 ηo
η sp 5 (A1.6)
ηo
∆P
Pi
5 1/2
P1
P2 F
21 G (A1.2)
A1.7 Substituting into Eq (A1.5) yields the following:
A1.3 Applying Poiseuelle’s Law to capillaries R3 and R4: ∆P η sp
5 (A1.7)
Pi 2η sp14
P1 ηQ 1
5 (A1.3)
P 2 η oQ 2 A1.7.1 Rearrange to give the following:
4∆P
η sp 5 (A1.8)
Q1 = flow rate through R1, R3, P i 2 2∆P
Q2 = flow rate through R2, R4,
η = viscosity of solution, and A1.8 Assumptions in Derivation:
ηo = viscosity of solvent. A1.8.1 Capillaries have equal flow resistance.
A1.4 The ratio of flow rates Q1/Q2 is equal to the inverse A1.8.2 Capillaries obey Poiseuelle’s Law.
ratio of the total resistance in each side of the bridge.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5225 - 14)
that may impact the use of this standard. (December 1, 2017)

(1) Revised 6.5 to clarify accuracy of balance being used. (3) Added Note 3.
(2) Subsections 11.2.1, 11.2.2, and 11.2.3: Removed passive
language.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5226 − 16

Standard Practice for


Dissolving Polymer Materials1
This standard is issued under the fixed designation D5226; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 4.1.1 A polymer and a list of suggested solvents for making


1.1 This practice outlines the parameters applicable to the a solution are listed in Annex A1.
preparation of a polymeric solution, such as solvent, 4.1.2 Table 1 designates the parameters for container, heat-
concentration, temperature, pressure, time, agitation, and heat- ing mode, and type of agitation.
ing mode. NOTE 2—To illustrate the use of the cell classifications with Table 1, a
1.2 The proper use of this practice requires knowledge of 2 % solution of poly(vinyl chloride) using cyclohexanone would be
written as:
solvents and their effect on polymeric materials.
PVC 2 cyclohexanone 2 20 2 66 2 40 2 BEC
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the where:
responsibility of the user of this standard to establish appro- PVC = abbreviation of the polymer from Annex A1,
priate safety and health practices and determine the applica- cyclohexanone = the solvent from Annex A1,
bility of regulatory limitations prior to use. 20 = weight of polymer in tenths of a percent,
66 = temperature in degrees Celsius,
NOTE 1—There is no known ISO equivalent to this standard. 40 = time in tenths of an hour,
B = glass container from Table 1,
2. Referenced Documents E = bath heater from Table 1, and
C = random agitation from Table 1.
2.1 ASTM Standards:2
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plas- 5. Significance and Use
tics 5.1 This practice embodies the specifications to describe the
2.2 Other Document: preparation of a polymeric solution.
Polymer Handbook3
6. Procedure
3. Terminology
6.1 Polymer—Select the applicable polymer from Annex A1
3.1 Definitions are in accordance with Terminology D883. and write its abbreviation.
3.2 Abbreviations are in accordance with Terminology
6.2 Solvent—Select the solvent applicable to the polymer
D1600.
from Annex A1.
4. Summary of Practice 6.3 Concentration—Write the polymer gram weight in
4.1 A polymer solution is described or prepared using the tenths of a percent per milliliter of solvent.
cell classifications listing the parameters relative to solvate the 6.4 Temperature—Write the solution temperature in degrees
polymer. The cell classifications are listed in the following Celsius.
order: polymer, solvent, concentration, temperature, time,
container, heating mode, and agitation. 6.5 Time—Write the time for solution in tenths of an hour.
6.6 Container—Select the type of container from Table 1.
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and 6.7 Heating Mode—Select the heating mode from Table 1.
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Sept. 1, 2016. Published September 2016. Originally 6.8 Agitation—Select the agitation mode from Table 1.
approved in 1992. Last previous edition approved in 2010 as D5226 - 98(2010)ɛ1.
DOI: 10.1520/D5226-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 7. Precision and Bias
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
7.1 No statement is made about the precision or bias of this
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. practice since the procedure is descriptive with no measure-
3
Available from John Wiley and Sons, New York, NY. ments being made.

*A Summary of Changes section appears at the end of this standard


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D5226 − 16
TABLE 1 Parameters 8. Keywords
Designation Container Heater Mode Agitation Mode
8.1 polymer solutions; solution preparation; solutions; sol-
A unspecified unspecified unspecified
B glass none none
vents
C sealed glass vial oven random
D metal hot plate magnetic stirrer
E fluoropolymer bath propeller blade
F block heater wrist action
G electric mantle ultrasonic
H microwave

ANNEX

(Mandatory Information)

A1. SUGGESTED SOLVENTS FOR POLYMERIC SOLUTIONS

A1.1 Note the following: A1.1.4 Solubility normally increases with rising tempera-
ture.
A1.1.1 The solvents in Table A1.1 are listed in random
order. A1.1.5 The temperature is for room temperature unless
noted.
A1.1.2 An increase in polymer molecular weight reduces
A1.1.6 The following abbreviations are used in Table A1.1:
solubility.
D.S. = degree of substitution,
A1.1.3 Branching increases the solubility compared to a S.C. = substituent content,
linear polymer of the same molecular weight. conc. = concentrated.
TABLE A1.1 Solvents
Abbreviation Polymer Solvents
ABA Acrylonitrile-butadiene-acrylate aromatic hydrocarbons, chlorinated hydrocarbons, tetrahydrofuran,
esters, ketones, N,N-dimethylformamide, N,N-dimethyl-acetamide (if
high acrylonitrile)
ABS Acrylonitrile-butadiene-styrene N,N-dimethylformamide, N,N-dimethylacetamide (if high acrylonitrile),
cyclohexanone (above 35°C), cyclohexanone/acetone,
methylcyclohexane/acetone, decahydronaphthalene/dimethyl oxalate,
benzene, toluene, ethylbenzene, styrene, lower chlorinated
hydrocarbons, phenol/acetone, tetrahydrofuran,
dimethyltetrahydrofuran, dioxane, methyl ethyl ketone, diisopropyl
ketone, glycol formal, ethyl acetate, butyl acetate, methyl-, ethyl-,
n-butyl phthalate, 1-nitropropane, carbon disulfide, tributyl phosphate,
phosphorus trichloride
Alkydes tetrahydrofuran
AMMA Acrylonitrile/metha methacrylate benzene, toluene, xylene, methylene chloride, chloroform, ethylene
chloride, chlorobenzene, isobutanol (hot), cyclohexanol (hot),
B-ethoxyethanol, dioxane, methyl ethyl ketone, diisopropyl ketone,
cyclohexanone, acetic acid, isobutyric acid, methyl formate, ethyl
acetate, cyclohexyl acetate, isobutyl propionate, butyl lactate
ADC Allyl diglycol carbonate benzene, chloroform, acetone
CMC Carboxylmethyl cellulose S.C. = 5 to 10 % —alkali
S.C. = 15 to 30 % —water (sodium salt)
S.C. = high—benzene/alcohol, benzene/acetone, chloroform, pyridine,
acetone, esters, tetrahydrofuran
CA Cellulose acetate D.S. = 0.6 to 0.8—water
D.S. = 1.3 to 1.7—2-methoxyethanol
D.S. = 2.0 to 2.3—methylene chloride/methanol at 80:20, chloroform/
methanol, benzyl alcohol, phenols, ethylene glycol ethers, dioxane,
diethanolamine, pyridine, aniline, acetone, cyclohexanone, formic acid,
glacial acetic acid, methyl acetate, ethyl acetate/nitrobenzene, glycol
monoethyl ether acetate, nitromethane, tetrahydrofuran
CAB Cellulose acetate-butyrate D.S. (acetate) = 0.8 and D.S. (butyrate) = 2.35—
benzene, toluene (hot), chloroform, carbon tetrachloride,
tetrachloroethane, methanol (hot), acetone, cyclohexanone, dioxane,
aliphatic esters, nitroethane
CAB Cellulose acetate-butyrate D.S. (acetate) = 2.1 and D.S. (butyrate) = 0.7—
chloroform, dichloroethane, tetrachloroethane, dioxane, acetone,
cyclohexanone, methyl acetate, ethyl acetate, nitroethane
CAP Cellulose acetate propionate benzene, dichloromethane, chlorobenzene, acetone, ethyl acetate

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D5226 − 16
TABLE A1.1 Continued
Abbreviation Polymer Solvents
CN Cellulose nitrate N = 6.8 % —water
N = 10.5 to 12 % —alcohol (lower), alcohol/diethyl ether, acetone,
amyl acetate, ethylene glycol ethers, acetic acid (glacial)
N = 12.7 % —halogenated hydrocarbons, ethanol/diethyl ether,
acetone, methyl amyl acetone, cyclohexanone, methyl acetate, ethyl
acetate, ethyl butyrate, ethyl lactate, ethylene glycol ether acetates,
ethylene carbonate, furan derivatives, nitrobenzene
CP Cellulose propionate benzene, dichloroethane, chlorobenzene, acetone, ethyl acetate
CTA Cellulose triacetate methylene chloride, methylene chloride/ethanol at 80:20, chloroform,
chloroform/alcohol, trichloroethane, tetrahydrofuran, dioxane, acetone,
acetone/water at 80:20, methyl acetate, ethylene glycol ether
acetates, ethylene carbonate
EPDM Diene-modified ethylene-propylene 1,2,4-trichlorobenzene, toluene at 75°C, 1,2,4-trichloro-benzene at
135°C
EP Epoxy, epoxide tetrahydrofuran
EC Ethyl cellulose D.S. = 0.5 to 0.7—aqueous alkali
D.S. = 1.0 to 1.5—pyridine, formic acid, water (cold), cuoxam
D.S. = 2—methylene chloride, chloroform, dichloroethylene,
chlorohydrins, ethanol, tetrahydrofuran
D.S. = 2.3—benzene, toluene, alkyl halogenoids, alcohols, furan
derivatives, ketones, acetic esters, carbon disulfide, nitromethane
D.S. = 3.0—benzene, toluene, methylene chloride, alcohols, esters
EEA Ethylene/ethyl acrylate aromatic hydrocarbons, chlorinated hydrocarbons, tetrahydrofuran,
esters, ketones
EMA Ethylene/methacrylic acid water, aqueous hydrogen chloride (0.002M above 30°C), dilute
aqueous sodium hydroxide
ETFE Ethylene-tetrafluoroethylene copolymer perfluorokerosene (350°C)
EVA Ethylene/vinyl acetate benzene, toluene, chloroform, carbon tetrachloride/ethanol,
dichloroethylene/ethanol at 20:80, chlorobenzene, methanol, ethanol/
water, n-butanol/water, allyl alcohol, 2,4-dimethyl-3-pentanol, benzyl
alcohol, tetrahydrofurfuryl alcohol, tetrahydrofuran,
dimethyltetrahydrofuran, dioxane, glycol ethers, glycol ether esters,
acetone, methyl ethyl ketone, acetic acid, lower aliphatic acids, vinyl
acetate, acetals, acetonitrile, nitromethane, N,N-dimethylformamide,
dimethyl sulfoxide, 1,2,4-trichlorobenzene at 135°C (if high ethylene
content)
LCP Liquid crystal polymer 50:50 1,2,4-trichlorobenzene/phenol at 175°C, pentafluorophenol
MF Melamine formaldehyde Very low molecular weight—alcohol, water
Intermediates—pyridine, formalin, formic acids, dilute and
concentrated acids
High molecular weight—m-cresol at 100°C, N,N-dimethylformamide,
N,N-dimethylacetamide, N-methyl pyrrolidone at 85 to 100°C
PF Phenol-formaldehyde Novalks and low molecular weight—hydrocarbons, diethyl ether,
acetone, esters, 4-tert-butylphenol and 4-phenylphenol polymers,
drying oils, tetrahydrofuran, methanol
Final resins—molten phenols (with some decomposition)
PAA Poly(acrylic acid) Atactic—methanol, ethanol, ethylene glycol, methyoxyethanol,
dioxane, formamide, N,N-dimethyl-formamide, water, dilute alkali
solution
Isotactic—dioxane/water at 80:20
PAN Polyacrylonitrile Polyacrylonitrile (PAN)—o-, m-, p-phenylene diamine,
N-formylhexamethyleneimine, N-nitrosopiperidine, maleic anhydride,
chloromaleic anhydride, succinic anhydride, acetic anhydride,
citraconic anhydride, g-butyrolactone, dioxanone, p-dioxanedione,
ethylene oxalate, ethylene carbonate, propylene carbonate,
2-oxazolidone, 1-methyl-2-pyridone, 1,5-dimethyl-2-pyrrolidone,
E-caprolactam, N,N-dimethyl-formamide, dimethylthioformamide,
N-methyl-B-cyanoethylformamide, cyanoaceticacid, a-cyano-
acetamide, N-methylacetamide, N,N-diethylacetamide, N,N-
dimethylacetamide, dimethylmethoxyacetamide, N,N-dimethyl-a,a,a-
trifluoroacetamide, N,N-dimethylpropionate, N,N,N’,N’-
tetramethyloxamide, hydroxyacetonitrile, chloro-acetonitrile/water,
B-hydroxypropionitrile, malonitrile, fumaronitrile, succinonitrile,
adiponitrile, bis(2-cyanoethyl)ether, bis(2-cyanoethyl)sulfide, bis(4-
cyanobutyl)sulfone, 1,3,3,5-tetracyanopentane, nitromethane/water
(94:6), 1,1,1-trichloro-3-nitro-2-propane, tri(2-cyanoethyl)nitromethane,
3-,4-nitrophenol, methylene dithiocyanate, trimethylene dithiocyanate,
dimethyl sulfoxide, tetramethylene sulfoxide, dimethyl sulfone, ethyl
methyl sulfone, 2-hydroxyethyl methyl sulfone, ethylene-1,2-bis-(ethyl
sulfone), dimethyl phosphite, diethyl phosphite, sulfuric acid, nitric
acid, p-phenol sulfonic acid, conc. aqueous lithium chloride, conc.
aqueous zinc chloride, conc. aqueous aluminum perchlorate, conc.
aqueous sodium thiocyanate, conc. aqueous calcium thiocyanate,
molten quaternary ammonium salts and their aqueous solutions

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D5226 − 16
TABLE A1.1 Continued
Abbreviation Polymer Solvents
PA Polyamide 6—m-cresol, chlorophenol, formic acid, acetic acid, trichloroacetic
acid, ethylene carbonate, sulfuric acid, phosphoric acid,
hexamethyltrisphosphoramide, hexafluoroisopropanol
6:6 (at room temperature)—trifluoroethanol, trichloroethanol, phenol,
cresols, chloral hydrate, formic acid, halogenated acetic acids,
hydrogen fluoride, hydrogen cyanide/methanol, liquid sulfur dioxide,
sulfuric acid, phosphoric acid, saturated solution of alcohol-soluble
salts, for example, calcium chloride, magnesium chloride, in methanol,
hexafluoroisopropanol
6:6 (at temperatures of 120 to 140°C)—benzyl alcohol, ethylene
chlorohydrin, 1,3-chloropropanol, 2-butene-1,4-diol, diethylene glycol,
acetic acid, formamide, N-acetylmorpholine, dimethyl sulfoxide
6:10—chlorobenzene, hexafluoroisopropanol, dimethyl succinate
(79°C)
11:—higher primary alcohols, N,N-dimethylformamide, dimethyl
sulfoxide, hexafluoroisopropanol
PA/PET Polyamide + Polyethylene terephthalate pentafluorophenol
PB Poly(butadiene) tetrahydrofuran, toluene, chloroform
PBAN Polybutadiene-acrylonitrile benzene, halogenated hydrocarbons, aliphatic, cycloaliphatic and
aromatic hydrocarbons, chlorinated hydrocarbons, tetrahydrofuran,
higher ketones, higher aliphatic esters, N,N-dimethylformamide, N,N-
dimethylacetamide (if high acrylonitrile content)
PBS Polybutadiene-styrene benzene, halogenated hydrocarbons, aliphatic, cycloaliphatic and
aromatic hydrocarbons, chlorinated hydrocarbons, tetrahydrofuran,
higher ketones, higher aliphatic esters
PBT Poly(butylene terephthalate) m-cresol at 100°C, hexafluoroisopropanol
PB Polybutene-1 see Polyethylene
PC Polycarbonate benzene, chloroform, acetone, tetrahydrofuran, methylene chloride
Neoprene Polychloroprene tetrahydrofuran, toluene
PEEK Polyetheretherketone 50:50 1,2,4-trichlorobenzene/phenol at 135°C
PEI Poly(ether imide) N-methyl pyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide
at 85°C
PES Poly(ether sulfone) tetrahydrofuran, N,N-dimethylformamide
PE Polyethylene High-density (HDPE) (at temperatures above 80°C)—aliphatic,
cycloaliphatic, and aromatic hydrocarbons, halogenated aliphatic,
cycloaliphatic, and aromatic hydrocarbons, higher aliphatic esters and
ketones, di-n-amyl ether
Low-density (LDPE)(LLDPE)—as high density, but temperatures 20 to
30°C lower depending on the degree of branching
CPE Polyethylene, chlorinated, 40 % tetrahydronaphthalene, toluene, xylene, tetrachloroethane,
Cl (at elevated temperature) chlorobenzene, cyclohexanone
CPE Polyethylene, chlorinated, 60 % Cl tetrahydronaphthalene, benzene, toluene, methylene chloride,
chloroform, dioxane, tetrahydrofuran, cyclohexanone, acetone/carbon
disulfide at 1:1
PEO Poly(ethylene oxide) benzene, toluene, methylene chloride, chloroform, carbon
tetrachloride, n-butanol, methyl ethyl ketone, cyclohexanone, water
PET Poly(ethylene terephthalate) chloral hydrate, phenol, phenol/tetrachloroethane at 1:1 by volume,
phenol/2,4,6-trichlorophenol at 10:7 by volume, chlorophenol,
hexafluoroisopropanol, nitrobenzene, dimethyl sulfoxide (hot),
halogenated aliphatic carboxylic acids, m-cresol at 100°C
PETG Poly(ethylene terephthalate), glycol comonomer see Poly(ethylene terephthalate)
PI Polyimide N,N-dimethylformamide, N,N-dimethylacetamide, N-methyl pyrrolidone
at 85°C
PIB Polyisobutylene tetrahydrofuran, toluene
Polyisoprene tetrahydrofuran, toluene
PMCA Poly(methyl-a-chloroacrylate) aromatic hydrocarbons, chlorinated hydrocarbons, tetrahydrofuran,
esters, ketones
PMMA Poly(methyl methacrylate) benzene, toluene, xylene, methylene chloride, chloroform, ethylene
chloride, chlorobenzene, isobutanol (hot), cyclohexanol (hot),
B-ethoxyethanol, dioxane, methyl ethyl ketone, diisopropyl ketone,
cyclohexanone, acetic acid, isobutyric acid, methyl formate, ethyl
acetate, cyclohexyl acetate, isobutyl propionate, butyl lactate, ethanol/
water, ethanol/carbon tetrachloride, isopropanol/methyl ethyl ketone at
1:1 above 25°C, formic acid, nitroethane, methylene chloride,
hexafluoroisopropanol
PMP Poly(4-methylpentene-1), isotactic see Poly(ethylene)
PCTFE Polymonochlorotrifluoroethylene cyclohexane (235°C), benzene (200°C), toluene (142°C), p-xylene
(140°C), 1,1,1-trichloroethane (120°C), carbon tetrachloride (114°C),
1,2,3-trifluoropentachloropropane, 1,1,2,2-tetrafluoro-3,3,4,4-
tetrachlorocyclobutane, 1,2-dichlorotrifluorobenzene, 2,5-
dinitrotrifluorobenzene (130°C), mesitylene (140°C),
hexamethyltrisphosphoramide
POM Polyoxymethylene, polyacetal (at elevated benzyl alcohol, phenol, chlorophenols, aniline, formamide, N,N-
temperatures) dimethylformamide, malodinitrile, g-butyrolactone, ethylene carbonate,
bromobenzene, diphenyl ether, benzyl benzoate
PPE Poly(phenylene ether) 1,2,4-trichlorobenzene at 135°C

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D5226 − 16
TABLE A1.1 Continued
Abbreviation Polymer Solvents
PP Polypropylene Atactic—hydrocarbons and chlorinated hydrocarbons at room
temperature, isoamyl acetate, diethyl ether
Isotactic (at temperatures above 135°C)—trichlorobenzene, xylenes,
decahydronaphthalene
PPO Poly(propylene oxide) benzene, toluene, carbon tetrachloride, methanol (hot), ethanol,
tetrahydrofuran, dioxane, acetone, methyl ethyl ketone
PSU Polysulfone methylene chloride, N,N-dimethylformamide, dimethyl sulfoxide
PS Polystyrene cyclohexane (above 35°C), cyclohexane/acetone, methylcyclohexane/
acetone, decahydronaphthalene/dimethyl oxalate, benzene, toluene,
ethylbenzene, styrene, lower chlorinated aliphatic hydrocarbons,
phenol/acetone, tetrahydrofuran, dimethyltetrahydrofuran, dioxane,
methyl ethyl ketone, diisopropyl ketone, cyclohexanone, glycol formal,
ethyl acetate, butyl acetate, methyl-, ethyl-, n-butyl phthalate,
1-nitropropane, carbon disulfide, tributyl phosphate, phosphorus
trichloride
PTFE Polytetrafluoroethylene perfluorokerosene (350°C)
PUR Polyurethane phenol, m-cresol, formic acid, sulfuric acid, tetrahydrofuran,
chloroform, N,N-dimethylformamide
PVK Polyvinylcarbazole benzene, toluene, xylene, methylene chloride, chloroform,
tetrachloroethane, chlorobenzene, tetrahydrofuran, dioxane,
cyclohexanone, benzyl acetate, conc. nitric acid, conc. sulfuric acid
PVP Polyvinylpyrrolidone water
PVAC Poly(vinyl acetate) benzene, toluene, chloroform, carbon tetrachloride/ethanol,
dichloroethylene/ethanol at 20:80, chlorobenzene, methanol, ethanol/
water, n-butanol/water, allyl alcohol, 2,4-dimethyl-3-pentanol, benzyl
alcohol, tetrahydrofurfuryl alcohol, tetrahydrofuran,
dimethyltetrahydrofuran, dioxane, glycol ethers, glycol ether esters,
acetone, methyl ethyl ketone, acetic acid, lower aliphatic esters, vinyl
acetate, acetals, acetonitrile, nitromethane, N,N-dimethylformamide,
dimethyl sulfoxide Syndiotactic—chloroform, chlorobenzene
PVAL Poly(vinyl alcohol) glycols (hot), glycerol (hot), piperazine, methylenediamine, formamide,
N,N-dimethylformamide, dimethyl sulfoxide (hot), water,
hexamethyltrisphosphoramide, tetrahydrofuran
PVB Poly(vinyl butural) Acetalization 70 %—alcohols, cyclohexanone, ethyl acetate, ethyl
glycol acetate Acetalization 77 %—methylene chloride, alcohols,
acetone, methyl ethyl ketone cyclohexanone, lower esters
Acetalization 83 %—methylene chloride, alcohols, ketones, lower
esters
PVC Poly(vinyl chloride) High molecular weight—tetrahydrofuran, acetone/carbon disulfide,
methyl ethyl ketone, cyclopentanone, cyclohexanone, N,N-
dimethylformamide, nitrobenzene, dimethyl sulfoxide
Low molecular weight—toluene, xylene, methylene chloride, ethylene
chloride, perchloroethylene/acetone, 1,2-dichlorobenzene, dioxane,
acetone/carbon disulfide, cyclopentanone, cyclohexanone, diisopropyl
ketone, mesityl oxide, isophorone, N,N-dimethylformamide,
nitrobenzene, hexamethyltrisphosphoramide, tricresyl phosphate
Chlorinated, 63 %—aromatic hydrocarbons, chloroform,
chlorobenzene, tetrahydrofuran, dioxane, acetone, cyclohexanone,
butyl acetate, nitrobenzene, N,N-dimethylformamide, dimethyl
sulfoxide
PVCA Poly(vinyl chloride-acetate) see Poly(vinyl chloride)
PVF Poly(vinyl fluoride) cyclohexanone (hot), N,N-dimethylformamide, dinitrile, N,N-
dimethylacetamide (hot), dimethyl sulfoxide (hot)
Chlorinated, 30 %—N,N-dimethylformamide
Chlorinated, 60 %—carbon tetrachloride
PVFM Poly(vinyl formed) benzene/alcohol at 70:30, toluene, methylene chloride, chloroform,
carbon tetrachloride/alcohol at 70:30, dichloroethylene,
dichloroethylene/diacetone alcohol at 50:50, 2-chloroethanol, benzyl
alcohol, furfural, tetrahydrofuran, dioxane, cyclohexanone, formic acid,
acetic acid, N,N-dimethylformamide
PVDC Poly(vinylidene chloride) tetrahydrofuran (hot), tetrahydronaphthalene (hot), trichloroethane,
pentachloroethane, 1,2-dichlorobenzene, trichlorobenzene,
tetrahydrofurfuryl alcohol, dioxane, cyclohexane, N,N-dimethylamide,
butyl acetate, N,N-dimethylformamide, N-methylpyrrolidone,
benzonitrile, tetrahydrofuran, cyclohexanone
PVDF Poly(vinylidene fluoride) cyclohexanone, g-butyrolactone, ethylene carbonate, propylene
carbonate, N,N-dimethylacetamide, N-methylpyrrolidone, dimethyl
sulfoxide
SI Silicone plastics tetrahydrofuran, chlorinated hydrocarbons, toluene
SAN Styrene-acrylonitrile N,N-dimethylformamide (if high acrylonitrile), also see Polystyrene
SB Styrene-butadiene chloroform, toluene
SMS Styrene/a-methylstyrene see Polystyrene
SRP Styrene-rubber plastics toluene
UP Unsaturated polyester tetrahydrofuran
UF Urea-formaldehyde hexafluoro-2-propanol, N,N-dimethylformamide, N,N-
dimethylacetamide at 85°C

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ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

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Designation: D5227 − 13

Standard Test Method for


Measurement of Hexane Extractable Content of Polyolefins1
This standard is issued under the fixed designation D5227; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* Determine the Precision of a Test Method


1.1 This test method describes an extraction/gravimetric 2.2 Federal Document:3
procedure for determination of the amount of hexane soluble 21 CFR 177.1520
low molecular weight material present in polyethylene,
3. Terminology
polypropylene, ethylene-propylene copolymers, and ethylene-
vinyl acetate copolymers. This test method is a modification of 3.1 The definitions given in Terminology D883, D1600, and
the Food and Drug Administration (FDA) procedure for E131 are applicable to this test method.
determining hexane extractables of polyolefins. This test 3.2 Abbreviations:
method is based upon the presumption that the weight of the 3.2.1 EVA—ethylene-vinyl acetate copolymer.
residue extract present in the solvent is equal to the amount
3.2.2 LDPE—low-density polyethylene.
extracted from the film sample and could therefore be quanti-
fied by measuring the weight loss of the extracted film, 3.2.3 HDPE—high-density polyethylene.
eliminating the complex and time-consuming evaporation 3.2.4 LLDPE—linear low-density polyethylene.
process described in 21 CFR 177.1520. 3.2.5 FDA—Food and Drug Administration.
1.2 This standard does not purport to address all of the 3.2.6 PP—polypropylene.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 Film samples are extracted with hexane for 2 h at 49.5
bility of regulatory limitations prior to use.
6 0.5°C, dried, and weighed.
1.3 The values stated in SI units are to be regarded as the
standard. Units used in 21 CFR 177.1520 are also used in this 4.2 The loss in weight of the film is presumed to be equal to
test method. Units are in conformance with Federal Code 21 the extractable content determined by solvent evaporation in
CFR 177.1520, from which this test method is derived. the FDA protocol.
NOTE 1—There is no known ISO equivalent to this standard. 5. Significance and Use
2. Referenced Documents 5.1 FDA requirements for maximum extractables are speci-
2 fied for resin and uses. This test method provides a means to
2.1 ASTM Standards: determine the amount of hexane-soluble low molecular weight
D883 Terminology Relating to Plastics material present in polyolefins. It is applicable to resins
D1239 Test Method for Resistance of Plastic Films to containing greater than 0.20 % extractables.
Extraction by Chemicals
D1600 Terminology for Abbreviated Terms Relating to Plas- 6. Apparatus
tics
6.1 Water Bath, maintained at 49.5 6 0.5°C.
E131 Terminology Relating to Molecular Spectroscopy
E691 Practice for Conducting an Interlaboratory Study to 6.2 Resin Kettle, 1500-mL.
6.3 Kettle Head, 3-neck, with one 45/50 and two 24/40
female joints, and appropriate stoppers.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. 6.4 Clamp.
Current edition approved June 1, 2013. Published July 2013. Originally approved
in 1992. Last previous edition approved in 2008 as D5227 - 01(2008)ε1. DOI:
6.5 Allihn Condenser, Size C, with 45/50 male joint.
10.1520/D5227-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Standards volume information, refer to the standard’s Document Summary page on Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
the ASTM website. www.dodssp.daps.mil.

*A Summary of Changes section appears at the end of this standard


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D5227 − 13
9.4 Using gloves and metal tweezers to avoid sample
contamination, cut 2.7 g of the prepared film sample (4 mil or
less in thickness) into 1-in. squares using clean sharp scissors.
NOTE 4—Care must be exercised when cutting the samples to avoid
ragged edges on the specimen. Small shards of film or contamination
present at initial weighing can easily be lost during the test, adversely
affecting the test results.
9.5 Weigh 2.5 6 0.05 g of film squares and record the initial
film weight to the nearest 0.1 mg. Also record the number of
film pieces.
NOTE 5—Forty or more squares will be obtained depending on the film
thickness. Some laboratories have found that a basket assembly, as shown
in Appendix X1, eliminates the need to count the film pieces before and
after the solvent extraction step.
9.6 Add the film sample to the hexane making sure all
squares become immersed in the solvent. (Use tweezers.)
Replace the kettle head with condenser column. Extract for 2 h.
FIG. 1 Resin Kettle Setup 9.7 After the extraction period:
9.7.1 Filter the contents of the resin kettle through the fritted
6.6 Plastic Sleeves, tetrafluoroethylene (TFE), to fit Allihn porcelain funnel.
condenser 45/50 male joint. 9.7.2 Transfer the film squares, using tweezers, to a 200-mL
Berzelius beaker and recount the film pieces to verify that none
6.7 Vacuum Oven, capable of maintaining 80 6 5°C and a were lost during transfer.
minimum of 25-in. Hg pressure. 9.7.3 Cover the beaker with a watchglass and place it in a
6.8 Magnetic Stirring Bar, egg-shaped, TFE-coated, 11⁄2 by vacuum oven at 80 6 5°C for 2 h.
⁄ in.
58 9.7.4 After 2 h, remove the covered beaker from the vacuum
6.9 Submersible Magnetic Stirring Motor, with power sup- oven and place it in a desiccator to cool to room temperature
ply. (estimated 1 h).
6.10 Analytical Balance, capable of weighing to 0.1 mg. 9.8 Remove the film squares using tweezers and weigh them
to the nearest 0.1 mg.
7. Reagents and Materials 9.9 Repeat 9.7.3 and 9.7.4 until a constant weight is
7.1 n-Hexane, aromatic free (<1 mg/L), minimum 85 % obtained.
n-Hexane-reagent grade or equivalent. The solvent must be
free of aromatic compounds that would significantly increase 10. Calculation
the solubility of the resin. The solvent grade specified repre- 10.1 Calculate the weight percent of extractables present in
sents the minimum required purity. the original sample as follows:
8. Materials ~ A 2 B ! 3 100 3 0.935
hexane extractables, % 5 (1)
A
8.1 Blown Film, compression molded films, or cast films are
suitable for testing. where:
8.2 Film, approximately 2.5 g, with a thickness not exceed- A = weight of original sample film, g,
B = weight of the film after extraction, g, and
ing 4 mil is required for a single determination.
0.935 = correlation factor to eliminate the bias between the
9. Procedure original FDA technique and this alternate test
method.
9.1 Assemble the resin kettle setup with glass stopper,
clamp, and magnetic stirring bar. (See Fig. 1.) 11. Report
9.2 Add 1000 mL of n-Hexane to the kettle assembly. 11.1 Report the hexane extractables to the nearest 0.01 % as
9.3 Stopper the kettle and clamp the assembly into the water calculated in 10.1.
bath set at 49.5 6 0.5°C.
12. Precision and Bias4
NOTE 2—Temperature is a critical factor in this analysis and must not
vary more than 1°C. If the temperature exceeds these limits, the test must 12.1 Hexane Extractable Content of Polyolefins:
be discontinued and restarted. The FDA protocol also states the tempera- 12.1.1 Table 1 is based on a round robin conducted in 1990
ture of the contents must be brought to 49.5 6 0.5°C within 20 to 25 min. in accordance with Practice E691, involving five materials
NOTE 3—The level of water in the bath must be kept at least 2 cm above
the level of the solvent in the kettle to ensure the temperature equilibrium.
Position the kettle so that the center bottle of the kettle is sitting on a 4
Supporting data are available from ASTM Headquarters. Request RR:D20-
submersible stirrer. Start stirring and allow the hexane to heat for 1 h. 1173.

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D5227 − 13
TABLE 1 Hexane Extractable Content of Polyolefins, Weight 12.1.2 Concept of r and R—If Sr and SR have been
Material Average Sr SR r R calculated from a large enough body of data, and for test results
HDPE 0.26 0.03 0.05 0.09 0.15 that were averages from testing five specimens.
LLDPE 0.88 0.11 0.16 0.31 0.46 12.1.2.1 Repeatability Limit, r—(Comparing two test results
LDPE 1.74 0.08 0.15 0.21 0.42
EVA 3.54 0.28 0.33 0.78 0.93 for the same material, obtained by the same operator using the
PP 3.80 0.29 0.35 0.81 0.98 same equipment on the same day.) The two test results should
be judged not equivalent if they differ by more than the r value
for that material.
12.1.2.2 Reproducibility Limit, R—(Comparing two test re-
sults for the same material, obtained by different operators
tested by ten laboratories. The materials were supplied by one using different equipment in different laboratories.) The two
laboratory. Each test result was an individual determination. test results should be judged not equivalent if they differ by
Each laboratory obtained six test results for each of the five more than the R value for that material.
materials. Each laboratory obtained two test results for each 12.1.2.3 Any judgment in accordance with 12.1.2.1 or
material tested each day for three days. 12.1.2.2 would have an approximate 95 % (0.95) probability of
NOTE 6—Caution: The following explanations of r and R (12.1.2 – being correct.
12.1.2.3) are only intended to present a meaningful way of considering the 12.1.3 Bias—There are no recognized standards by which to
approximate precision of this test method. The data in Table 1 should not estimate bias of this test method.
be rigorously applied to acceptance or rejection of material, as those data
are specific to the round robin and may not be representative of other lots, 13. Keywords
conditions, materials, or laboratories. Users of this test method should
apply the principles outlined in Practice E691 to generate data specific to 13.1 ethylene-propylene copolymers; ethylene-vinyl acetate
their laboratory and materials, or between specific laboratories. The copolymers; extractables; FDA; hexane; plastics; polyethyl-
principles of 12.1.2 – 12.1.2.3 would then be valid for such data. ene; solvent extraction

APPENDIX

(Nonmandatory Information)

X1. BASKET ASSEMBLY FOR n -HEXANE EXTRACTABLES

X1.1 If one uses the basket assembly shown in Fig. X1.1, X1.1.2 Remove the excess solvent by briefly blowing the
the following steps should be performed after the 2-h hexane basket with a stream of nitrogen or dry air.
extraction (9.6) Also, the sample and basket must be weighed X1.1.3 Place the basket in a vacuum oven for 2 h at 806
together and recorded before starting the extraction: 5°C, then cool to ambient temperature in a desiccator (esti-
X1.1.1 Rinse the basket and contents by immersing several mated 1 h).
times in fresh n-hexane contained in a small beaker, allowing X1.1.4 Reweigh the basket and its contents to the nearest
the basket to drain between rinsings. 0.1 mg.

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D5227 − 13

FIG. X1.1 Basket for n-Hexane Extractables1

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5227 –
01(2008)ε1) that may impact the use of this standard. (June 1, 2013)

(1) Removed permissive language. (3) Revised X1.1.


(2) Removed materials manufacturers information.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
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Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5260 − 16

Standard Classification for


Chemical Resistance of Poly(Vinyl Chloride) (PVC)
Homopolymer and Copolymer Compounds and Chlorinated
Poly(Vinyl Chloride) (CPVC) Compounds1
This standard is issued under the fixed designation D5260; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D1784 Specification for Rigid Poly(Vinyl Chloride) (PVC)


1.1 This classification covers the method for determining Compounds and Chlorinated Poly(Vinyl Chloride)
and classifying the resistance of poly(vinyl chloride) (PVC) (CPVC) Compounds
homopolymer and copolymer compounds, and chlorinated D4216 Specification for Rigid Poly(Vinyl Chloride) (PVC)
poly(vinyl chloride) (CPVC) compounds in chemicals by and Related PVC and Chlorinated Poly(Vinyl Chloride)
simple immersion testing of unstressed specimens. (CPVC) Building Products Compounds
D4396 Specification for Rigid Poly(Vinyl Chloride) (PVC)
1.2 This classification is applicable to any PVC or CPVC
and Chlorinated Poly(Vinyl Chloride) (CPVC) Com-
compound as defined in Specifications D1784, D4216, D4396,
pounds for Plastic Pipe and Fittings Used in Nonpressure
or D4551.
Applications
1.3 The values stated in SI units are to be regarded as D4551 Specification for Poly(Vinyl Chloride) (PVC) Plastic
standard. Flexible Concealed Water-Containment Membrane
1.4 The text of this standard references notes and footnotes
which provide explanatory material. These notes and footnotes 3. Terminology
(excluding those in tables and figures) shall not be considered
3.1 Definitions and Abbreviations:
as requirements of this standard.
3.1.1 Definitions are in accordance with Terminology D883
1.5 This standard does not purport to address all of the and abbreviations with Terminology D1600 unless otherwise
safety concerns, if any, associated with its use. It is the
indicated.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use.
NOTE 1—There are no ISO standards covering the subject matter of this
4.1 Reference this chemical resistance classification for any
classification. PVC/CPVC material compound specification wherein a level
of resistance to specific chemicals is required for satisfactory
2. Referenced Documents product performance.
2.1 ASTM Standards:2 4.2 Listing of a chemical in the annex does not imply
D543 Practices for Evaluating the Resistance of Plastics to PVC/CPVC compatibility or resistance to the chemical. Some
Chemical Reagents of the chemicals listed could be deleterious to a specific
D883 Terminology Relating to Plastics compound, causing radical changes in the physical properties.
D1600 Terminology for Abbreviated Terms Relating to Plas- Resistance to these chemicals is not intended to be a practical
tics requirement in a specification.

1
4.3 For resistance to mixtures of chemicals, it is suggested
This classification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic
that the blend be tested rather than accepting the resistance of
Materials. the individual chemicals because of a possible solvency
Current edition approved May 1, 2016. Published May 2016. Originally enhancement of the combined chemicals.
approved in 1992. Last previous edition approved in 2010 as D5260 - 04(2010).
DOI: 10.1520/D5260-16. 4.4 The specimens tested in this classification are un-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or stressed. When service conditions include stress or other
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on factors, or both, test chemical resistance of the PVC/CPVC
the ASTM website. compound under actual service conditions.

*A Summary of Changes section appears at the end of this standard


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D5260 − 16
5. Basis of Classification 8.1.1 The test chemical is designated from the alphanumeri-
5.1 The chemical resistance of a PVC or CPVC compound cal list of chemicals in the annex. This alphanumeric designa-
is composed of the cell classifications specified from Table 1. tion is the first three digits of the chemical resistance cell.
For example, the resistance of PVC to 25 % acetic acid at 8.1.2 The concentration of the chemical from row two of
ambient temperature would be written as a cell classification of Table 1 is designated as the fourth digit of the chemical
A05231: resistance cell.
Class
8.1.3 The test temperature from row three of Table 1 is
Chemical (acetic acid from annex) A05 designated as the fifth number of the chemical resistance cell.
Concentration of 25 % 2 8.1.4 The resistance of a compound from row four of Table
Temperature of 23°C 3
Resistance 1
1 is designated as the sixth number of the chemical resistance
cell. Grade a compound for its resistance to the testing of 8.1.1
NOTE 2—The cell-type format provides the means of classifying – 8.1.3 as follows:
chemical resistance. This type of format is subject to possible misappli-
cation in classifying a chemical resistance that is unobtainable with Resistant Marginally Non-
commercially available materials. Consult the manufacturer regarding this Resistant Resistant
classification. Linear Swelling 0% <5 % >5 %
Change in Weight <1 % <10 % >10 %
Change in Shore Hardness no change <5 units >5 units
6. Performance Requirements
6.1 The chemical resistance shall be for a compound that 9. Inspection
meets the physical property and processing requirements of the
9.1 Inspection of the product shall be agreed upon between
application.
the purchaser and the supplier as part of the purchase contract.
7. Sampling
7.1 A batch or lot shall be considered as a unit of manufac- 10. Rejection and Rehearing
ture and is permitted to consist of a blend of two or more 10.1 Product that fails to conform to the requirements of this
production runs of material. classification shall not be certified as meeting the requirements
7.2 Sample using a statistically acceptable procedure. of this classification. Report rejection to the producer or
supplier promptly and in writing. In case of dissatisfaction with
8. Test Methods the results of the test, the producer or supplier is permitted to
8.1 Determine the chemical resistance of a compound fol- make claim for a rehearing.
lowing the procedure of Test Method D543 except the expo-
sure period shall be for 30 days. Note the chemical, 11. Keywords
concentration, test temperature, and resistance in accordance 11.1 chemical resistance; chlorinated poly(vinyl chloride)
with 8.1.1 – 8.1.4. This data is compiled in Table 1 and polymers; poly(vinyl chloride) copolymers; poly(vinyl chlo-
comprises the six digits of the chemical resistance cell. ride) polymers
TABLE 1 Chemical Resistance of a Compound
Designation Cell Limits
Property and Unit
Order Number 0 1 2 3 4 5 6 7
1 to 3 chemical unspecified use number of chemical from annex
4 concentration, % unspecified 0 to 19 20 to 39 40 to 59 60 to 79 80 to 99 100
5 temperature,° C unspecified <0 0 to 19 20 to 39 40 to 59 60 to 79 80 to 100 >100
6 resistance unspecified R MR NR

ANNEX

(Mandatory Information)

A1. ALPHANUMERICAL LIST OF CHEMICALS

Acetaldehyde A01 Ammonia Biflouride A19


Acetamide A02 Ammonium Carbonate A20
Acetate Solvent A03 Ammonium Casenite A21
Acetic Acid, Glacial A04 Ammonium Chloride A22
Acetic Acid A05 Ammonium Hydroxide A23
Acetic Anhydride A06 Ammonium Nitrate A24
Acetone A07 Ammonium Oxalate A25

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Acetylene A08 Ammonium Persulfate A26


Acrylonitrile A09 Ammonium Phosphate, Dibasic A27
Aluminum Chloride A10 Ammonium Phosphate, Monobasic A28
Aluminum Fluoride A11 Ammonium Phosphate, Tribasic A29
Aluminum Hydroxide A12 Ammonium Sulfate A30
Aluminum Potassium Sulfate A13 Ammonium Thio-Sulfate A31
Aluminum Sulfate A14 Amyl Acetate A32
Amines A15 Amyl Alcohol A33
Ammonia, Anhydrous A16 Amyl Chloride A34
Ammonia, Liquid A17 Aniline A35
Ammonia, Nitrate A18 Aqua Regia (80 % HCl ⁄ 20 % H2 SO4) A36
Arsenic Acid A37

Barium Carbonate B01 Benzyl Alcohol B14


Barium Chloride B02 Borax (Sodium Borate) B15
Barium Cyanide B03 Boric Acid B16
Barium Hydroxide B04 Brewey Slop B17
Barium Nitrate B05 Bromine B18
Barium Sulfate B06 Butadiene B19
Barium Sulfide B07 Butane B20
Beer B08 Butter B21
Beet Sugar Liquids B09 Buttermilk B22
Benzaldehyde B10 Butyl Acetate B23
Benzene B11 Butyl Alcohol B24
Benzoic Acid B12 Butylene B25
Benzol B13 Butyric Acid B26

Calcium Bisulfide C01 Chlorobenzene (mono) C20


Calcium Carbonate C02 Chloroform C21
Calcium Chloride C03 Chlorosulfuric Acid C22
Calcium Hydroxide C04 Chlorox (bleach) C23
Calcium Hypochlorite C05 Chocolate Syrup C24
Calcium Sulfate C06 Chromic Acid C25
Calgon C07 Cider C26
Cane Juice C08 Citric Acid C27
Carbolic Acid......(See Phenol)...... Coffee C28
Carbon Bisulfide C09 Copper Chloride C29
Carbon Dioxide C10 Copper Cyanide C30
Carbon Disulfide C11 Copper Fluorborate C31
Carbon Monoxide C12 Copper Nitrate C32
Carbon Tetrachloride C13 Copper Sulfate C33
Carbonated Water C14 Cream C34
Carbonic Acid C15 Cresols C35
Catsup C16 Cresylic Acid C36
Chloroacetic Acid C17 Cyclohexane C37
Chlorinated Glue C18 Cyanic Acid C38
Chlorine, Anhydrous Liquid C19

Detergents D01 Diethylene Glycol D04


Diethylene D02 Diphenyl Oxide D05
Diacetone Alcohol D03 Dyes D06

Epsom Salts...(See Magnesium Sulfate) Ethyl Chloride E06


Ethane E01 Ethyl Sulfate E07
Ethanolamine E02 Ethylene Chloride E08
Ether E03 Ethylene Dichloride E09
Ethyl Acetate E04 Ethylene Glycol E10
Ethyl Alcohol E05 Ethylene Oxide E11

Fatty Acids F01 Freon 22 F13


Ferric Chloride F02 Freon 113 F14
Ferric Nitrate F03 Freon T.F. F15
Ferric Sulfate F04 Fruit Juice F16
Ferrous Chloride F05 Fuel Oil #1 F17
Ferrous Sulfate F06 Fuel Oil #2 F18
Fluorboric Acid F07 Fuel Oil #3 F19
Fluosilicic Acid F08 Fuel Oil #5A F20
Formaldehyde F09 Fuel Oil #5B F21

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Formic Acid F10 Fuel Oil #6 F22


Freon 11 F11 Furan Resin F23
Freon 12 (wet) F12 Furfural F24

Gasoline (unleaded) G01 Glycerine G06


Gasoline (unleaded premium) G02 Glycolic Acid G07
Gelatin G03 Gold Monocyanide G08
Glucose G04 Grape Juice G09
Glue, P.V.A. G05 Grease G10

Heptane H01 Hydrochloric Acid H09


Hexane H02 Hydrocyanic Acid H10
Hexyl Alcohol H03 Hydrofluoric Acid H11
Honey H04 Hydrofluosilicic Acid H12
Hydraulic Oil (Petroleum) H05 Hydrogen Peroxide H13
Hydraulic Oil (Synthetic) H06 Hydrogen Sulfide, Aqueous H14
Hydrazine H07 Hydroxyacetic Acid H15
Hydrobromic Acid H08

Ink I01 Isopropyl Acetate I05


Iodine I02 Isopropyl Ether I06
Isobutyl Alcohol I03 Isotane I07
Isopropyl Alcohol I04

JP 3 Jet Fuel J01 JP 5 Jet Fuel J03


JP 4 Jet Fuel J02

Kerosene K01

Lacquers L01 Lead Sulfamate L06


Lactic Acid L02 Ligroin L07
Lard L03 Lime L08
Latex L04 Lubricants L09
Lead Acetate L05

Magnesium Carbonate M01 Methyl Acrylate M17


Magnesium Chloride M02 Methyl Alcohol M18
Magnesium Hydroxide M03 Methyl Bromide M19
Magnesium Nitrate M04 Methyl Butyl Ketone M20
Magnesium Oxide M05 Methyl Cellosolve M21
Magnesium Sulfate M06 Methyl Chloride M22
Maleic Acid M07 Methyl Dichloride M23
Maleic Anhydride M08 Methyl Ethyl Ketone M24
Mash M09 Methyl Isobutyl Ketone M25
Mayonnaise M10 Methyl Isopropyl Ketone M26
Melamine M11 Methyl Methacrylate M27
Mercuric Chloride M12 Methylamine M28
Mercuric Cyanide M13 Methylene Chloride M29
Mercury M14 Milk M30
Methyl Acetate M15 Mineral Oil M31
Methyl Acetone M16 Molasses M32
Mustard M33

Naptha N01 Nickel Sulfate N04


Napthalene N02 Nitric Acid N05
Nickel Chloride N03 Nitrobenzene N06

Oils: Oils:
Anise O01 Olive O15
Bay O02 Orange O16
Bone O03 Palm O17
Castor O04 Peanut O18

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Cinnamon O05 Peppermint O19


Citric O06 Pine O20
Clove O07 Rape Seed O21
Coconut O08 Rosin O22
Cod Liver O09 Sesame Seed O23
Corn O10 Soybean O24
Cotton Seed O11 Sperm O25
Ginger O12 Oleic Acid O26
Lemon O13 Oleum O27
Linseed O14 Oxalic Acid O28

Paraffin P01 Potash P23


Pentane P02 Potassium Bicarbonate P24
Perchloroethylene P03 Potassium Bromide P25
Petrolatum P04 Potassium Carbonate P26
Phenol P05 Potassium Chlorate P27
Phosphoric Acid P06 Potassium Chloride P28
Photographic Developer P07 Potassium Chromate P29
Plating Solution:
Antimony P08 Potassium Cyanide P30
Arsenic P09 Potassium Dichromate P31
Brass P10 Potassium Hydroxide P32
Bronze P11 Potassium Nitrate P33
Cadmium P12 Potassium Permanganate P34
Chrome P13 Potassium Sulfate P35
Copper P14 Propane (liquified) P36
Gold P15 Propyl Alcohol P37
Indium P16 Propylene Glycol P38
Iron P17 Pyridene P39
Lead P18 Pyrogallic Acid P40
Nickel P19
Silver P20
Tin P21
Zinc P22

Rosins R01 Rust Inhibitors R03


Rum R02

Salad Dressing S01 Sodium Polyphosphate, monobasic S26


Sea Water S02 Sodium Polyphosphate, dibasic S27
Shellac (bleached) S03 Sodium Polyphosphate, tribasic S28
Shellac (orange) S04 Sodium Silicate S29
Silicone S05 Sodium Sulfate S30
Silver Bromide S06 Sodium Sulfide S31
Silver Nitrate S07 Sodium Tetraborate S32
Soap Solutions S08 Sodium Thiosulfate S33
Sodium Acetate S09 Sorgum S34
Sodium Aluminate S10 Soy Sauce S35
Sodium Bicarbonate S11 Stannic Chloride S36
Sodium Bisulfate S12 Stannic Fluoborate S37
Sodium Bisulfite S13 Starch S38
Sodium Carbonate S14 Stearic Acid S39
Sodium Chlorate S15 Stoddard Solvent S40
Sodium Chloride S16 Styrene S41
Sodium Chromate S17 Sugar (liquids) S42
Sodium Cyanide S18 Sulfate Liquors S43
Sodium Hydroxide S19 Sulfur Chloride S44
Sodium Hypochlorite S20 Sulfur Dioxide S45
Sodium Metaphosphate S21 Sulfur Trioxide S46
Sodium Metasilicate S22 Sulfuric Acid S47
Sodium Nitrate S23 Sulfurous Acid S48
Sodium Perborate S24 Syrup S49
Sodium Peroxide S25

Tallow T01 Tomato Juice T08


Tannic Acid T02 Trichloroethane T09
Tanning Liquors T03 Trichloroethylene T10
Tartaric Acid T04 Trichloropropane T11
Tetrachloroethane T05 Tricresylphosphate T12
Tetrahydrofuran T06 Triethylamine T13

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Toluene T07 Turpentine T14

Urine U01

Vegetable Juice V01 Vinegar V02

Water, Distilled W01 Whey W06


Water, Fresh W02 Whiskey W07
Water, Mine, Acid W03 Wine W08
Water, Salt W04 White Liquor (pulp mill) W09
Weed Killers W05 White Water (pulp mill) W10

Xylene X01

Zinc Chloride Z01 Zinc Sulfate Z03


Zinc Hydrosulfite Z02

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5260 -
04(2010)) that may impact the use of this standard. (May 1, 2016)

(1) Removed reference to withdrawn standard Specification


D3915.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5272 − 08 (Reapproved 2013)

Standard Practice for


Outdoor Exposure Testing of Photodegradable Plastics1
This standard is issued under the fixed designation D5272; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 3. Terminology
1.1 This practice defines test conditions applicable when 3.1 The terminology given in Terminology E772 and Ter-
Practices D1435 and G7 are employed for the outdoor expo- minology D883 is applicable to this practice.
sure testing of photodegradable plastics.
1.2 This standard does not purport to address all of the 4. Significance and Use
safety concerns, if any, associated with its use. It is the 4.1 When discarded as litter, articles made using photode-
responsibility of the user of this standard to establish appro- gradable plastics are subject to attack by daylight (particularly
priate safety and health practices and determine the applica- solar-ultraviolet radiation), oxygen, heat, and water. The 5°
bility of regulatory limitations prior to use. exposure angle used in this practice represents typical condi-
NOTE 1—There is no known ISO equivalent to this standard.
tions for degradation experienced by litter.
4.2 This practice requires characterization of the duration of
2. Referenced Documents exposure in terms of solar-ultraviolet radiation. Solar-
2.1 ASTM Standards:2 ultraviolet radiation varies considerably as a function of
D882 Test Method for Tensile Properties of Thin Plastic location and time of year. This can cause dramatic differences
Sheeting in the time required to produce a specified level of degradation
D883 Terminology Relating to Plastics in a polymer. Daro4 has shown that when the same lot of
D1435 Practice for Outdoor Weathering of Plastics polyethylene containing an iron-salt prodegradant is exposed at
D3593 Test Method for Molecular Weight Averages/ Distri- various times of the year in a single location, the time required
bution of Certain Polymers by Liquid Size-Exclusion to produce an average of two chain scissions per molecule
Chromatography (Gel Permeation Chromatography GPC) varied by over 130 %. Daro, and Zerlaut and Anderson5 have
Using Universal Calibration (Withdrawn 1993)3 shown that this variability can be significantly reduced when
D3826 Practice for Determining Degradation End Point in total solar or solar-ultraviolet radiation, or both, is used to
Degradable Polyethylene and Polypropylene Using a Ten- characterize the exposure increments.
sile Test 4.3 In addition to variations in level of daylight and solar-
E772 Terminology of Solar Energy Conversion ultraviolet radiation, there are significant differences in
G7 Practice for Atmospheric Environmental Exposure Test- temperature, and moisture stresses between different locations,
ing of Nonmetallic Materials and between different years, or periods within a single year, at
G169 Guide for Application of Basic Statistical Methods to a single location. Because of this variability, results from this
Weathering Tests test cannot be used to predict the absolute rate at which
G183 Practice for Field Use of Pyranometers, Pyrheliom- photodegradable plastics degrade. Results from this test can be
eters and UV Radiometers used to compare relative rates of degradation for materials
exposed at the same time in the same location. Results from
multiple exposures of a common lot of material (during
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and
different seasons over several years) at different sites can be
is the direct responsibility of Subcommittee D20.96 on Environmentally Degradable used to compare the relative rates at which a particular
Plastics and Biobased Products. photodegradable plastic will degrade in each location.
Current edition approved April 1, 2013. Published April 2013. Originally
approved in 1992. Last previous edition approved in 2008 as D5272 - 08. DOI:
10.1520/D5272-08R13.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Daro, A., et al, “Degradation of Polymer Blends IV, Natural Weathering of Low
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Density and Linear Low Density Polyethylene,” European Polymer Journal, Vol 26,
Standards volume information, refer to the standard’s Document Summary page on No. 1, 1990, pp. 47–52.
5
the ASTM website. Zerlaut, G. L., and Anderson, T. A., “Ultraviolet Radiation as a Timing
3
The last approved version of this historical standard is referenced on Technique for Outdoor Weathering of Materials,” Society of Automotive Engineers,
www.astm.org. SAE Technical Paper Number 850348 , 1985.

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NOTE 2—An inherent limitation in solar-radiation measurements is that 60 to 70 % open. Use a noncorroding material for the mounting
they do not reflect the effects of variations in temperature and moisture bars. 6061T6 aluminum or untreated wood are typical materi-
exposure, which often can be as important as solar radiation. The same
solar-ultraviolet radiation increment will not necessarily give the same als used for the mounting bars. Fig. 1 is a top view showing
changes in properties of the test specimen in different exposure sites. typical rack construction.
Results from this practice must be regarded as giving only a general 5.2.2 Exposure Rack B—Unpainted exterior-grade plywood
indication of the degree of degradability and should always be considered
in terms of characteristics of the exposure site as well.
forms the rack surface to which specimens are directly at-
tached. Replace the plywood when there is any evidence of
4.4 Where measurement of total solar-ultraviolet radiation delamination or fiber separation which could produce sharp
is not possible, exposure duration can be determined by the edges and damage exposed specimens. Medium-density over-
number of days, weeks, or months exposed. When this practice
lay (MDO) or high-density overlay (HDO) plywood are
is used, a reference material whose degradation properties have
satisfactory substrates and will require less frequent replace-
been well established must be exposed at the same time as the
ment than plywood with no overlay.
other materials being tested. The reference material used must
be agreed upon by all interested parties. The time to produce a NOTE 4—There is less air circulation around the specimens when Rack
specified level of degradation for each material in this simul- B exposures are used. Degradation rates from exposures using Rack B will
taneous exposure is then compared. It is also a good practice to be somewhat faster than those using Rack A because specimen tempera-
use reference materials when exposure length is determined by tures will be higher. Comparisons between materials should only be made
with exposures conducted at the same time and using the same rack type.
total solar or solar UV radiant exposure.
NOTE 3—A reference material can be a single lot of material which has
5.3 Solar Radiometers:
shown consistent results after a number of exposures. It is not necessary 5.3.1 Ultraviolet Radiometer—Unless otherwise specified,
that the composition or properties of the reference material be character- use a total UV radiometer that measures ultraviolet radiation
ized and certified by a recognized standards agency or group. from 295 to 385 mm. Operate the radiometer in accordance
5. Apparatus with Practice G183. Narrow band radiometers (for example,
with 20 nm bandpass) can also be used if agreed upon by all
5.1 Use exposure racks constructed in accordance with the interested parties. Operate narrow band radiometers in accor-
requirements of Practice G7. Unless otherwise specified, posi- dance with Practice G183.
tion the exposure racks so that specimens face the equator and
NOTE 5—The use of narrow band filter UV radiometers having selective
so that the exposed surfaces are 5° from the horizontal. If other spectral sensitivity may not be sensitive to all variations of solar-
exposure rack orientations are used, they must be reported. ultraviolet radiation. Monitoring at a narrow band (for example, 20 nm)
5.2 Use one of the following rack constructions for expos- may not relate to the total photodegradation of the plastic material, which
is a result of a complex interaction of many factors, including sensitivity
ing photodegradable plastic specimens:
across a broad wavelength region.
5.2.1 Exposure Rack A—Positionable mounting bars used
for attaching specimens shall be arrayed over a regular mesh 6. Sampling
expanded-metal (aluminum or stainless steel) sheet backing.
Use 16–18 gage metal with approximately 0.5-in. openings. It 6.1 Sample using a statistically acceptable procedure agreed
is recommended that the surface area of the expanded metal be upon by interested parties.

FIG. 1 Typical Rack Construction for Exterior Exposures of Photodegradable Plastics

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7. Procedure spectral regions where the plastic material is most sensitive
7.1 Attach the ends of specimens of photodegradable plastic may also be employed to follow exposure increments.
to be exposed to the positionable mounting bars or plywood 7.5 After specimens are exposed for the desired amount of
rack. Films or specimens that are nearly flat can be attached total solar-ultraviolet radiation, measure the specified property
using a pressure sensitive tape with a durable adhesive and or properties. Typical properties measured are molecular
backing. Staples may be used with plywood racks or with weight (in accordance with Test Method D3593) and tensile
wood mounting bars. Specimens with odd shapes can be strength and elongation (in accordance with Test Methods
attached directly to the expanded metal or plywood using D882). For polyolefins, degree of oxidation can be monitored
nonferrous bolts and large washers or by any other suitable using a carbonyl index, which is the ratio of carbonyl infrared
method. Ensure that the test specimens are inscribed or absorbance at approximately 1715 cm−1 to an invariant absor-
otherwise labeled with an identifying number, letter, or symbol. bance characteristic of the polymer (for example, C-H stretch
Expose at least three replicate specimens for each material and at approximately 3000–2840 cm−1). The degradation end point
exposure increment used. of polyolefins can be determined by a tensile test in accordance
NOTE 6—Pressure sensitive tapes with aluminum foil backing and
with Practice D3826. Measure the same properties of an
acrylic pressure sensitive adhesives have been found to be suitable for unexposed specimen of each material being tested. If a
attaching flat films and specimens to the exposure rack. reference material is used, determine its properties and express
7.2 Ensure that the UV radiometer is mounted at an angle of the time to degradation for all other materials as a function of
5° from the horizontal, facing the equator. If specimens are the time to produce a specific degree of degradation in the
exposed at a different angle, mount the UV radiometer at the reference material.
same angle as the specimens. NOTE 7—Guide G169 provides information about using statistical
analysis techniques to compare properties of exposed and unexposed
7.3 Mount the specimens on the exposure rack for the time specimens.
desired to produce the prescribed level of total solar-ultraviolet
radiation. It is recommended that a series of exposure incre- 8. Report
ments be used for each material being tested to determine the 8.1 Report the following information for each material
rate of degradation as a function of total solar or solar- exposed:
ultraviolet radiant energy dose. Table 1 shows monthly and 8.1.1 Complete identification and description (for example,
annual average total solar-ultraviolet radiation incident on 5° dimensions) of material tested.
surfaces in representative humid subtropical and desert cli- 8.1.2 Location of exposure and type of exposure rack used.
mates. 8.1.2.1 Any exposure angle other than 5°.
7.4 If total ultraviolet radiant energy is used to determine 8.1.3 Dates exposure started and completed.
exposure increments, measure the increments using the instru- 8.1.3.1 Total time exposed (expressed in days, weeks, or
mentation in accordance with 5.3.1. Express total solar- months).
ultraviolet exposures in joules per square metre, with data 8.1.4 Solar-ultraviolet radiant exposure:
reported to four significant figures. If agreed on by all 8.1.4.1 If total ultraviolet radiation is used, it shall be
interested parties, the ultraviolet radiant energy in specified expressed in joules per square metre. Record manufacturer and
narrow wavelength intervals (or bands) that closely conform to model of UV radiometer employed, date of last calibration, and
calibrating laboratory.
TABLE 1 Average Monthly Solar-Ultraviolet Radiation (295 to 385 8.1.5 General appearance and results of tests used to char-
nm) on a 5° SurfaceA acterize the properties on unexposed samples of each material
NOTE 1—The climate data for Miami also meets the criteria for a
being exposed.
tropical summer rain climate given in the Koppen Climate Classification 8.1.6 General appearance and results of tests used to char-
System. acterize the properties of specimens from each exposure
Average Solar-Ultraviolet Radiation (MJ/m2, 295–385 nm) increment. Report the average and standard deviation from
Month Subtropical Climate Desert Climate each test used to measure properties of replicate specimens.
Miami, FL (26°N latitude) Phoenix, AZ (34°N latitude) 8.1.7 Complete description or reference to characterization
January 19.6 16.6 tests used to evaluate material properties.
February 21.6 19.5
March 28.4 29.0
April 32.2 36.1
9. Precision and Bias
May 33.3 41.1 9.1 It is not practicable to specify the precision of the
June 28.6 41.7
July 29.8 40.3 procedure in this practice because it is dependent upon the
August 27.6 37.7 ASTM test methods used to determine the specific properties
September 24.7 32.1 being measured. The precision and bias for the individual test
October 23.5 25.7
November 18.7 18.0 methods can be used in the analysis of data from exposures
December 17.5 15.3 used to assess the differences in materials.
Annual 305.5 352.5
A
9.2 Because of the variability in solar radiation,
Data in this table are the averages for monthly total solar UV radiation data
reported from 1985 to 2005. temperature, and moisture levels between sites and between
different times at the same site, results from this practice

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should only be used to compare relative rates of degradation
for materials exposed at the same time in the same location
using the same exposure rack construction.
10. Keywords
10.1 aging; degradable plastic; exterior exposure; outdoor
exposure; photodegradation; ultraviolet radiation; weathering

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

Copyright by ASTM Int'l (all rights reserved); Sat Jun 20 15:20:10 EDT 2020
4
Downloaded/printed by
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5279 − 13

Standard Test Method for


Plastics: Dynamic Mechanical Properties: In Torsion1
This standard is issued under the fixed designation D5279; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This test method covers the use of dynamic mechanical 2.1 ASTM Standards:2
instrumentation for gathering and reporting the viscoelastic D618 Practice for Conditioning Plastics for Testing
properties of thermoplastic and thermosetting resins and com- D4065 Practice for Plastics: Dynamic Mechanical Proper-
posite systems in the form of rectangular specimens molded ties: Determination and Report of Procedures
directly or cut from sheets, plates, or molded shapes. The D4092 Terminology for Plastics: Dynamic Mechanical
torsional data generated may be used to identify the thermo- Properties
mechanical properties of a plastics material or composition.
3. Terminology
1.2 This test method is intended to provide means for
3.1 For definitions applicable to this test method, refer to
determining the torsional modulus of plastics as a function of
Terminology D4092.
temperature using nonresonant forced-vibration techniques, as
outlined in Practice D4065. Plots of the elastic (storage), loss 4. Summary of Test Method3
(viscous), and complex moduli and tan delta, as a function of
frequency, time, or temperature are indicative of significant 4.1 This test method covers the determination of the shear
transitions in the thermomechanical performance of the poly- modulus of plastics using dynamic mechanical techniques. A
meric material system. test specimen of rectangular cross section is tested in dynamic
torsion. The specimen is gripped longitudinally between two
1.3 This test method is valid for a wide range of frequencies, clamps. The specimen of known geometry is placed in me-
typically from 0.01 to 100 Hz. chanical torsional displacement at either a fixed frequency, or
1.4 Apparent discrepancies may arise in results obtained variable frequencies at either isothermal conditions, or with a
under differing experimental conditions. These apparent differ- linear temperature increase. The elastic or loss modulus, or
ences from results observed in another study can usually be both, of the polymeric material system are measured in torsion.
reconciled without changing the observed data by reporting in 5. Significance and Use
full (as described in this test method) the conditions under
which the data were obtained. 5.1 This test method provides a simple means of character-
izing the thermomechanical behavior of plastics materials
1.5 Test data obtained by this test method are relevant and using very small amounts of material. The data obtained may
appropriate for use in engineering design. be used for quality control, research and development, and
1.6 The values stated in SI units are to be regarded as establishment of optimum processing conditions.
standard. 5.2 Dynamic mechanical testing provides a sensitive
1.7 This standard does not purport to address all of the method for determining thermomechanical characteristics by
safety concerns, if any, associated with its use. It is the measuring the elastic and loss moduli as a function of
responsibility of the user of this standard to establish appro- frequency, temperature, or time. Plots of moduli and tan delta
priate safety and health practices and determine the applica- of a material versus temperature provide graphical representa-
bility of regulatory limitations prior to use. tions indicative of functional properties, effectiveness of cure
(thermosetting resin system), and damping behavior under
NOTE 1—This test method is equivalent to ISO 6721, Part 7. specified conditions.

2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
and is the direct responsibility of Subcommittee D20.10 on Mechanical Properties. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Sept. 1, 2013. Published Septmeber 2013. Originally the ASTM website.
3
approved in 1992. Last previous edition approved in 2008 as D5279 - 08. DOI: The particular method for measurement of the elastic and loss moduli and tan
10.1520/D5279-13. delta depends upon the individual instrument’s operating principles.

*A Summary of Changes section appears at the end of this standard


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D5279 − 13
5.3 This test method can be used to assess ramps), cooling (in steps or ramps), maintaining a constant
5.3.1 The modulus as a function of temperature, specimen environment, or a combination thereof. A tempera-
5.3.2 The modulus as a function of frequency, ture controller should be sufficiently stable to permit measure-
5.3.3 The effects of processing treatment, including ment of environmental chamber temperature to within 1°C.
orientation, 7.3 Nitrogen or other inert gas supply for purging purposes.
5.3.4 Relative resin behavioral properties, including cure
and damping, 8. Test Specimens
5.3.5 The effects of substrate types and orientation (fabri-
cation) on elastic modulus, and 8.1 Any rectangular specimen, representative of the mate-
5.3.6 The effects of formulation additives that might affect rial being tested and within the fixturing capabilities of the
processability or performance. specific test instrument employed, shall be used so long as an
accurate description of the specimen is clearly stated in the test
5.4 Before proceeding with this test method, reference report.
should be made to the specification of the material being tested.
Any test specimen preparation, conditioning, dimensions, or NOTE 2—The test specimens may be cut from sheets, plates, or molded
shapes, or may be molded to the desired finished dimensions.
testing parameters, or combination thereof, covered in the
relevant ASTM materials specification shall take precedence 9. Calibration
over those mentioned in this test method. If there are no
relevant ASTM materials specifications, then the default con- 9.1 Calibrate the instrument using procedures recommended
ditions apply. by the manufacturer.

6. Interferences 10. Conditioning


6.1 Since small test specimen geometries are used, it is 10.1 Conditioning—Condition the test specimens at 23.0 6
essential that the specimens be representative of the material 2.0°C and 50 6 5 % relative humidity for not less than 40 h
being tested. prior to testing in accordance with Procedure A of Practice
D618, unless otherwise specified by the contract or relevant
7. Apparatus material specification.
7.1 The function of the apparatus is to hold a rectangular
test specimen so that the material acts as the elastic and 11. Procedure
dissipative element in a mechanically driven torsional system. 11.1 Use an untested specimen for each measurement.
Dynamic mechanical instruments operate at a forced, constant Measure the width and thickness of the specimen to the nearest
amplitude, and either at a fixed frequency, or variable frequen- 0.03 mm at the center of the specimen and enter those
cies. dimensions into the test program using the instrument’s soft-
7.2 The apparatus shall consist of the following: ware.
7.2.1 Fixed Member—A fixed or essentially stationary 11.2 Clamp the test specimen between the movable and
member carrying one grip. stationary members using shim stock, if necessary, to minimize
7.2.2 Movable Member—A movable member carrying a slippage within the clamp.
second grip. 11.3 Preload the test specimen so that a positive normal
7.2.3 Grips—Grips for holding the test specimen between force is maintained during the test. Monitor the normal force
the fixed member and the movable member. The grips shall be during testing to ensure adequate preloading.
mechanically aligned, that is, they shall be attached to the fixed
and movable member, respectively, in such a manner that they 11.4 Measure the jaw separation between the movable and
will move into alignment as soon as any load is applied, so that stationary members to the nearest 0.03 mm and enter that
the long axis of the test specimen will coincide with the dimension into the test program using the instrument’s soft-
direction of the applied pull through the center line of the grip ware.
assembly. NOTE 3—Tests may be conducted in several modes depending on the
7.2.3.1 The test specimen shall be held in such a way that desired characterization requirements and the properties of interest.
slippage relative to the grips is minimized. Generally those modes include a strain sweep during which the tempera-
ture and frequency are maintained at constant values; a frequency sweep
7.2.4 Deformation (Strain Device)—A device for applying a
during which the temperature and strain are maintained at constant values;
continuous linear deformation (strain) to the specimen. In the a temperature sweep during which the strain and frequency are maintained
force-displacement device the deformation (strain) is applied at constant values or a frequency-temperature sweep during which the
and then released. (See Table 1 of Practice D4065.) strain is maintained at a constant value and properties are measured across
7.2.5 Detectors—Devices for determining dependent and a range of frequencies at step increments of temperature.
independent experimental parameters, such as force (stress), 11.5 Based on the type of test being conducted:
deformation (strain), frequency, and temperature. Temperature 11.5.1 Select the frequency (or range of frequency) for
should be measurable with a precision of 61°C, frequency to dynamic-torsional displacement as desired.
61 %, and force to 61 %. 11.5.2 Select the torsional-displacement amplitude (or range
7.2.6 Temperature Controller and Oven— A device for of amplitude) as desired, making sure it is within the material’s
controlling the temperature, either by heating (in steps or linear elastic region.

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D5279 − 13
NOTE 4—An independent strain sweep test may need to be run to 13.1.3 Conditioning procedure,
establish this property. 13.1.4 Description of the instrument used for the test,
11.5.3 Select the temperature (or range of temperature), 13.1.5 Description of the calibration procedure,
dwell time and either ramp rate or step increments to be used 13.1.6 Identification of the sample atmosphere by gas
if temperature is to be varied. composition, purity, and rate used,
11.5.3.1 Temperature increases should be controlled to 1 to 13.1.7 Width and thickness of specimen,
2°C/min for linear increases or 2 to 5°C/min (with a minimum
13.1.8 Jaw separation distance,
of 1-min thermal-soak time for step increases). These soak
times should be set to assure thermal equilibrium of the test 13.1.9 Frequency of dynamic displacement,
material. Appropriate soak times are generally related to the 13.1.10 Amplitude of displacement,
mass of the test specimen and to the ramp rate or step 13.1.11 Thermal gradient; heating rate,
increment being used. 13.1.12 Number of specimens tested,
11.6 Conduct the desired test recording the appropriate data. 13.1.13 Table of data including moduli, tan delta, frequency,
strain, and temperature as appropriate, and
12. Calculations 13.1.14 A plot of the modulus (moduli) and tan delta as
12.1 The equations listed in Practice D4065 are used to appropriate. (See Fig. 1.)
calculate the important rheological properties measured in
forced, nonresonant dynamic displacement: 14. Precision and Bias

where: 14.1 The repeatability standard deviation has been deter-


mined for the following materials. Laboratory A evaluated a
G' = storage (elastic) modulus in torsion,
G" = loss (viscous) modulus in torsion, polyurethane sample and the values in Table 1 were obtained
G* = complex modulus in torsion, and with the same test method in the same laboratory by the same
d* = tan delta. operator using the same equipment in the shortest practical
period of time using test specimens taken at random from a
13. Report single quantity of homogeneous material. Laboratory B tested
13.1 Report the following information: the same material and obtained the results shown in Table 1.
13.1.1 Complete identification of the material tested, includ-
ing type, source, manufacturer’s code, number, form, principal 15. Keywords
dimensions, and previous history as available, 15.1 dynamic mechanical rheological properties; elastic;
13.1.2 Description and direction of cutting and loading loss; storage; tan delta; torsional shear modulus; viscoelastic
specimen, including preload force, behavior; viscous

FIG. 1 Dynamic Mechanical Modulus in Torsion as a Function of Temperature

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D5279 − 13
TABLE 1 DMRT-Torsion, Elastic Modulus, G’ (E8 Pascals) or (E9
dynes/cm2) at Selected Temperatures
Laboratory –40°C 0°C 40°C 80°C
A
Mean 3.773 0.2038 0.03624 0.03532
Standard 0.008 0.0067 0.00032 0.00087
Deviation
B
Mean 3.568 0.2263 0.03206 0.02758
Standard 0.160 0.0461 0.00142 0.00023
Deviation

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5279 - 08)
that may impact the use of this standard. (September 1, 2013)

(1) Revised Section 8 to reduce permissive language. (2) Added Note 2 and renumbered subsequent notes.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5296 − 19

Standard Test Method for


Molecular Weight Averages and Molecular Weight
Distribution of Polystyrene by High Performance Size-
Exclusion Chromatography1
This standard is issued under the fixed designation D5296; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 1.5 This international standard was developed in accor-


1.1 This test method covers the determination of molecular dance with internationally recognized principles on standard-
weight (MW) averages and the distribution of molecular ization established in the Decision on Principles for the
weights for linear, soluble polystyrene by high-performance Development of International Standards, Guides and Recom-
size-exclusion chromatography (HPSEC). This test method is mendations issued by the World Trade Organization Technical
not absolute and requires the use of commercially available Barriers to Trade (TBT) Committee.
narrow molecular weight distribution (MWD) polystyrene
standards for calibration. This test method is applicable for 2. Referenced Documents
samples containing molecular weight components that have 2.1 ASTM Standards:3
elution volumes falling within the elution volume range D883 Terminology Relating to Plastics
defined by polystyrene standards (that is, molecular weights D2857 Practice for Dilute Solution Viscosity of Polymers
generally from 2000 to 2 000 000 g·mol−1). D3016 Practice for Use of Liquid Exclusion Chromatogra-
1.2 The HPSEC is differentiated from traditional size- phy Terms and Relationships
exclusion chromatography SEC (also referred to as gel perme- E685 Practice for Testing Fixed-Wavelength Photometric
ation chromatography (GPC)) in that the number of theoretical Detectors Used in Liquid Chromatography
plates per metre with an HPSEC system is at least ten times E691 Practice for Conducting an Interlaboratory Study to
greater than that for traditional SEC (see Terminology D883 Determine the Precision of a Test Method
and Practice D3016).2 The HPSEC systems employ low-
volume liquid chromatography components and columns 3. Terminology
packed with relatively small (generally 3 to 20 µm) micropo- 3.1 Definitions—For definitions of technical terms pertain-
rous particles. High-performance liquid chromatography in- ing to plastics used in this test method see Terminology D883.
strumentation and automated data handling systems for data
acquisition and processing are required. 4. Summary of Test Method
1.3 The values stated in SI units are to be regarded as the 4.1 In this test method a dilute solution of a polystyrene
standard. sample is injected into a liquid mobile phase containing the
1.4 This standard does not purport to address all of the same solvent used to prepare the polymer solution. The mobile
safety concerns, if any, associated with its use. It is the phase transports the polymer into and through a chromato-
responsibility of the user of this standard to establish appro- graphic column (or set of columns connected in series) packed
priate safety, health, and environmental practices and deter- with a solid or semirigid, porous substrate which separates the
mine the applicability of regulatory limitations prior to use. polymer molecules according to their size in solution. Starting
Specific precautionary statements are given in Section 9. from injection, a detector continuously monitors the eluate as a
function of elution volume (or time). Upon emerging from the
NOTE 1—There is no known ISO equivalent to this standard. column(s), the size-separated molecules are detected and
recorded according to their concentration. Through calibration,
the elution volumes (or times) are converted to molecular
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Nov. 1, 2019. Published December 2019. Originally
3
approved in 1992. Last previous edition approved in 2011 as D5296 – 11. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D5296-19. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
See also AMD Bibliography and Bibliography Supplements AMD 40-S1, 40-S2, Standards volume information, refer to the standard’s Document Summary page on
and 40-S3 on Size Exclusion Chromatography, available from ASTM Headquarters. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D5296 − 19
weights, and various molecular weight parameters for the 7.2 Essential Components—The essential components of
sample are calculated from the molecular weight/concentration instrumentation are a solvent reservoir, solvent pumping
data. system, sample injector, packed column(s), solute detector, low
dead-volume liquid chromatography tubing and fittings, waste
5. Significance and Use container, recorder, and an automated data-handling system.
5.1 General Utility—The molecular weight (MW) and mo- Any component used shall meet the safety and performance
lecular weight distribution (MWD) are fundamental character- requirements specified as follows.
istics of a polymer sample. They are used for a wide variety of 7.2.1 The interrelationships of the components are shown
correlations for fundamental studies, processing, or product schematically in Fig. 1. For instruments that have injector,
applications. For example, the observed MWD is compared to column(s), detector, or other components operated above
one predicted from assumed kinetics or mechanisms for a ambient temperature, the use of a degasser located in the
polymerization reaction. Differences between the values will solvent reservoir or between the reservoir and pumping system
allow alteration of theory or experimental design. Similarly, the is recommended to remove air from the solvent. Typical
strength, melt flow, and other properties of a polymer sample laboratory glassware and an analytical balance are also needed.
usually are dependent on MW and MWD. Determinations of NOTE 2—A number of systems and components for performing HPSEC
MW and MWD are used for quality control of polymers. are available commercially.
5.2 Limitations—Because of the need for specific calibra- 7.3 Solvent Reservoir—The solvent reservoir must hold
tion of the polymer type under study, and because of the sufficient solvent to ensure consistency of composition for a
specific nature of polymer/solvent/column-packing number of runs or analyses. The reservoir shall permit control
interactions, this test method is valid only for polystyrene and of the environment in contact with the solvent, and be
non-exclusion effects are to be avoided. However, many of the completely inert to the solvent employed. In addition, some
principles of the method have been applied in generating means of agitation (for example, magnetic stirring) is recom-
HPSEC methods for other polymer systems, for example, using mended to ensure uniform composition.
the principles of universal calibration. (see Practice D3016). 7.4 Solvent Pumping System—The principal requirement of
a pumping system is production of a constant and pulseless
6. Units and Symbols flow of solvent through the columns. In general, the rate of
6.1 Units and symbols related to function are given in Table flow shall be adjustable between 0.1 and 5.0 mL/min and
1. back-pressures shall not exceed limits specified by the column
manufacturer (for example, 28 MPa). If the elution volume is
6.2 Equivalencies used in this test method are as follows:
not being measured directly or corrected for systematic
Common Unit/Symbol SI Unit or Symbol
changes, the precision in the flow rate must be at least 60.3 %
1 mL·min−1 = 1.667 × 10−8 m3 ·s̄−1 as measured under the conditions and over the time interval
1 × 107 dyn·cm−2 = 145 psi = 1 MPa required for running a typical analysis.
7. Apparatus 7.5 Sample Injector—The purpose of an injection system is
to generate a sharply defined zone of solution containing the
7.1 Introduction—Liquid high-performance size-exclusion sample when introducing the sample into the flow stream. A
chromatography (HPSEC) is a specific form of liquid chroma- valve and loop assembly or any of a number of commercially
tography and is differentiated from traditional SEC in that available high-performance liquid chromatography automatic
HPSEC uses columns with at least ten times the number of injection systems is suitable for this purpose. Requirements
theoretical plates per metre. The principal distinguishing fea- include minimal contribution to band spreading, injector ability
ture of HPSEC is the column packing material that is discussed to operate at the back-pressure generated by the columns,
as follows. repeatability of injection volume, and no carryover.
7.6 Columns—Stainless steel columns with uniform and
highly polished inside walls are usually selected for HPSEC.
TABLE 1 Units and Symbols Related to Function Columns with lengths ranging from 15 to 50 cm and special
Common Unit/ SI Unit/ end fittings, frits, and connectors designed to minimize dead
Function
Symbol Symbol volume and mixing are recommended. Micro-particulate, semi-
Basic property definition Molecular weight (Daltons) g·mol−1 rigid organic gels, and rigid solid, porous packing materials are
Solvent flow rate mL·min−1 m3 ·s−1
A
Sample weight (mass) mg
A
Sample solution volume µL, mL
A
Pore size Å
A
Particle Size µm
A
Elution volume µL, mL
A
Elution time s
A
Chromatogram peak mm
heights
Column back pressure dyn·cm−2 (psi) N·m−2 or pascal (Pa)
A
Same as common unit.
FIG. 1 Schematic of an HPSEC System

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D5296 − 19
used for HPSEC. Generally, the packing materials have narrow wavelength are important to ensure a MW-independent concentration
particle size distributions with particle sizes in the range from response. Failure to do so may result in erroneous MW-averages and a
distorted MWD.
3 to 20 µm. Packing materials also are available in a variety of
shapes and pore sizes. Columns are either packed with particles 7.8 Tubing and Fittings—All tubing between the sample
of relatively uniform pore size or with a “mixed bed” of injector and the detector shall be no greater than 0.25-mm
particles to produce a broad range of pore sizes for polymer [0.010-in.] internal diameter and of sufficient thickness for use
separation. If a set of columns is used, it is recommended that at pressures up to 42 MPa. Connecting tubings shall be kept as
the columns be connected starting from the injector outlet in short as possible and all fittings and connectors must be
order of columns having the smallest to those having the designed to prevent mixing and have low dead volumes.
largest packing pore size. 7.9 Recorder/Plotter—Either a recording potentiometer
NOTE 3—Column packing materials and packed HPSEC columns are with a full-scale response of at least 2 s or a printing device
available commercially from a number of manufacturers. Users of this test connected to a data handling system is recommended to plot
method are advised to follow manufacturers’ guidelines and recommen- the chromatographic data. Choose a pen response and signal-
dations for the care and use of their HPSEC columns. For example,
manufacturers’ guidelines may override the preceding recommendation
to-noise ratio so that the concentration signal is not appreciably
for ordering the placement of columns in a column set because of concern perturbed.
about the fragility of smaller pore size packing materials.
7.10 Data Handling Systems—Means must be provided for
7.7 Detectors—The purpose of the detector is to continu- determining chromatographic peak heights or integrated area
ously monitor the concentration of solute eluting from the segments at prescribed intervals under the HPSEC chromato-
chromatographic column(s). Consequently, the detector must gram and for handling and reporting the data. This is best
be sufficiently sensitive and respond linearly to the solute accomplished by means of a computer or a real-time data
concentration. Additionally, the detector must not appreciably acquisition system with either off-line or on-line data process-
distort the concentration gradient in the emerging stream. This ing.
requirement imposes severe limitations on the volume of
solution available for detection. For example, use of detectors NOTE 6—Data acquisition and handling systems for HPSEC have not
been standardized. However, it is noted that a number of different
with cell volumes greater than 15 µL generally will not be manufacturers now provide chromatography data systems that include
accepted with this test method. Most detectors employed for HPSEC software. Also, some users have developed their own specialized
HPSEC are based upon photometric measurements (refractive HPSEC computer software.
index, UV-visible, fluorescence and infrared absorbance). Prac- 7.11 Other Components—Special solvent line filters, pres-
tice E685 serves as a guide for testing the performance of sure monitors, pulse dampers, flowmeters, thermostated ovens,
photometric detectors used in high-performance liquid chro- syphon counters, plotters, raw data storage systems, software,
matographic systems. Other detectors with appropriate sensi- and so forth are oftentimes incorporated with the essential
tivity are also acceptable. The differential refractometer has components previously listed.
moderate sensitivity and general utility. It provides a signal
proportional to the difference in refractive index (∆RI) between 7.12 HPSEC System—Any satisfactory combination of the
the solvent and the column eluate. The detector shall be able to above components that will meet the performance require-
respond to 10−7 to 10−8 ∆RI unit with cell volumes ≤ 10 µL. ments of Section 12.
NOTE 4—The change in the specific refractive index increment (dn/dc) 8. Reagents and Materials
of polystyrene is negligible at molecular weights greater than about 5000
g·mol−1. No appreciable error in molecular weight averages will be 8.1 Solvent—Tetrahydrofuran (THF) is recommended as the
introduced with this detector for polystyrene as long as its number-average solvent for this test method. However, any solvent that is
molecular weight, Mn, is greater than 5000 g·mol−1. The principal
disadvantage of the differential refractometer is that precise control of
compatible with the HPSEC system components and column
temperature, pressure, and flow rate is required to maintain a stable signal packing materials and is considered to be a good solvent for
for an appropriate level of sensitivity. For example, most organic liquids polystyrene is acceptable. To a certain extent, the choice of
have a temperature coefficient of 10−4 RI units per K. Consequently, the solvent dictates the operating temperature, as well as the
temperature within the RI detector cell must be controlled to within 10−4 detector, selected for the HPSEC system. The temperature must
°C.
NOTE 5—Benzoyl peroxide is commonly used as a free radical initiator be sufficiently high to keep the eluent viscosity low (usually 1
for styrene in the synthesis of polystyrene. The presence of small cp or less) and yet not too high to cause eluent to boil or degas.
concentrations of initiator fragments containing strong chromophores, Considering detector limitations, solvents having refractive
such as the benzoate group resulting from the decomposition of benzoyl indices similar to that of polystyrene are not preferred for use
peroxide, as polymer end groups can significantly alter the ultraviolet with differential refractive index detectors; while those absorb-
(UV) absorption characteristics of polystyrene.4 Since the relative con-
centration of such end groups increases with decreasing polymer MW, the ing strongly in the UV, such as toluene, shall not be used with
relationship between detector response and polymer concentration (molar UV (254-nm) detectors. Solvent purity and consistency must
absorptivity in the Beer-Lambert law) may change with MW. Photometric also be considered when choosing a solvent. For example,
detectors (UV and fluorescence) are particularly sensitive to the presence unless freshly distilled and kept in an all glass (amber)
of strong chromophoric end groups. Choice of detector and selection of
container under an inert gas, THF will react with oxygen to
form peroxides that absorb in the UV and are hazardous upon
4
Garcia Rubio, L. H., Ro, N., and Patel, R. D., Macromolecules, 17, 1984, p. evaporative concentration. Therefore, THF must either contain
1998. an antioxidant such as 0.025 to 0.1 % w ⁄v butylated hydroxy

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D5296 − 19
toluene, or be continuously blanketed or sparged with an inert 10.5 Data Handling System—Users are advised to follow
gas like helium to prevent peroxide formation. recommendations of their computer or data system manufac-
8.2 Polymer Standards—Unimodal, narrow MWD (M̄w /M̄n turer for setting data acquisition and integration parameters.
< 1.1) polystyrene standards of known molecular weight are
preferred for calibration. Ideally, the average molecular 11. Preparation of Solutions
weights of the standards are based on absolute MW methods 11.1 Polymer Samples—Solutions are prepared by weighing
such as end-group analysis, osmometry, light scattering, or 10 to 50 mg of the polymer sample into a clean, dry, 50-mL
ultracentrifugation. flask having a screw cap lined with solvent-resistant material or
8.3 Low MW Standards—Low MW compounds, such as into glasswares such as volumetric flasks fitted with ground
o-dichlorobenzene, that are used for determining plate count or glass stoppers. Next, the flask is filled two thirds with solvent
as internal standards must be of high purity. Sulfur is an syphoned from the solvent reservoir and then stoppered. The
excellent internal standard for monitoring changes in eluent polymer must be dissolved at room temperature. Magnetic
flow rate in most HPSEC systems where THF is used as the stirring devices or laboratory shakers are recommended to aid
solvent. Sulfur elutes after the HPSEC “junk” peak composed dissolution. Excessive temperature or ultrasonic devices have
of low MW compounds or injected air, or both, and is available been known to cause the polymer to degrade at times and
in high purity. therefore, must not be used with this test method. After the
polymer has dissolved, additional solvent from the solvent
9. Hazards reservoir is added to fill the flask. An alternative way is to
9.1 Solvents used in this test method are likely to be toxic or prepare the solution from “stock” solutions containing an
highly flammable, or both. Direct contact with the skin and internal standard as described in 11.3. Polystyrene solutions
inhalation of solvent vapors shall be avoided. The user is prepared with solvents such as THF are very stable, as long as
advised to consult literature and follow recommended proce- M < 500 000 g·mol−1. However, it is a good practice to analyze
dures pertaining to the safe handling of the solvent. Similar the polymer solutions within 24 h of their preparation.
precautions are to be followed with respect to the handling of 11.2 Polymer Standards—The same procedure as described
low MW standards. in 11.1 is used with the exception that “cocktails” of two or
more narrow MWD polymer standards be prepared in the same
10. Preparation of Apparatus flask. Such cocktail solutions are useful for MW calibration
10.1 Assembly—The HPSEC system must be assembled and for determining resolution. It is recommended that higher
into an integrated package as shown in Fig. 1 and readied for MW polymer standards (M > 800 000 g·mol−1) be prepared as
operation. For commercial systems, manufacturers’ guidelines single, more dilute solutions to reduce problems relating to
and recommendations shall be followed for assembly and polymer size in solution and concentration during calibration.
operation. NOTE 7—To ensure good precision, the mass of each injected standard
10.2 Temperature—An operating temperature is not speci- and sample must be consistent from analysis to analysis.
fied in this test method. Maintain a relatively constant tem- 11.3 Low MW Standards—The same procedure as described
perature of the critical internal components (injection loop, in 11.1 is used to prepare dilute solutions (0.1 % w/v) of low
column(s), detector, and connecting tubing) that is consistent MW standards such as o-dichlorobenzene for determining the
with the choice of solvent. The temperature of the previously plate count number (see 12.1). Dilute solutions (≤0.01 % w ⁄v)
mentioned internal components during an analysis must be of low MW compounds also are sometimes prepared to
within 3°C of their temperature at calibration. introduce internal standards into polymer solutions. “Stock”
10.3 Flow Rate—Column and instrument manufacturers’ solutions containing an internal standard, such as sulfur when
recommendations shall be followed when selecting a flow rate THF is the solvent, have been used directly in the preparation
and starting the solvent pumping system. A flow rate of 1 6 0.1 of polymer solutions or be added as aliquots to solutions
mL·min−1 is suggested, but not required, for this test method. If already prepared.
necessary, the pumping system is adjusted to deliver a rela- NOTE 8—A typical “stock” solution contains 0.03 % w ⁄v sulfur can be
tively constant and pulseless flow of eluent from the detector prepared using THF from the solvent reservoir. It is sometimes desirable
outlet. Flow rate is measured by determining either the volume to use an ultrasonic device to assist dissolution of the sulfur. Sulfur can be
or weight of solvent eluted over a sufficiently long period of detected using differential refractive index and UV (254- nm) detectors.
time and under suitable conditions to guarantee a precision of 11.4 Filtration—It is recommended that all solutions be
at least 60.3 %. Flow rates must be determined during filtered through membrane filters to remove lint and other
calibration and, if practical, before or after each analysis. materials likely to obstruct the columns and other system
Alternatively, use an internal standard (see 12.5) or a flow- components. Except for very high MW samples, membrane
measuring device, such as a syphon dump, to monitor changes filters with pore sizes in the range from 0.2 to 0.5 µm are
in flow rate. recommended. (The membrane pore size must not exceed 5
10.4 Detector—Detector settings and wavelength selection, µm.) The filters must be inert to the solvent and not become
in the case of photometric detectors, shall provide optimum clogged during filtration.
sensitivity for solute detection without causing undue baseline NOTE 9—Filtration often reveals the presence of gel in solutions even
noise or overloading of the output signal. though the solutions appear clear to the eye, as is the case with many

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D5296 − 19
microgels. During filtration, gel particles are likely to plug the pores of the W = peak width in elution volume (or time) units as
filter, noticeable by an excessive pressure needed for filtration. If such an
obstruction occurs, the soluble portion of the polymer may be partially
determined by measuring the distance between the
removed during filtration, the obstructed membrane now acting as an baseline intercepts of lines drawn tangent to the peak
ultra-filtration device. In this case, the polymer in the filtrate may no inflection points as shown in Fig. 2.
longer be representative of the soluble portion of the sample. Therefore, if
extensive plugging of the membrane pores is indicated, the meaning of the
12.1.2 Since N is a dimensionless parameter, the plate count
chromatographic results is open to doubt. number has the same value, regardless, whether VR and W are
measured in elution volume or elution time units. To compare
11.5 Test for Sample Solution Suitability—The mass of
plate count numbers for different systems, N is usually normal-
polymer injected for an HPSEC analysis is typically between
ized with respect to the total column(s) length, L; that is:
0.05 and 0.5 mg depending on the expected breadth of the
molecular weight distribution. Use smaller sample size for N' 5 N/L (2)
polymers of narrower MW distribution or higher MW. This 12.1.3 The HPSEC columns are expected to equal or exceed
method assumes that the mass of polymer injected is suffi- N' = 13 100 plates·m−1. The HPSEC systems not meeting this
ciently small such that the hydrodynamic volume of the performance requirement shall be examined and, if necessary,
polymer and the chromatographic separation mechanism do the column(s) replaced. Occasional monitoring of the plate
not depend upon the mass or concentration of polymer in- count is useful in trouble-shooting problems in the total
jected. However, if the injected solution concentration is too HPSEC system as well as problems relating to column(s)
high, especially for higher polymer molecular weight samples, performance.
the peak elution volume (time) and shape of the chromatogram
will be affected and possible leads to an erroneous MW 12.2 Resolution—Resolution, R, is a more meaningful pa-
determination. It is therefore advisable to rerun an unknown rameter for chromatographic performance than plate count
sample or standard at one half its original concentration (while number N'. R provides an indication of the separating
doubling detector sensitivity) to ensure that its peak elution is capability, as well as dispersion or band broadening effects, of
reproducible. If a change is observed, the run shall be repeated a column or column set. The resolution of two standard
with a still lower concentration of sample. The relationship polymers having narrow MWDs (M̄w/Mn < 1.1) is defined as
between log MW and mass injected is usually a continuous the specific resolution:
function. Dilutions shall be made until a low-range mass is R s 5 2· ~ V R2 2 V R1 ! / @ ~ W 1 1W 2 ! ·log10 ~ M 1 /M 2 ! # (3)
achieved which still provides adequate signal-to-noise to
where:
distinguish between MW values of interest. For polystyrene in
THF, the slope of the plot of log MW versus mass injected is VR 1, VR 2 = peak elution volumes or times measured at the
small; therefore, repeated dilutions will not greatly affect the peak maximum of polymer Standards 1 and 2,
determined MW.
W1, W2 = peak widths of Standards 1 and 2 measured in
elution volume or times units as indicated in
12. Performance Requirements
Fig. 3, and
12.1 Plate Count Number—The plate count number, N, is a M1, M2 = peak molecular weights of Standards 1 and 2.
dimensionless quantity related to column efficiency and pro- 12.2.1 The two standards shall differ in known molecular
vides an indication of dispersion processes in chromatographic weight values by a factor of about ten and shall be chromato-
systems. Various procedures and methods of calculation have graphed at a concentration of ≤0.05 % w/v and an injection
been successfully applied to estimate N. Users of this test volume ≤100 µL. It is recommended that the resolution
method are advised to follow recommendations of the column parameter Rs be determined over each decade of molecular
manufacturer when initially evaluating their columns. The weight for which this test method applies and that at least three
plate count number are to be determined under the same polymer standards be used. This test method requires that
conditions as those applied for this test method. For example, calculated R s values equal or exceed 1.7 for sufficient resolu-
utilize the following test conditions for both plate count tion over the applicable molecular weight range for samples
determination and testing: analyzed. Since resolution is a dimensionless parameter, Rs will
Solvent—Tetrahydrofuran (THF) have the same value as long as consistent units (elution volume
Temperature—30°C
Flow Rate—1 mL·min−1 or elution time) are used for its evaluation.
Test Solute—o-dichlorobenzene
Concentration—# 0.1 % w ⁄v
Injection Volume—1 to 5 µL
12.1.1 Assuming that the solute peak is symmetrical and has
a nearly Gaussian shape, the following approximation is used
to calculate the plate count number:
plate count, N 5 16 ~ V R /W ! 2 (1)

where:
VR = peak elution volume (or time) measured at the peak
maximum of the test solute and
FIG. 2 Measurement of Peak Width

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D5296 − 19
similar to that of a polymer peak (1 to 10 min) and therefore
must be minimized before analyses are conducted. The occur-
rence of long-term noise usually signifies that the chromato-
graphic system is not functioning properly. Long-term noise
shall not exceed 5 % of the maximum polymer peak signal.
Drift is defined as the average slope of the noise envelope
measured over a period of 1 h. Drift is not a problem if the
slope is constant over the time required to run an HPSEC
analysis and if the data handling system is capable of correct-
ing for sloping baselines. Erroneous results is likely to occur if
FIG. 3 Determination of Resolution, Rs , Using Narrow MWD drift exceeds 2 % of the maximum polymer peak signal and the
Polystyrene Standards M1 > M2
data system is unable to compensate for a sloping baseline.
12.5 Flow Rate—If uncorrected, small differences (> 0.3 %)
NOTE 10—Mixtures or “cocktails” of three or more polymer standards in the solvent flow rate, between the time the HPSEC system is
may be run to determine several Rs values with a single injection. For calibrated and when sample analyses are run, will have the
example, a mixture of polystyrene standards of molecular weight 10 000; potential to cause large systematic errors in MW values
100 000 and 1 000 000 g·mol−1 may be run to determine Rs over the MW
obtained. Determine the average flow rate of the system by
range from 10 000 to 1 000 000 g·mol−1. Alternatively, a mixture of 2000;
20 000; 200 000 and 2 000 000 g·mol−1 standards may be run to determine measuring either the volume or weight of solvent eluted over
Rs over a broader MW range. It is important to keep solution concentra- the time interval required for an analysis. If the flow rate varies
tions sufficiently low to avoid possible concentration effects (see 11.5). by more than 0.3 % over a period of several days, users are
12.2.2 Baseline resolution shall be observed for the elution strongly advised to add a flow-measuring device to their
peaks generated by mixtures of standards as previously de- system or to include an internal standard with samples injected
scribed. Such mixtures are extremely useful in determining for monitoring changes in eluent flow rate.
changes in HPSEC system performance and shall be run 13. Calibration
frequently to ensure calibration (see 13.2).
12.2.3 Resolution has also been defined in terms of the slope 13.1 Selection of Polystyrene Standards—Prepare fresh so-
of the HPSEC calibration curve (see 13.4). Present the calibra- lutions of polystyrene calibration standards as outlined in 11.2.
tion curve using a straight line with Slope S over the elution The calibration solutions shall be as dilute as possible to reduce
volume region of the polymer samples being analyzed, and Eq concentration effects. Indeed since the solutions are used only
3 becomes: for calibration and are not being analyzed for MW, much
higher noise levels are acceptable than what is indicated in
R s 5 @ 20.5 S· ~ W 1 1W 2 ! # 21 (4) 12.4. Equivalent standards from any source are acceptable. A
If W = W1 × W2 for polymer standards eluting within the minimum number of three standards per decade of molecular
straight region of the calibration curve, a limiting value of weight need to be run to calibrate over the MW range covered
resolution will be defined as follows: by the samples being analyzed. The samples need to be
chromatographed first to establish the estimated range.
limR s 5 ~ 2W·S ! 21 (5)
13.2 Injection of Polystyrene Standards—Make injections
In this case, changes in the slope of the calibration curve or with a clean micro-syringe (or automatic injector system).
peak width of a polymer standard would indicate a change in Flush the injector loop with solvent and expel air bubbles from
HPSEC system performance. the syringe before each injection. Add the internal standard, if
12.3 Detector Response—Select HPSEC operating condi- used, to solution before injection. Filtered solutions containing
tions and detector settings to optimize detector response. The two or more polystyrene standards are injected for calibration
user is referred to Practice E685 as a guide for testing the if the molecular weights of the standards are less than 800 000
performance of liquid chromatography detectors. Practice g·mol−1 and the elution peaks of the standards are baseline
E685 addresses determination of detector response in Sections resolved as shown in Fig. 3.
5 and 7. In order for this test method to be valid, the detected 13.2.1 Users are advised to inject higher MW (≥ 800 000
peak height or total integrated peak area of the eluted polymer g·mol−1) standards as separate solutions and at several different
must be directly proportional to the mass of polymer injected. concentrations. Each calibration standard shall be completely
A linear (Beer-Lambert law) relationship must be demonstrated eluted before the next standard solution is injected. The
for polystyrene as shown in Fig. 2. injection volumes of all standard solutions must be identical,
12.4 Baseline Stability—Conditions must be selected to regardless of concentration. The maximum recommended in-
minimize baseline noise. Practice E685 classifies noise as jection volume is related to the diameter (and packing volume)
short-term, long-term and drift. The inverse frequency or time of the HPSEC column(s). For columns with diameters of 0.6 to
period of short-term noise is much shorter than the elution time 0.8 cm, the injection volume shall be ≤100 µL. For column
of a polymer sample and therefore has the potential to be used diameters of 0.8 to 1.0 cm, injection volumes ≤150 µL are
to define the lower limit of detectability. In general, short-term recommended.
noise shall not exceed 2 % of the maximum polymer peak 13.3 Data Acquisition—Optimize data system parameters to
signal. Long-term noise refers to noise over a time interval determine elution peak maxima and corresponding elution

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D5296 − 19
volumes (or times) for the various polymer standards (and
internal standard). The elution volume is the product of elution
time and flow rate. Plot elution volumes (or times) at peak
maxima determined for each of the higher MW (≥ 800 000
g·mol−1) standards versus the concentration or mass inject and
then extrapolate to “zero” concentration to estimate the “true”
or concentration independent values of VR. (Determine and
record an average peak elution volume (or time) of the internal
standard VIS when the system is calibrated.)
NOTE 11—Measure peak elution volume (or time) from the point at
which the sample is injected to the location (or time) of the observed
maximum of the recorded chromatographic peak (see Fig. 2).
13.4 Generation of Calibration Curve—Obtain the HPSEC
calibration curve by plotting the measured peak elution
volumes, VR (or time) versus the logarithmic calculated “peak”
or mean molecular weight values (Mw·Mn)½ of the calibration
standards. By the nature of the HPSEC separation mechanism,
the calibration curve generally assumes an s-shape (as shown
by the dashed line in Fig. 5) that asymptotically approaches
total exclusion near the void volume at high MW (Solute A)
and approaches total permeation near the total column liquid
volume at low MW (Solute D). The useful separation region
covering a finite MW range resides between these two ex-
tremes. Use data handling systems or computer software to
treat the calibration data, if available.
13.4.1 This test method does not discriminate between the
various treatments except to recommend that users attempt to FIG. 5 HPSEC Calibration Curve
smooth or obtain a “best fit” of the data since errors are
associated with MW values reported for some standard poly- 14. Procedure
mers. The objective of the calibration curve is to relate an
experimental elution parameter VR to a respective polystyrene 14.1 Preparation for Analysis—Prepare polymer sample
MW value. solutions as described in 11.1, 11.4, and 11.5 and add an
13.4.2 Through column design or selection, it is sometimes internal standard, if used, to each sample solution before
possible to obtain a calibration curve that is essentially linear injection. Alternatively, use a “stock” solution containing an
over a broad MW range. For polymers that elute within this internal standard for monitoring eluent flow rate to prepare
region (for example, Solutes B and C in Fig. 5), a simple polymer sample solutions (see 11.3). Prepare the apparatus and
proportional relationship exists between Log M and VR. The fulfill the performance requirements (see Section 12).
proportionality constant equals the slope S of the linear region 14.2 Injection of Sample Solutions—Follow guidelines de-
of the calibration curve as follows: scribed in 13.2. The injection volume must be identical to that
log10 M 5 S o 1S·V R (6)
selected for calibration. A sharp increase or “pulse” in back
pressure upon injection indicates a serious problem in the
and So is a constant for the system. HPSEC system that must be remedied before continuing with
this test method. The sample and internal standard, if present,
must be fully eluted before the next sample is injected.
14.3 Baseline Determination—Satisfy baseline criteria dis-
cussed in 12.4. Identify elution volumes Va and Vb correspond-
ing to the beginning and end of the polymer chromatogram (see
Fig. 6). The baseline between Va and Vb is assumed to be linear;
that is, a straight line.

FIG. 4 Linear Detector Response to Polystyrene Sample Concen- FIG. 6 Typical Chromatogram for Which This Test Method is
tration Applicable

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D5296 − 19
14.3.1 The establishment of Va, the low elution volume 15. Calculation
(high MW) end of the chromatogram, is straightforward. Here, 15.1 Tabulation of Data—Record data as indicated in Table
the baseline is usually stable and not influenced by low MW X1.1 of Appendix X1. Obtain the appropriate values for M
impurities. using the MW calibration curve outlined in 13.4.
14.3.2 The establishment of Vb is more difficult and depends
largely upon the separation of the polymer peak from peaks of 15.2 Calculation of Molecular Weight Averages—Calculate
low MW impurities and the recovery of a stable baseline. With the number-, weight-, and z-average molecular weights (M̄n ,
baseline resolution and recovery the choice of Vb is obvious. M̄w , and M̄z ) using data from Table X1.1 and the following
14.3.3 Fig. 6 shows the chromatogram for a polystyrene expressions.
sample with adequate separation between polymer and impu- N N

rity peaks and good baseline recovery. In this example, Va and Mn 5 ( A / ( ~A


i51
i
i51
i /M i ! (9)
Vb were chosen to be 18.99 and 29.49 mL, respectively. N N
14.3.4 Fig. 7 shows the chromatogram for a polystyrene Mw 5 ( ~A
i51
i ·M i ! / (A
i51
i (10)
with incomplete separation of the polymer and impurity peaks.
N N
The polymer apparently has a low MW “tail” that extends into
the region (M < 2000 g·mol−1) where this test method is no
Mz 5 (
i51
~ A i ·M i 2 ! / ( ~ A i ·M i !
i51
(11)

longer valid. This test method does not encompass the problem If the elution volume interval ∆Vi is constant, parameters Ai
of establishing the correct baseline and cut off limits for the and Mi are the chromatographic peak slice area and polystyrene
chromatogram shown in Fig. 7 and therefore is not applicable MW associated with the (corrected) elution volume Vi and N is
to such a sample. equal to the number of data points obtained from the chro-
14.4 Data Acquisition—It is possible that data systems and matogram between Va to Vb (see 14.3). An example of this
computer software handle data acquisition differently. Upon method of calculating the molecular weight averages is given
acquisition, data under the polymer elution peak is usually in Appendix X1. If N is sufficiently large, the use of area
handled in discrete segments Ai (integrated area slices) or as segments Ai or peak heights Hi will yield equivalent results.
digitized chromatogram heights Hi by recording the vertical 15.3 Calculation of Intrinsic Viscosity—Determine the in-
displacements between the chromatogram trace and the base- trinsic viscosity [η] of a polymer in dilute solution experimen-
line at elution volumes Vi over designated intervals. A mini- tally using Test Method D2857.5 The value of [η] is related to
mum of 40 area segments or heights are required by this test polymer MW by the following Mark-Houwink equation:
method.
@ η # 5 K·M av (12)
14.5 Flow Rate Correction—If the HPSEC system does not
contain a continuous flow rate monitor or some device, such as where K and a are constants for a given polymer/solvent
a syphon dump, that automatically and precisely monitors system at a specified temperature and Mv is the viscosity-
elution volume increments, then the flow rate must be within average molecular weight that is calculated from HPSEC data:
0.3 % of its value measured at calibration. Otherwise, using an
internal standard is recommended. When an internal standard Mv 5 F( ~
i51
N

A i ·M ia ! /
N

(A
i51
i G 1/a

(13)
is used, correct sample elution volumes Vi ' or times ti ' (made
consistent with calibration values) by the following relation: Values of K and a appropriate to the polymer type and the
solvent and temperature conditions used in Test Method D2857
corrected V i 5 V i '· ~ V IS! / ~ V IS! ' (7) must be applied when calculating the parameter from HPSEC
or: data. Acceptable parameters for polystyrene in dilute THF
solution at 25°C are K = 0.016 mL·g−1 and a = 0.706.5
corrected t i 5 t i '· ~ t IS! / ~ t IS! ' (8)
15.4 Molecular Weight Distributions: Cumulative Weight
where: Fraction Distribution—Calculate the cumulative distribution
(VIS) and (tIS ) = average elution volume and time, by integrating the chromatogram to different elution volumes
respectively, of the internal standard mea- (molecular weights) using standard numerical integration pro-
sured at calibration and cedures and then dividing these areas by the total area under
(VIS)' and (tIS )' = elution volume and time of the internal the chromatogram. This area ratio is the cumulative weight
standard obtained with the sample analy- fraction Wi and equals the weight fraction of polymer having
sis. retention volumes greater than Vi and molecular weights less
than Mi. To display the distribution graphically, plot Wi versus
log10 Mi. An example of this method of calculating the
cumulative weight fraction distribution using peak area slices
is given in Appendix X1. If peak heights are determined and
the elution volume interval Vi is constant, the cumulative
weight fraction of solute of MW less than and equal to Mi is
defined as follows and illustrated in Fig. X2.1:
FIG. 7 Example of Chromatogram for Which This Test Method is
5
Not Applicable Provder, T., and Rosen, E. M., Separation Science, SESCA, 5, 1970, p. 437.

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D5296 − 19
i i N
analysis of linear polystyrene samples. Inaccurate molecular
Wi 5 1 2 (H
j51
N , j 512 ( H /( H
j51
j
j51
j (14)
weight values will be obtained if this test method is applied to
15.5 Molecular Weight Distributions: Differential Molecu- branched polystyrene samples.
lar Weight Distribution—Weight differential distribution func- 17.2 Tables 2-8 are based on an interlaboratory study
tions fw (M) and Fw (log10 M) are defined in Appendix X2. If conducted in 1990 in accordance with Practice E691, involving
determined correctly, plots of the differential distribution 3 polystyrene materials tested by 28 laboratories. For each
functions versus log10 M obtained using different HPSEC material, test solutions were prepared by the individual
systems to analyze the same sample will be identical. The laboratories, and these solutions were analyzed in triplicate
distribution function is defined as follows and illustrated in Fig. using various liquid chromatography (HPSEC) systems and
X2.1: test conditions. Some test results were rejected because the
F w ~ log10 M i ! 5 2H N,i / ~ dlog10 M/dV! (15) chromatographic systems failed to meet performance criteria
for plate count (N), resolution (Rs), calibration, flow rate,
The differential molecular weight distribution is determined detector response, baseline stability, data acquisition, or sample
using Eq 16. preparation. For this reason, test results from only 18 labora-
dW/d ~ log10M ! 5 log10M (16) tories are included in the statistical analysis presented in Tables
2-8.
16. Report
NOTE 12—The explanations of r and R are only intended to present a
16.1 Report the following information: meaningful way of considering the approximate precision of this test
16.1.1 Apparatus: method. The data of Tables 2-8 should not be applied to acceptance or
16.1.1.1 System type and model number, rejection of materials, as these data apply only to the materials tested in
the round robin and are unlikely to be rigorously representative of other
16.1.1.2 Column(s) packing type, dimensions, and
lots, formulations, conditions, materials, or laboratories. Users of this test
manufacturer, method should apply the principles outlined in Practice E691 to generate
16.1.1.3 Column temperature, °C, data specific to the materials and laboratory (or between specific labora-
16.1.1.4 Solvent (plus additives and treatment, if any), tories). The principles of 17.2.1 – 17.2.1.3 would then be valid for such
16.1.1.5 Solvent flow rate (mL·min−1), data.
16.1.1.6 Detector type and model number, 17.2.1 Concept of r and R in Tables 2-8—If Sr and SR have
16.1.1.7 Internal standard or flow monitor (if used), or both, been calculated from a large enough body of data, and for test
16.1.1.8 Injection volume, µL, and results that were averages from testing 3 solutions for each test
16.1.1.9 Polymer sample solution concentration (mg·mL−1). result, then:
16.1.2 Plate Count and Resolution: 17.2.1.1 Repeatability Limit (r)—The value below which
Plate Count N' (plates/metre) = ___, using ___ as the test solute. the absolute difference between two individual test results
Resolution Rs = ___, using standards ___ and ___ and (Eq 3-5) ___. obtained under repeatability conditions may be expected to
16.1.3 Calibration Standards: occur with a probability of approximately 0.95 (95 %).
Source Description (Mw ·Mn)½ Peak VR 17.2.1.2 Reproducibility Limit (R)—The value below which
1. the absolute difference between two individual test results
2. obtained under reproducibility conditions may be expected to
3.
4. occur with a probability of approximately 0.95 (95 %).
5. 17.2.1.3 When required, conducting equivalence testing on
6. numerical data from two sources shall be conducted in accor-
etc.
dance with E2935 or any known method for judging the
16.1.4 Calculated Molecular Weight Averages and Hetero- equivalence of two means, for example a t-test.
geneity Parameters:
17.3 Bias—There are no recognized standards by which to
M̄n = _____
M̄w = _____ M̄w /M̄n = _____ estimate bias of this method.
M̄z = _____ M̄z /M̄n = _____
18. Keywords
16.1.5 Calculated Viscosity-Average MW and Intrinsic Vis-
cosity: 18.1 high-performance size exclusion chromatography
M̄v = _____ [η] = _____ mL·g −1 (HPSEC); molecular weight average; molecular weight distri-
using K = _____ mL·g−1 and a = _____ bution; polystyrene
17. Precision and Bias TABLE 2 Repeatability and Reproducibility of Mn Measurements
for Polystyrene
17.1 Limitations and Considerations—To obtain molecular
weights from high-performance size exclusion chromatogra- Material Average Sr SR r R

phy (HPSEC), calibration must be employed using standard A 98 389 4 524 7 850 12 667 21 679
B 118 533 4 691 10 869 13 134 30 433
samples of known molecular weight and the same chemical C 159 898 1 600 11 433 4 481 32 013
type as the unknowns. This test method is limited to the

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TABLE 3 Repeatability and Reproducibility of Mw Measurements
for Polystyrene
Material Average Sr SR r R
A 258 122 6 131 17 860 17 167 50 008
B 383 459 8 043 33 637 22 521 94 182
C 167 745 3 036 12 057 8 501 33 761

TABLE 4 Repeatability and Reproducibility of Mz Measurements


for Polystyrene
Material Average Sr SR r R
A 493 511 31 966 73 406 89 504 205 536
B 935 058 28 228 160 256 80 864 448 717
C 174 470 3 787 13 199 10 604 36 957

TABLE 5 Repeatability and Reproducibility of Mw /Mn


Measurements for Polystyrene
Material Average Sr SR r R
A 2.6380 0.0871 0.2675 0.2440 0.7491
B 3.2572 0.1175 0.3890 0.3290 1.0890
C 1.0496 0.0111 0.0230 0.0311 0.0643

TABLE 6 Repeatability and Reproducibility of Mz /Mn


Measurements for Polystyrene
Material Average Sr SR r R
A 5.0912 0.2314 0.7676 0.6480 2.1493
B 7.9011 0.4956 1.5701 1.3877 4.3963
C 1.0912 0.0138 0.0366 0.0385 0.1023

TABLE 7 Repeatability and Reproducibility of Mv Measurements


for Polystyrene
Material Average Sr SR r R
A 233 518 9.086 17 422 25 441 48 783
B 335 318 5.142 23 424 14 397 65 586
C 166 381 630 11 577 1 763 32 416

TABLE 8 Repeatability and Reproducibility of [η] Measurements


for Polystyrene
Material Average Sr SR r R
A 97.601 1.925 5.239 5.390 14.670
B 126.639 2.209 7.568 6.186 21.192
C 77.458 1.496 4.087 4.188 11.443

APPENDIXES

(Nonmandatory Information)

X1. SAMPLE CALCULATIONS FROM SECTIONS 14 and 15

See Table X1.1.


TABLE X1.1 Sample Calculations From Sections 14 and 15A
i
1 Vi (mL) Mi (g·mol−1) Ai o Ai Wi Fw (log10 Mi)
i51

1 18.99 2 175 000 0 0 1 0


2 19.14 1 993 000 70 70 0.9998 0.0041
3 19.29 1 828 000 150 220 0.9995 0.0089

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D5296 − 19
TABLE X1.1 Continued
i
1 Vi (mL) Mi (g·mol−1) Ai o Ai Wi Fw (log10 Mi)
i51

4 19.44 1 680 000 230 450 0.9990 0.0138


5 19.59 1 344 000 340 790 0.9983 0.0207
6 19.74 1 422 000 455 1245 0.9973 0.0281
7 19.89 1 310 000 650 1895 0.9958 0.0403
8 20.04 1 207 000 879 2774 0.9939 0.0553
9 20.19 1 115 000 1271 4045 0.9911 0.0814
10 20.34 1 030 000 1756 5801 0.9872 0.1138
11 20.49 952 900 2273 8074 0.9822 0.1482
12 20.64 881 700 2906 10 980 0.9758 0.1911
13 20.79 816 500 3598 14 578 0.9678 0.2394
14 20.94 756 900 4330 18 908 0.9583 0.2906
15 21.09 701 800 5141 24 049 0.9470 0.3474
16 21.24 651 200 5950 29 999 0.9338 0.4054
17 21.39 604 600 6778 36 777 0.9189 0.4661
18 21.54 561 800 7583 44 360 0.9021 0.5264
19 21.69 522 300 8491 52 851 0.8834 0.5923
20 21.84 485 700 9339 62 190 0.8628 0.6551
21 21.99 451 900 10 159 72 349 0.8404 0.7181
22 22.14 420 700 10 899 83 248 0.8164 0.7735
23 22.29 391 600 11 577 94 825 0.7908 0.8241
24 22.44 364 700 12 050 106 875 0.7643 0.8640
25 22.59 339 900 12 302 119 177 0.7371 0.8887
26 22.74 316 900 12 918 132 095 0.7086 0.9352
27 22.89 295 400 13 202 145 297 0.6795 0.9560
28 23.04 275 400 13 478 158 775 0.6498 0.9759
29 23.19 256 700 13 553 172 328 0.6199 0.9870
30 23.34 239 500 13 666 185 994 0.5897 0.9969
31 23.49 223 300 13 711 199 705 0.5595 0.9940
32 23.64 208 200 13 565 213 270 0.5296 0.9888
33 23.79 194 300 13 541 226 811 0.4997 0.9904
34 23.94 181 200 13 353 240 164 0.4702 0.9690
35 24.09 168 900 13 104 253 268 0.4413 0.9518
36 24.24 157 600 12 867 266 135 0.4130 0.9352
37 24.39 146 900 11 852 277 987 0.3868 0.8581
38 24.54 136 900 12 277 290 264 0.3597 0.8837
39 24.69 127 500 11 932 302 196 0.3334 0.8528
40 24.84 118 800 11 500 313 696 0.3080 0.8246
41 24.99 110 700 11 163 324 859 0.2834 0.7963
42 25.14 103 000 10 684 335 543 0.2599 0.7558
43 25.29 95 890 10 248 345 791 0.2372 0.7226
44 25.44 89 210 9803 355 594 0.2156 0.6858
45 25.59 82 930 9351 364 945 0.1950 0.6506
46 25.74 77 090 8869 373 814 0.1754 0.6121
47 25.89 71 580 8278 382 092 0.1572 0.5650
48 26.04 66 430 7753 389 845 0.1401 0.5276
49 26.19 61 660 7306 397 151 0.1240 0.4928
50 26.34 57 140 6728 403 879 0.1091 0.4491
51 26.49 52 950 6191 410 070 0.0955 0.4102
52 26.64 49 020 5709 415 779 0.0829 0.3690
53 26.79 45 250 5189 420 968 0.0714 0.3360
54 26.94 41 900 4704 425 672 0.0610 0.3053
55 27.09 38 700 4171 329 843 0.0518 0.2647
56 27.24 35 700 3681 433 524 0.0437 0.2312
57 27.39 32 920 3286 436 810 0.0365 0.2040
58 27.54 30 320 2913 439 723 0.0300 0.1788
59 27.69 27 900 2525 442 248 0.0245 0.1531
60 27.84 25 640 2178 444 426 0.0197 0.1297
61 27.99 23 520 1905 446 331 0.0155 0.1122
62 28.14 21 580 1562 447 893 0.0120 0.0911
63 28.29 19 760 1313 449 206 0.0091 0.0754
64 28.44 18 080 1148 450 354 0.0066 0.0651
65 28.59 16 520 892 451 246 0.0046 0.0499
66 28.74 15 080 774 452 020 0.0029 0.0426
67 28.89 13 740 580 452 600 0.0016 0.0315
68 29.04 12 510 401 453 001 0.0008 0.0215
69 29.19 11 360 250 453 251 0.0002 0.0132
70 29.34 10 314 95 453 346 0 0.0049
71 29.49 9340 0 453 346 0 0

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D5296 − 19
N N N N
A
M n 5 o A i / o s A i /M i d 5115 000 g·mol21 M w 5 o s A i ·M i d / o A i 5253 000 g·mol21
i51 i51 i51 i51
N N
M z 5 o s A i ·M i 2 d / o s A i ·M i d 5446 000 g·mol21 M w /M n 52.20 M z /M n 53.88
i51 i51

Mv 5 Fo N

i51
N

s A i ·M i 2 d / o A i
i51
G 1/a
5229 000 g·mol21 f η g 50.016 M v 0.706 597.3 mL·g 21

X2. DERIVATION OF WEIGHT DIFFERENTIAL AND CUMULATIVE MOLECULAR WEIGHT DISTRIBUTION FUNCTIONS

X2.1 The weight differential distribution of molecular 2H N ~ V !


fw ~M! 5 (X2.7)
weight fw (M) is defined as the weight population density or 2.303 M ~ dlog10 M/dV!
frequency distribution of molecular weights. The weight frac-
tion of polymer is fw (M)dM in the molecular weight interval M and:
to (M + dM) or Fw (log10 M)dlog10 M from log10 M to (log10 2H N ~ V !
F w ~ log10 M ! 5 (X2.8)
M + dlog10 M). Since: ~ dlog10 M/dV!
f w ~ M ! dM 5 f w ~ M ! 2.303 M dlog10 M 5 F w ~ log10 M ! dlog10 M X2.1.4 The derivatives in Eq X2.7 and Eq X2.8 are best
(X2.1) obtained by analytically differentiating the calibration curve.
X2.1.1 Furthermore, the weight fraction integrated over all For example, if a polynomial is fit to the calibration points:
molecular weights equals unity; that is, log10 M 5 a1b·V1c·V 2 1f·V 3 (X2.9)
` `
*0
f w ~ M ! dM 5 * 0
F w ~ log10 M ! dlog10 M 5 1 (X2.2) Where a, b, c, and f are constants, then the derivative to be
substituted into Eq X2.7 and Eq X2.8 is:
X2.1.2 For a mass detector the unnormalized detector signal
H(V) is given by the following: dlog10 M/dV 5 b12c·V13f·V 2 (X2.10)

H ~ V ! 5 }C ~ V ! (X2.3) X2.2 Using finite difference expressions to approximate the


where C(V) is the concentration of solute in mass per unit derivative should be avoided because of inaccuracies for
volume eluted at retention volume, V, and is the detector nonlinear portions of the curve. Also, caution is advised in
response factor. The normalized signal HN (V) is equal there- fitting polynomials to investigate how the polynomial extrapo-
fore to the raw chromatogram; and the weight fraction of solute lates into regions beyond the first and last data points of the
in the elution volume range V to V + dV, is given by the calibration curve. The curve fitting procedure must give
following equation: reasonable extrapolations. Although not always possible, the
C ~ V ! dV H ~ V ! dV
best approach is to work only within the range of the
` 5 ` 5 H N ~ V ! dV (X2.4) calibration data and not rely on any extrapolation. The follow-
*
0
C ~ V ! dV * 0
H ~ V ! dV ing cumulative weight distribution function is generated from
X2.1.3 The integral area may be calculated for both uniform Eq X2.4 and represents the weight fraction of solute in the
and nonuniform elution volume intervals ∆V using the trap- elution volume range Va to V or molecular weight range Ma to
ezoidal rule: M:

(S D
V

* `
H ~ V ! dV 5
N21
H i 1H i11
·∆V i (X2.5)
W~M! 5 1 2 * Va
H N ~ V ! dV (X2.11)
0 i51 2

where: The weight fraction less than and equal to Mi is given by the
following:
∆Vi = Vi +1 − Vi.
(S D
i21
H N,j 1H N,j11
From Eq X2.2 and Eq X2.4 the identity: Wi 5 1 2 ·∆V j (X2.12)
j52 2
` `
*0
fw~ M ! dM 2 * 0
H N ~ V ! dV (X2.6)
X2.3 The weight differential and cumulative distribution
and the weight differential distribution functions are ob- plots for the data in Appendix X1, plotted using Eq X2.8 and
tained by: Eq X2.12, are shown as Fig. X2.1 and Fig. X2.2.

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FIG. X2.1 Weight Differential Distribution Plot for the Data of


Appendix X1 as Computed From Eq X2.5b

FIG. X2.2 Cumulative Weight Distribution Plot for the Data of


Appendix X1 as Computed From Eq X2.6b

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D4020 – 11) that may impact the use of this standard. (November 1, 2019)

(1) Updated definitions in Precision and Bias, Section 17. (2) Removed permissive language from several sections.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5319 − 17 An American National Standard

Standard Specification for


Glass-Fiber Reinforced Polyester Wall and Ceiling Panels1
This standard is issued under the fixed designation D5319; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 1.8 This standard does not purport to address all of the
1.1 This specification covers the classification, materials of safety concerns, if any, associated with its use. It is the
construction, workmanship, physical requirements, and meth- responsibility of the user of this standard to establish appro-
ods of testing glass-fiber-reinforced polyester composite wall priate safety, health and environmental practices and deter-
and ceiling panels intended for use in light construction and mine the applicability of regulatory limitations prior to use.
semi-structural applications. NOTE 1—There is no known ISO equivalent to this standard.
1.2 Supplementary information on chemical resistance, im- 1.9 This international standard was developed in accor-
pact resistance, and installation practice are provided in Ap- dance with internationally recognized principles on standard-
pendix X1. ization established in the Decision on Principles for the
1.3 The classification of these composite panels into classes Development of International Standards, Guides and Recom-
based on relative response to a laboratory test shall not be mendations issued by the World Trade Organization Technical
considered a fire-hazard classification. Barriers to Trade (TBT) Committee.

1.4 Laboratory flammability tests (Test Methods E84 and 2. Referenced Documents
D1929) applicable to this specification should be used to 2.1 ASTM Standards:2
measure and describe the properties of materials, products, or D374/D374M Test Methods for Thickness of Solid Electri-
assemblies in response to heat and flame under controlled cal Insulation
laboratory conditions and should not be used to describe or D618 Practice for Conditioning Plastics for Testing
appraise the fire hazard or conditions. However, results may be D883 Terminology Relating to Plastics
used as elements of a fire risk assessment which takes into D1600 Terminology for Abbreviated Terms Relating to Plas-
account all of the factors which are pertinent to an assessment tics
of the fire hazard of a particular end use. D1929 Test Method for Determining Ignition Temperature
1.5 The intent of this specification is to define the class, of Plastics
grade, and general laminate properties of the composite wall D2244 Practice for Calculation of Color Tolerances and
and ceiling liner panels in order to ensure a quality product Color Differences from Instrumentally Measured Color
which will perform in the intended application. This specifi- Coordinates
cation is not intended to restrict or limit technological changes E84 Test Method for Surface Burning Characteristics of
affecting performance when changes are agreed upon between Building Materials
the purchaser and manufacturer. E631 Terminology of Building Constructions
1.6 The values stated in inch-pound units are to be regarded 3. Terminology
as the standard. The values given in parentheses are provided
for information only. 3.1 General—Definitions are in accordance with Terminolo-
gies D883 and E631 and abbreviations with Terminology
1.7 The text of this specification references notes and D1600, unless otherwise indicated.
footnotes that provide explanatory material. These notes and
footnotes (excluding those in Tables and Figures) shall not be 3.2 Definitions of Terms Specific to This Standard:
considered as requirements of this specification. 3.2.1 camber, n—non-linearity of the long axis of a panel.
NOTE 2—In the process of water jet, knife, saw, or rotary shear
trimming of a continuous panel, sidewards motion of the panel through the
1
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.24 on Plastic Building
2
Products. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2017. Published September 2017. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1992. Last previous edition approved in 2012 as D5319 – 12. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5319-17. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D5319 − 17
cutting medium can be induced by imbalances in the system. The resulting provide lower smoke density or higher fire retardancy, catalyst
trim cuts, although maintaining parallelism between the long sides, may residues, stabilizers, pigments, dyes, filters, or other types of
describe a continuous curve, rather than a straight line along the long axis
of the panel. Imbalances in side-to-side cure rates or material distribution
reinforcing fibers.
may also produce this phenomenon. This curvature of the long axis may
create problems with installation of the panel. Limits are placed on the 6. Physical Properties
degree of non-linearity to minimize those problems. 6.1 Size (Length and Width)—Tolerance for nominal length
4. Classification and width specified shall be 60.25 in. (6.35 mm). Panel
lengths over 12 ft (3.7 m) shall have a tolerance of 60.5 in.
4.1 The panels covered by this specification are divided into (12.7 mm) when measured in accordance with 8.2.
four classifications based on relative response to the laboratory
flammability of Test Method E84. 6.2 Squareness—Panels shall be within 0.125 in. (3.18 mm)
4.1.1 Class A—Flame spread index 0 to 25, smoke devel- of square when measured in accordance with 8.3.
opment index of 450 or less. 6.3 Thickness—Tolerance on the specified thickness shall be
4.1.2 Class B—Flame spread index 26 to 75, smoke devel- within 610 % when determined in accordance with 8.4.
opment index of 450 or less. 6.4 Camber—Tolerance on camber shall be 60.25 in. (6.35
4.1.3 Class C—Flame spread index 76 to 200, smoke mm) when determined in accordance with 8.5.
development index of 450 or less.
4.1.4 Class D—General purpose, no flame spread or smoke 6.5 Color—Color shall be as specified by the purchaser and
development indices. uniform throughout the sheet when examined in accordance
with 8.6.
NOTE 3—Refer to 1.3 on flammability testing and fire hazard classifi-
cation. 6.6 Ignition Properties—All panels shall have a minimum
4.2 These classifications may be further subdivided into self-ignition temperature of 650°F (343°C) when tested in
grades based on nominal thickness when tested in accordance accordance with Test Method D1929.
with 8.4: 6.7 All composite wall and ceiling liners shall have a USDA
4.2.1 Grade 1—0.027 to 0.033 in. (0.69 to 0.84 mm); 0.030 acceptance for incidental food contact.
in. nominal (0.76 mm).
4.2.2 Grade 2—0.036 to 0.044 in. (0.91 to 1.12 mm); 0.040 7. Workmanship
in. nominal (1.02 mm). 7.1 The composite shall conform to the nominal
4.2.3 Grade 3—0.040 to 0.050 in. (1.02 to 1.27 mm); 0.045 dimensions, shall be fully cured, and shall not contain major
in. nominal (1.14 mm). visual cracks, pinholes, foreign inclusions, or surface wrinkles
4.2.4 Grade 4—0.054 to 0.066 in. (1.37 to 1.68 mm); 0.060 that would impact or otherwise affect serviceability.
in. nominal (1.52 mm).
4.2.5 Grade 5—0.067 to 0.083 in. (1.70 to 2.11 mm); 0.075 8. Test Methods
in. nominal (1.91 mm). 8.1 Conditioning—Condition the test specimens in accor-
4.2.6 Grade 6—0.081 to 0.099 in. (2.06 to 2.51 mm); 0.090 dance with Procedure A of Method D618 where conditioning is
in. nominal (2.29 mm). required.
4.2.7 Grade 7—0.108 to 0.132 in. (2.74 to 3.35 mm); 0.120
in. nominal (3.05 mm). 8.2 Length and Width—Lay the panel on the flat surface and
measure with a steel tape. Measure the length on both sides and
4.3 Within the classification of grade and class of composite the center to the nearest 0.0625 in. (1.59 mm) and average the
panel described in this specification are commercial products three measurements. Measure the width at each end and in the
with the following variations as agreed upon between the center to the nearest 0.0625 in. and average the three measure-
purchaser and manufacturer. ments.
4.3.1 Size (Length and Width)—The nominal sizes available
are 23.75 in. (603.25 mm) to 120 in. (3048 mm) in width and 8.3 Squareness—Any type of jig that has two rails perpen-
47.75 in. (1212.85 mm) to 500 continuous feet of coil stock dicular to one another, each length at least equal to the length
(152 m) in length. of the side of the panel in contact with the rail, may be used to
4.3.2 Thickness—The nominal thicknesses available are determine squareness. Place the panels in the jig so that the
0.0303 in. (0.77 mm) to 0.120 in. (3.05 mm). longest edge of the panel touches the horizontal rail along the
4.3.3 Surface—The two most popular surfaces available are entire length, and the vertical edge (shorter edge) touches the
textured and smooth. vertical rail at some point along the entire length. Measure the
maximum distance between the vertical rail and the short edge
5. Materials of the panel at the corner opposite the one touching the rail.
5.1 The polyester resin used in the composite shall be a Measure to the nearest 0.0625 in. (1.6 mm). Rotate the panel
thermosetting polyester resin with cross-linking monomers 180° on the axis perpendicular to the face of the panel and
composed of polymeric esters in which the recurring ester repeat the test.
groups are an integral part of the main polymer chain. The resin 8.4 Thickness—Thickness readings shall be taken every 6
shall be reinforced with glass fibers. The polyester resin may in. (152 mm) across the width and along the length of the
contain additives for various purposes, such as additives to panel. Measurements shall be taken with a large foot

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D5319 − 17
micrometer, having an anvil size of 0.5 in. (12.7 mm) mini- 10. Certification
mum and accurate to 0.0001 in. (0.003 mm). Refer to Test 10.1 Manufacturers shall supply certification of compliance
Methods D374/D374M. Average all measurements for a final with this specification in the form of a statement appended or
value. affixed to invoices, or of labels affixed to panels or to
wrappings. In any form, the certification shall state as follows:
8.5 Camber—Lay the longest edge of the panel beside a
10.1.1 The name of the manufacturer,
straightedge on a flat surface with both ends touching the
10.1.2 The fact of conformance with this specification by
straight edge. If necessary, rotate the panel 180°. Measure the number designation: ASTM D5319,
greatest distance between the panel and the straightedge to the 10.1.3 The nominal weight per square foot (square metre) or
nearest 0.0625 in. (1.59 mm). nominal thickness,
8.6 Color—Examine the panel visually from a distance of 10.1.4 Type, and
10 ft (3 m) for color uniformity. Color tolerance may be 10.1.5 Grade.
checked using outdoor lighting or, in critical applications, a 11. Packaging and Package Marking
colorimeter using the Hunter L, a, b scale. Refer to Test 11.1 Packaging—The panels shall be packed in containers
Method D2244. Color tolerance shall be agreed upon between so constructed as to ensure acceptance by common or other
the purchaser and manufacturer. carriers for safe transportation to the point of delivery.
8.7 Burning Characteristics—Determine burning character- 11.2 Marking:
istics and smoke development values in accordance with Test 11.2.1 Shipping containers shall be marked as agreed upon
Method E84. between the purchaser and manufacturer.
11.2.2 Labels on individual panels shall include Specifica-
9. Retest and Rejection tion D5319, type, and grade.

9.1 If any panel fails to meet the agreed upon requirements, 12. Keywords
a second set of specimens shall be taken for retesting to 12.1 building construction; composite panels glass-fiber-
establish conformity in accordance with the agreement. reinforced polyester; laminates; wall and ceiling panels

APPENDIX

(Nonmandatory Information)

X1. SUPPLEMENTARY INFORMATION

X1.1 Chemical Resistance—Generally, glass-fiber- that Test Method D3029, Method G, be used and the values be
reinforced polyester plastic panels will provide satisfactory agreed upon between the purchaser and manufacturer prior to
service for long periods of time. However, exposure to chemi- purchase until the new method is developed.
cal atmospheres may cause greater color change and greater
X1.3 Installation Practice—The method of installation has
fiber exposure than exposure to normal conditions. Since it is
a bearing on the performance of the composite in use. Consult
impossible to describe all of the possible conditions of expo-
the manufacturer’s recommendation for their products. In
sure to chemical atmospheres, it is recommended that specific addition, a documentFiber Glass Reinforced Panel Council
exposure conditions be discussed with the panel manufacturer Installation Guide for On-Site Application of Wall and Ceiling
prior to purchase. Panels3 may be used.
X1.2 Impact Resistance—Work is presently underway to X1.4 Physical Properties—See Table X1.1.
develop a test method for impact resistance. Since there are
many methods in determining the impact resistance of glass- 3
Developed by the SPI Composites Institute, 355 Lexington Ave., New York,
fiber-reinforced polyester plastic panels, it is recommended NY 10017, April 1985.

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D5319 − 17
TABLE X1.1 Typical Physical Properties for Interior Wall and
Ceiling LinerA
ASTM Test
Property ValueB , psi
Method
Flexural strength 8 000 to 10 000 D790
Flexural modulus 0.3 to 0.5 × 106 D790
Tensile strength 6 000 to 8 000 D638
Compressive strength 13 000 to 16 000 D695
A
This table is for reference purposes only. The values shown in Table X1.1 reflect
the typical performance criteria for application on smooth solid-wall surfaces, for
example, plaster, gypsum board, poured concrete, concrete block, etc. Specialized
applications may require values other than those stated in Table Table X1.1. For
example, interior liner for cold storage may require higher values to minimize
possible product failure in extreme conditions.
B
For specific product values, refer to the manufacturers’ published literature. All
published physical property data shall report the test methods used to obtain the
specific data.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5319–12)
that may impact the use of this standard. (September 1, 2017)

(1) Section 2: Added D374M reference, this standard has been (5) Deleted 8.7, renumber 8.8 to 8.7.
reinstated. (6) Deleted old Section 9 (Inspection). Renumbered old Sec-
(2) Section 2: Deleted D3029 reference, standard has been tions 10 – 12 to 9 – 12.
withdrawn. (7) Reworded 9.1.
(3) Deleted 4.3.3, renumbered 4.3.4 to 4.3.3. (8) Reworded 10.1.
(4) Deleted 6.6, renumber 6.7 and 6.8

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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Designation: D5336 − 15a

Standard Classification System and Basis for Specification for


Polyphthalamide (PPA) Injection Molding Materials1
This standard is issued under the fixed designation D5336; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This classification system covers polyphthalamide ma- 2.1 ASTM Standards:2
terials suitable for injection molding. D256 Test Methods for Determining the Izod Pendulum
1.2 The properties included in this classification system are Impact Resistance of Plastics
those required to identify the compositions covered. Other D618 Practice for Conditioning Plastics for Testing
requirements necessary to identify particular characteristics D638 Test Method for Tensile Properties of Plastics
important to specialized applications are to be specified by D648 Test Method for Deflection Temperature of Plastics
using suffixes as given in Section 5. Under Flexural Load in the Edgewise Position
D790 Test Methods for Flexural Properties of Unreinforced
1.3 This classification system allows for the use of recycled and Reinforced Plastics and Electrical Insulating Materi-
materials provided that all specification requirements are met. als
1.4 This classification system is intended to be a means of D792 Test Methods for Density and Specific Gravity (Rela-
calling out plastics materials used in the fabrication of end tive Density) of Plastics by Displacement
items or parts. It is not intended for the selection of materials. D883 Terminology Relating to Plastics
Material selection can be made by those having expertise in the D1600 Terminology for Abbreviated Terms Relating to Plas-
plastics field only after careful consideration of the design and tics
the performance required of the part, the environment to which D2857 Practice for Dilute Solution Viscosity of Polymers
it will be exposed, the fabrication process to be employed, the D3418 Test Method for Transition Temperatures and En-
costs involved, and the inherent properties of the material other thalpies of Fusion and Crystallization of Polymers by
than those covered by this classification system. Differential Scanning Calorimetry
1.5 The values stated in SI units are to be regarded as the D3641 Practice for Injection Molding Test Specimens of
standard (see IEEE/ASTM SI-10). The values given in paren- Thermoplastic Molding and Extrusion Materials
theses are for information only. D3801 Test Method for Measuring the Comparative Burning
Characteristics of Solid Plastics in a Vertical Position
1.6 The following precautionary caveat pertains only to the D3835 Test Method for Determination of Properties of
test methods portion, Section 11, of this classification system: Polymeric Materials by Means of a Capillary Rheometer
This standard does not purport to address all of the safety D3892 Practice for Packaging/Packing of Plastics
concerns, if any, associated with its use. It is the responsibility D4000 Classification System for Specifying Plastic Materi-
of the user of this standard to establish appropriate safety and als
health practices and determine the applicability of regulatory D5225 Test Method for Measuring Solution Viscosity of
limitations prior to use. Specific precautionary statements are Polymers with a Differential Viscometer
given in 11.7.1. D5630 Test Method for Ash Content in Plastics
NOTE 1—There is no known ISO equivalent to this standard. D6869 Test Method for Coulometric and Volumetric Deter-
mination of Moisture in Plastics Using the Karl Fischer
1
Reaction (the Reaction of Iodine with Water)
This standard is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials
2
(Section D20.15.09). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2015. Published October 2015. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1992. Last previous edition approved in 2015 as D5336 - 15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5336-15A. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D5336 − 15a
D7209 Guide for Waste Reduction, Resource Recovery, and 3.2 Definitions of Terms Specific to This Standard:
Use of Recycled Polymeric Materials and Products (With- 3.2.1 polyphthalamide, PPA, n—a polyamide in which resi-
drawn 2015)3 dues of terephthalic acid or isophthalic acid or a combination
E29 Practice for Using Significant Digits in Test Data to of the two comprise at least 55 molar percentage of the
Determine Conformance with Specifications dicarboxylic acid portion of the repeating structural units in the
IEEE/ASTM SI-10 Standard for Use of the International polymer chain.
System of Units (SI): The Modern Metric System
4. Classification
2.2 Underwriters Laboratories Standard:
UL94 Standard for Tests for Flammability of Plastic Mate- 4.1 The polyphthalamide materials are designated “PPA,” as
rials4 specified in Terminology D1600.
2.3 ISO Standards:5 4.2 Unreinforced polyphthalamide materials are classified
ISO 75-1 Determination of Temperature of Deflection into groups according to crystallinity. These groups are subdi-
Unnder Load – Part 1:General Test Methods vided into classes and grades as shown in Table PPA.
ISO 75-2 Determination of Temperature of Deflection
NOTE 2—An example of this classification system is as follows:
Unnder Load – Part 2: Plastics and Ebonite
The designation PPA0121 would indicate from Table PPA:
ISO 179-1 Determination of Charpy Impact Strength—Part
1: Non-Instrumented Impact Test PPA = Polyphthalamide as found in Terminology D1600
ISO 294-1 Injection Moulding of Test Specimens of Ther- 01 (Group) = Semicrystalline PPA
2 (Class) = Low-temperature molding material
moplastic Materials—Part 1: General Principles, 1 (Grade) = With the corresponding requirements shown in Table PPA
Multipurpose-Test Specimens and Bars
4.2.1 To facilitate the incorporation of future or special
ISO 527-1 Determination of Tensile Properties—Part 1:
materials, the “other/unspecified” category (00) for group, (0)
General Principles
for class, and (0) for grade is shown. The basic properties of the
ISO 527-2 Determination of Tensile Properties—Part 2:
material can be obtained from Table A as they apply.
Testing Conditions
ISO 3451-1 Determination of Ash General Methods 4.3 Reinforced and lubricated versions of the polyphthal-
ISO 3451-4 Determination of Ash, Polyamides amide materials are classified in accordance with Tables PPA
ISO 15512 Determination of Water Content and A, where Table PPA specifies the unreinforced material and
Table A the properties after the addition of reinforcements or
3. Terminology lubricants at the nominal level indicated (see 4.3.1).
3.1 Definitions—The terminology used in this classification NOTE 3—This part of the classification system uses the percent of
system is in accordance with Terminologies D883 and D1600. reinforcements or additives, or both, in the callout of the modified basic
material. The types and percentages of reinforcements and additives is
sometimes shown on the supplier’s technical data sheet. If necessary
3
The last approved version of this historical standard is referenced on additional callout of these reinforcements and additives can be accom-
www.astm.org. plished by use of the suffix of the system (see Section 5).
4
Available from Underwriters Laboratories (UL), 333 Pfingsten Rd., NOTE 4—Materials containing reinforcements or fillers, or both, at
Northbrook, IL 60062-2096, http://www.ul.com. nominal levels not in multiples of five are included in the nearest grade
5
Available from American National Standards Institute (ANSI), 25 W. 43rd St., designation. For example, a material with a nominal glass fiber level of
4th Floor, New York, NY 10036, http://www.ansi.org. 33 % is included with Grade G35.

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D5336 − 15a

TABLE PPA Requirements for Unreinforced Polyphthalamide Resins


Inherent Melting Glass
ViscosityA Temperature,B TransitionB ,
Group Description Class Description Grade Description dL/g °C Tg, °C
01 semicrystalline 1 high-temperature molding 1 0.80-1.06 305-320 115-130
2 0.70-1.00 315-330 115-130
PPA 0 Other
2 low-temperature molding 1 0.80-1.05 320-335 90-105
2 0.85-0.95 290-305 85-95
3 0.85-1.05 300-315 85-95
0 Other
0 Other 0 Other
00 Other 0 Other 0 Other
A
Practice D2857 or Test Method D5225 with conditions as specified in 11.7 of this classification system.
B
Test Method D3418 using a heating rate of 10°C/min.

TABLE A Detail Requirements of Special Reinforced PPAs Using ASTM Methods


NOTE—All mechanical properties are determined on dry-as-molded injection molded specimens.
Property 0 1 2 3 4 5 6 7 8 9
Inherent viscosity,A Test Method D2857, B 0.60 0.7 0.75 0.8 0.85 0.9 0.95 1 C

dL/g, min
Tensile strength, Test Method D638D , B
45 (6500) 75 (10 900) 90 (13 000) 100 (14 500) 135 (19 600) 200 (29 000) 230 (33 400) 255 (37 000) C

MPaE (psi), min


F B C
Flexural modulus, Test Method D790 , 1.5 (218) 2.5 (363) 3.0 (435) 5.5 (798) 6.5 (943) 10.0 (1450) 13.5 (1958) 15.0 (2175)
GPA (kpsi), min
G H B C
Izod impact, Test Method D256 J/m 20 (0.38) 40 (0.75) 60 (1.1) 90 (1.6) 100 (1.9) 350 (6.6) 500 (9.4) 650 (12.1)
(ft-lbf/in), min
B C
Deflection Temperature Test Method 100 125 160 185 210 235 260 285
D648I , °C, min
A
See 11.7 of this classification system for specific conditions.
B
Unspecified requirement.
C
Specific value must be given in call-out.
D
Test Method D638, Type I tensile bar. The speed of testing shall be as described in 11.2 of this classification system.
E
MPa × 145 = psi.
F
Test Method D790 with a 1-mm (0.05-in.)/min testing speed.
G
Test Methods D256, Test Method A.
H
J/m × 0.01873 = ft-lb/in.
I
Test Method D648, using 1820-kPa (264-psi) stress.

TABLE B Detail Requirements of Special Reinforced PPAs Using ISO Methods


NOTE—All mechanical properties are determined on dry-as-molded injection molded specimens.
Property 0 1 2 3 4 5 6 7 8 9
Tensile strength, ISO 527 MPa minA B
45 75 90 100 135 200 230 255 C

Tensile modulus, ISO 527 GPa minD B


1.5 3.5 5.5 7.5 9.5 12.0 14.0 18.0 C

Charpy, ISO 179-1, J/m2, minE B


2.0 4.0 5.5 7.5 9.0 11.0 13.0 15.0 C
B C
Deflection Temperature Under Load, 100 125 160 185 210 235 260 285
F
ISO 75-2 method Af, °C, min
B
To be determined
A
ISO 527, Type IA tensile bar. The speed of testing shall be as described in 12.2 of this classification system.
B
Unspecified requirement.
C
Specific value must be given in call-out.
D
ISO 527, Type 1A tensile bar. The Speed of testing shall be 1 mm/min.
E
ISO 179-1, Test specimen shall be taken from the center portion of multipurpose tensile bar.
F
ISO 75-2, The test specimen shall be taken from the center portion of the multipurpose tensile bar, 4 mm thick, and tested in the flatwise position.

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D5336 − 15a
4.3.1 Reinforced, filled, and lubricated variations of the PPA0121G33A56577
basic materials are identified by a single letter from Table 1 that
PPA0121 = Semicrystalline, low-temperature molding grade polyphthalamide
indicates the filler and/or reinforcement used and two digits to from Table PPA,
indicate the nominal quantity in percent by weight. A second G33 = Glass reinforced at 33 % nominal,
letter, from Table 1A, when desired, is used to indicate the form A = Table A property requirements,
5 = Inherent viscosity, min 0.85 dL/g,
or structure of the reinforcement and/or filler, but not used for 6 = Tensile strength, min 200 MPa,
functional mixtures. Thus, a letter designation G for glass, E 5 = Flexural modulus, min 6.5 GPa,
for beads or spheres or balls, and 33 for percent by weight, 7 = Izod impact, min 500 J/m,
7 = Deflection temperature, min 260°C, and
GE33, specifies a reinforced or filled material with 33 percent If no properties are specified, the designation would be PPA0121G33.
by weight in the form of glass beads, spheres or balls. The
reinforcement letter designations and associated tolerance 5. Suffixes
levels are shown in the previous table (1). Form and structure 5.1 When additional requirements are needed for the mate-
letter designations are shown in the following table (1A). rials covered in this classification system that are not covered
in Tables PPA, A, or B, then those requirements shall be
TABLE 1 Reinforcement-FillerA SymbolsB and Tolerances designated through the use of suffixes.
Symbol Material Tolerance (Based on 5.1.1 A list of suffixes found in Classification System D4000
the Total Mass) (Table 3) is useful for additional requirements as appropriate.
C Carbon or graphite fiber ±3 %
G Glass reinforced ±3 % 5.2 Flammability callouts were changed in 2007. Therefore
L Lubricants (for example, Depends upon the
PTFE, graphite) material and
callouts written before 2007 are different from those written in
process—To be 2007 and later.
specified 5.2.1 If the requirements for the polyphthalamide material
M Mineral ±3 %
R Combinations of ±3 % for the total
in 4.3.3 also included flammability requirements, the following
reinforcements or fillers, reinforcement or filler, example illustrates the call-out based on ASTM D4000-04:
or both or both
PPA0121G33A06577FL34
A
Ash content of filled and/or reinforced materials is to be determined using either
Test Method D5630 or ISO 3451-1 where applicable. PPA0121G33A06577 = Same as 4.3.3
B
Additional symbols will be added to this table as required. F = Flammability requirements
L = UL94 recognition required
3 = UL recognition at 0.80-mm min thickness
4 = UL rating 94V-0
TABLE 1A Symbols for the Form or Structure of Fillers and
Reinforcing Materials 5.2.2 The following example illustrates the call-out based
Symbol Form or Structure on ASTM D4000-07:
C Chips, cuttings
PPA0121G33A06577FF003
D Fines, powders
E Beads, spheres, balls
PPA0121G33A65770 = Same as 4.3.3
F Fiber
F = Flammability requirements
G Ground
F = Vertical burn rate by ASTM D3801 or UL 94V
H Whiskers
0 = Rating of designation V-0
K Knitted fabric
03 = 0.80 mm minimum specimen thickness
L Layer
M Mat (fabric, thick)
N Non-woven (fabric, thin) 6. General Requirements
P Paper 6.1 Basic requirements from Tables PPA and A or B, as they
R Roving
S Flake apply, are always in effect unless these requirements are
T Cord superseded by specific suffix requirements, which always take
V Veneer
W Woven fabric
precedence. Properties in Tables A and B supersede properties
Y Yarn in Table PPA when reinforced or filled materials are specified.
X Not specified
6.2 The material compositions shall be uniform and shall
conform to the requirements specified herein.
4.3.2 Tables A and B Detail Requirements—An identifying
number is made up of the letter “A” or “B,” depending on 7. Detail Requirements
whether ASTM or ISO test methods are used, and five digits 7.1 The materials shall conform to the requirements pre-
comprising the cell numbers in the order in which the proper- scribed in Tables PPA and A or B, and the suffix requirements
ties appear. as they apply.
4.3.2.1 Although the values listed in Tables A and B are 7.2 For the purpose of determining conformance, all speci-
necessary to include the range of properties available in fied limits for a specification (line callout) are absolute limits,
existing materials, this does not imply that every possible as defined in Practice E29.
combination of the properties exists or can be obtained. 7.2.1 With the absolute method, an observed value or a
4.3.3 An example of this classification system for a 33 % calculated value is not rounded, but is to be compared directly
glass-reinforced polyphthalamide material, using ASTM test to the specified limiting value. Conformance or nonconfor-
methods (Table A) is as follows: mance with the specification is based on this comparison.

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D5336 − 15a
8. Sampling NOTE 9—Test Method D648 and ISO 75-2 will probably yield different
heat distortion temperatures.
8.1 Sampling shall be statistically adequate to satisfy the
requirements of 12.4. A batch/lot of material shall be consid- 11.7 Inherent Viscosity (IV)—Test Method D2857 or D5225
ered as a unit of manufacture as prepared for shipment, and is with the following modifications:
permitted to consist of two or more “production runs” or 11.7.1 Solvent—Prepare a filtered solution containing a
batches. 60/40 weight percent of phenol/ tetrachloroethane (TCE).
(Warning—Phenol tetrachloroethane is a very dangerous sol-
9. Specimen Preparation vent. It is toxic by ingestion, inhalation, and absorption. Refer
to the appropriate material safety data sheet for information on
9.1 Mold test specimens by an injection molding process the proper handling of this material.)
(see Practice D3641 or ISO 294). Use the following conditions: 11.7.2 Sample Size—Use a sample size of 0.400 6 0.003 g
Class Grade Melt Temperature° C (°F) Mold Temperature min, °C (°F) of resin/100 mL of solvent. IV determinations are not recom-
1 1 325-335 (620-635) 135 (275)
2 335-345 (635-650) 135 (275)
mended for materials that contain fillers or reinforcements.
2 1 and 3 330-345 (625-650) 65 (150) However, if the sample does contain filler, select the appropri-
2 2 320-330 (605-625) 65 (150) ate sample size from the following table:
9.2 Materials used in the preparation of test specimens shall % Ash Sample Size, g
contain no more than 0.2 % moisture.
10 0.4444
NOTE 5—If the moisture content exceeds the limits previously stated, 20 0.5000
drying the material by methods such as at a temperature of 80 - 100°C in 25 0.5333
vacuum or in a stream, of nitrogen or in a desiccant bed dryer, or both, 30 0.5714
35 0.6154
until the moisture content is within the stated limits have been found to be
40 0.6666
satisfactory. 45 0.7273

10. Conditioning NOTE 10—A sample size to produce a resin concentration of 0.4
g/100mL shall be used. The sample sizes shown in the table were
10.1 Obtain test data using dry-as-molded specimens, de- calculated by the following equation:
fined as those that upon removal from the mold are immedi- 0.4
ately sealed in containers that are impermeable to water vapor. sample weight 5 3 100 (1)
100 2 % filler
Condition specimens a minimum of 2 h in sealed containers at
23 6 2°C prior to testing. 11.7.3 Dissolve the sample in the inherent viscosity (IV)
solvent by heating and stirring on a hot plate. Monitor the
NOTE 6—Physical properties of polyphthalamides are dependent upon
the moisture content of the molded item. Refer to the manufacturers’ temperature with a surface thermometer to be sure that it does
literature for details. not exceed 130°C.
10.2 Conduct tests, other than solution viscosity and those 11.7.4 If the sample contains a filler, it must be filtered to
conducted at elevated temperatures, in the standard laboratory remove the filler after all of the resin has dissolved.
atmosphere (see Practice D618) of 23 6 2°C and 50 6 10 % 11.7.5 Calculation:
relative humidity. Do not remove individual specimens from IV 5 ln~ S t /B t ! /C (2)
sealed containers until immediately before testing. where:
NOTE 7—The tolerance specified is the maximum allowed variation IV = inherent viscosity at 30°C, dL/g,
around the set points. It is not to be taken as the range of acceptable set St = average sample flow time, s,
points. Bt = average blank flow time, s, and
C = polymer concentration, g/dl.
11. Test Methods
11.8 Moisture—Test methods D6869 or ISO 15512, Method
11.1 Determine the properties enumerated in this classifica- B.
tion system by means of test methods referenced.
11.2 Tensile Strength—Test Method D638, using a Type I 12. Inspection and Certification
test specimen or ISO 527, using Type 1A specimens. A testing 12.1 Inspection and certification of the materials supplied
speed of 5 mm (0.2 in.)/min or 50 mm (2.0 in.)/min if with reference to a specification based on this classification
elongation exceeds 10 %. system shall be for conformance to the requirements specified
NOTE 8—ASTM D638 and ISO 527 could yield different results. herein.
11.3 Flexural Strength—Test Methods D790, using a testing 12.2 Lot acceptance inspection shall be the basis on which
speed of 1 mm (0.05 in.)/min. acceptance or rejection of a lot is made. The lot acceptance
11.4 Izod Impact—Test Methods D256, Test Method A. inspection shall consist of the following tests that ensure
process control during manufacturing as well as those neces-
11.5 Charpy Impact—ISO 179-1, Method 1eA sary to ensure certifiability in accordance with 12.4.
11.6 Deflection Temperature—Test Method D648, using a 12.2.1 Inherent viscosity only for unreinforced or unfilled
maximum outer fiber stress of 1.82 Mpa (264 psi), or ISO 75-2, polymer as described in Table PPA.
Method Af with a specimen height of 4.0 mm. 12.2.2 Moisture content, and

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D5336 − 15a
12.2.3 Filler content (see Test Method D5630 or ISO 3451), detailed information about statistical process control.
when applicable. 12.5 A report of test results shall be furnished when re-
12.3 A periodic check inspection shall consist of the tests quested. The report shall consist of results of the lot-acceptance
specified for all requirements of the materials under this inspection for the shipment, the percent by weight of recycled
classification system. Inspection frequency shall be adequate to plastic, as defined in 3.1.47 of Guide D7209, if requested, and
ensure the material is certifiable in accordance with 12.4. the results of the most recent periodic-check inspection.
12.4 Certification shall be that the material was 13. Packaging and Marking
manufactured, by a process in statistical control, sampled, 13.1 For packing, packaging, and practice marking, the
tested, and inspected in accordance with this classification provisions of Practice D3892 apply.
system, and that the average values for the lot meet the
requirements of the specification (line callout). 14. Keywords
NOTE 11—The ASTM publication, Manual on Presentation of Data and 14.1 inherent viscosity; line call-out; moisture analysis;
Control chart Analysis, 7th Edition, Stock number MNL7A, provides molding material; plastic; polyphthalamide

APPENDIX

(Nonmandatory Information)

X1. CALCULATION FOR VISCOSITY NUMBER (VN)

X1.1 Viscosity number (VN) is defined as the ratio of the To further elaborate on the situation where the IV is known
viscosities of the (dilute) solution of the polymer to the and the VN needs to be calculated, we note that 11.7.5 by the
viscosity of the solvent divided by the concentration of the equation: IV = ln (St / Bt) / C.
polymer in the solvent. In this instance efflux time (t) can be This can be re-arranged to: (St / Bt) = e(C × IV)
substituted for viscosity (ɳ). Substituting in the VN equation, this leads to:
VN = (e(C × IV) – 1 / C)
VN 5 ~~ t 2 t c ⁄ t o 2 t oc ! 2 1 ! ⁄C (0)
Using the above relation for C = 0.4 of PCTE as used in 11.7
VN = viscosity number, of this standard, leads to following correlation table (Table
t = flow time of the sample, X1.1).
tc = Hagenbach correction of the solution,
to = flow time of the solvent, TABLE X1.1 Correlation Table
toc = Hagenbach correction of the solvent, and
IV VN IV VN IV VN IV VN
C = polymer concentration. 0.70 81 0.82 97 0.94 114 1.06 132
0.71 82 0.83 98 0.95 116 1.07 134
Assuming the correction factors for the solution and solvent 0.72 83 0.84 100 0.96 117 1.08 135
approach zero the equation becomes, 0.73 85 0.85 101 0.97 119 1.09 137
VN = ((t / to) – 1) / C, or when using the symbols as in 11.7.5 0.74 86 0.86 103 0.98 120 1.10 138
0.75 87 0.87 104 0.99 121 1.11 140
of this standard, 0.76 89 0.88 105 1.00 123 1.12 141
0.77 90 0.89 107 1.01 124 1.13 143
VN 5 ~~ S t ⁄ B t ! 2 1 ! ⁄C (0)
0.78 92 0.90 108 1.02 126 1.14 144
0.79 93 0.91 110 1.03 127 1.15 146
VN = viscosity number, 0.80 94 0.92 111 1.04 129 1.16 148
St = average sample flow time, 0.81 96 0.93 113 1.05 130 1.17 149
Bt = average solvent flow time, and NOTE: Using a different concentration or a different solvent would change the
results.
C = polymer concentration.

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SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5336 - 15)
that may impact the use of this standard. (October 1, 2015)

(1) Added Guide D7209 to 2.1. (5) Added Table 1A.


(2) Revised Table 1. (6) Deleted 4.3.1.1, which is now included in 4.3.1.
(3) Added Note 3, Note 4, and Note 7, and subsequent notes (7) Revised 12.5.
were renumbered. (8) Added Appendix X1.
(4) Revised 4.3. (9) Some editorial changes were made.

Committee D20 has identified the location of selected changes to this standard since the last issue (D5336 - 09)
that may impact the use of this standard. (April 1, 2015)

(1) This five year review included editorial changes. (4) Deleted old Section 7. The requirements in old Section 7
(2) The title was changed. are now included in Section 6 and the new Section 7.
(3) Added Note 5 and renumbered subsequent notes. Renumbered subsequent sections.

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of infringement of such rights, are entirely their own responsibility.

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Designation: D5336 − 15a

Standard Classification System and Basis for Specification for


Polyphthalamide (PPA) Injection Molding Materials1
This standard is issued under the fixed designation D5336; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This classification system covers polyphthalamide ma- 2.1 ASTM Standards:2
terials suitable for injection molding. D256 Test Methods for Determining the Izod Pendulum
1.2 The properties included in this classification system are Impact Resistance of Plastics
those required to identify the compositions covered. Other D618 Practice for Conditioning Plastics for Testing
requirements necessary to identify particular characteristics D638 Test Method for Tensile Properties of Plastics
important to specialized applications are to be specified by D648 Test Method for Deflection Temperature of Plastics
using suffixes as given in Section 5. Under Flexural Load in the Edgewise Position
D790 Test Methods for Flexural Properties of Unreinforced
1.3 This classification system allows for the use of recycled and Reinforced Plastics and Electrical Insulating Materi-
materials provided that all specification requirements are met. als
1.4 This classification system is intended to be a means of D792 Test Methods for Density and Specific Gravity (Rela-
calling out plastics materials used in the fabrication of end tive Density) of Plastics by Displacement
items or parts. It is not intended for the selection of materials. D883 Terminology Relating to Plastics
Material selection can be made by those having expertise in the D1600 Terminology for Abbreviated Terms Relating to Plas-
plastics field only after careful consideration of the design and tics
the performance required of the part, the environment to which D2857 Practice for Dilute Solution Viscosity of Polymers
it will be exposed, the fabrication process to be employed, the D3418 Test Method for Transition Temperatures and En-
costs involved, and the inherent properties of the material other thalpies of Fusion and Crystallization of Polymers by
than those covered by this classification system. Differential Scanning Calorimetry
1.5 The values stated in SI units are to be regarded as the D3641 Practice for Injection Molding Test Specimens of
standard (see IEEE/ASTM SI-10). The values given in paren- Thermoplastic Molding and Extrusion Materials
theses are for information only. D3801 Test Method for Measuring the Comparative Burning
Characteristics of Solid Plastics in a Vertical Position
1.6 The following precautionary caveat pertains only to the D3835 Test Method for Determination of Properties of
test methods portion, Section 11, of this classification system: Polymeric Materials by Means of a Capillary Rheometer
This standard does not purport to address all of the safety D3892 Practice for Packaging/Packing of Plastics
concerns, if any, associated with its use. It is the responsibility D4000 Classification System for Specifying Plastic Materi-
of the user of this standard to establish appropriate safety and als
health practices and determine the applicability of regulatory D5225 Test Method for Measuring Solution Viscosity of
limitations prior to use. Specific precautionary statements are Polymers with a Differential Viscometer
given in 11.7.1. D5630 Test Method for Ash Content in Plastics
NOTE 1—There is no known ISO equivalent to this standard. D6869 Test Method for Coulometric and Volumetric Deter-
mination of Moisture in Plastics Using the Karl Fischer
1
Reaction (the Reaction of Iodine with Water)
This standard is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials
2
(Section D20.15.09). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2015. Published October 2015. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1992. Last previous edition approved in 2015 as D5336 - 15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5336-15A. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D5336 − 15a
D7209 Guide for Waste Reduction, Resource Recovery, and 3.2 Definitions of Terms Specific to This Standard:
Use of Recycled Polymeric Materials and Products (With- 3.2.1 polyphthalamide, PPA, n—a polyamide in which resi-
drawn 2015)3 dues of terephthalic acid or isophthalic acid or a combination
E29 Practice for Using Significant Digits in Test Data to of the two comprise at least 55 molar percentage of the
Determine Conformance with Specifications dicarboxylic acid portion of the repeating structural units in the
IEEE/ASTM SI-10 Standard for Use of the International polymer chain.
System of Units (SI): The Modern Metric System
4. Classification
2.2 Underwriters Laboratories Standard:
UL94 Standard for Tests for Flammability of Plastic Mate- 4.1 The polyphthalamide materials are designated “PPA,” as
rials4 specified in Terminology D1600.
2.3 ISO Standards:5 4.2 Unreinforced polyphthalamide materials are classified
ISO 75-1 Determination of Temperature of Deflection into groups according to crystallinity. These groups are subdi-
Unnder Load – Part 1:General Test Methods vided into classes and grades as shown in Table PPA.
ISO 75-2 Determination of Temperature of Deflection
NOTE 2—An example of this classification system is as follows:
Unnder Load – Part 2: Plastics and Ebonite
The designation PPA0121 would indicate from Table PPA:
ISO 179-1 Determination of Charpy Impact Strength—Part
1: Non-Instrumented Impact Test PPA = Polyphthalamide as found in Terminology D1600
ISO 294-1 Injection Moulding of Test Specimens of Ther- 01 (Group) = Semicrystalline PPA
2 (Class) = Low-temperature molding material
moplastic Materials—Part 1: General Principles, 1 (Grade) = With the corresponding requirements shown in Table PPA
Multipurpose-Test Specimens and Bars
4.2.1 To facilitate the incorporation of future or special
ISO 527-1 Determination of Tensile Properties—Part 1:
materials, the “other/unspecified” category (00) for group, (0)
General Principles
for class, and (0) for grade is shown. The basic properties of the
ISO 527-2 Determination of Tensile Properties—Part 2:
material can be obtained from Table A as they apply.
Testing Conditions
ISO 3451-1 Determination of Ash General Methods 4.3 Reinforced and lubricated versions of the polyphthal-
ISO 3451-4 Determination of Ash, Polyamides amide materials are classified in accordance with Tables PPA
ISO 15512 Determination of Water Content and A, where Table PPA specifies the unreinforced material and
Table A the properties after the addition of reinforcements or
3. Terminology lubricants at the nominal level indicated (see 4.3.1).
3.1 Definitions—The terminology used in this classification NOTE 3—This part of the classification system uses the percent of
system is in accordance with Terminologies D883 and D1600. reinforcements or additives, or both, in the callout of the modified basic
material. The types and percentages of reinforcements and additives is
sometimes shown on the supplier’s technical data sheet. If necessary
3
The last approved version of this historical standard is referenced on additional callout of these reinforcements and additives can be accom-
www.astm.org. plished by use of the suffix of the system (see Section 5).
4
Available from Underwriters Laboratories (UL), 333 Pfingsten Rd., NOTE 4—Materials containing reinforcements or fillers, or both, at
Northbrook, IL 60062-2096, http://www.ul.com. nominal levels not in multiples of five are included in the nearest grade
5
Available from American National Standards Institute (ANSI), 25 W. 43rd St., designation. For example, a material with a nominal glass fiber level of
4th Floor, New York, NY 10036, http://www.ansi.org. 33 % is included with Grade G35.

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D5336 − 15a

TABLE PPA Requirements for Unreinforced Polyphthalamide Resins


Inherent Melting Glass
ViscosityA Temperature,B TransitionB ,
Group Description Class Description Grade Description dL/g °C Tg, °C
01 semicrystalline 1 high-temperature molding 1 0.80-1.06 305-320 115-130
2 0.70-1.00 315-330 115-130
PPA 0 Other
2 low-temperature molding 1 0.80-1.05 320-335 90-105
2 0.85-0.95 290-305 85-95
3 0.85-1.05 300-315 85-95
0 Other
0 Other 0 Other
00 Other 0 Other 0 Other
A
Practice D2857 or Test Method D5225 with conditions as specified in 11.7 of this classification system.
B
Test Method D3418 using a heating rate of 10°C/min.

TABLE A Detail Requirements of Special Reinforced PPAs Using ASTM Methods


NOTE—All mechanical properties are determined on dry-as-molded injection molded specimens.
Property 0 1 2 3 4 5 6 7 8 9
Inherent viscosity,A Test Method D2857, B 0.60 0.7 0.75 0.8 0.85 0.9 0.95 1 C

dL/g, min
Tensile strength, Test Method D638D , B
45 (6500) 75 (10 900) 90 (13 000) 100 (14 500) 135 (19 600) 200 (29 000) 230 (33 400) 255 (37 000) C

MPaE (psi), min


F B C
Flexural modulus, Test Method D790 , 1.5 (218) 2.5 (363) 3.0 (435) 5.5 (798) 6.5 (943) 10.0 (1450) 13.5 (1958) 15.0 (2175)
GPA (kpsi), min
G H B C
Izod impact, Test Method D256 J/m 20 (0.38) 40 (0.75) 60 (1.1) 90 (1.6) 100 (1.9) 350 (6.6) 500 (9.4) 650 (12.1)
(ft-lbf/in), min
B C
Deflection Temperature Test Method 100 125 160 185 210 235 260 285
D648I , °C, min
A
See 11.7 of this classification system for specific conditions.
B
Unspecified requirement.
C
Specific value must be given in call-out.
D
Test Method D638, Type I tensile bar. The speed of testing shall be as described in 11.2 of this classification system.
E
MPa × 145 = psi.
F
Test Method D790 with a 1-mm (0.05-in.)/min testing speed.
G
Test Methods D256, Test Method A.
H
J/m × 0.01873 = ft-lb/in.
I
Test Method D648, using 1820-kPa (264-psi) stress.

TABLE B Detail Requirements of Special Reinforced PPAs Using ISO Methods


NOTE—All mechanical properties are determined on dry-as-molded injection molded specimens.
Property 0 1 2 3 4 5 6 7 8 9
Tensile strength, ISO 527 MPa minA B
45 75 90 100 135 200 230 255 C

Tensile modulus, ISO 527 GPa minD B


1.5 3.5 5.5 7.5 9.5 12.0 14.0 18.0 C

Charpy, ISO 179-1, J/m2, minE B


2.0 4.0 5.5 7.5 9.0 11.0 13.0 15.0 C
B C
Deflection Temperature Under Load, 100 125 160 185 210 235 260 285
F
ISO 75-2 method Af, °C, min
B
To be determined
A
ISO 527, Type IA tensile bar. The speed of testing shall be as described in 12.2 of this classification system.
B
Unspecified requirement.
C
Specific value must be given in call-out.
D
ISO 527, Type 1A tensile bar. The Speed of testing shall be 1 mm/min.
E
ISO 179-1, Test specimen shall be taken from the center portion of multipurpose tensile bar.
F
ISO 75-2, The test specimen shall be taken from the center portion of the multipurpose tensile bar, 4 mm thick, and tested in the flatwise position.

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D5336 − 15a
4.3.1 Reinforced, filled, and lubricated variations of the PPA0121G33A56577
basic materials are identified by a single letter from Table 1 that
PPA0121 = Semicrystalline, low-temperature molding grade polyphthalamide
indicates the filler and/or reinforcement used and two digits to from Table PPA,
indicate the nominal quantity in percent by weight. A second G33 = Glass reinforced at 33 % nominal,
letter, from Table 1A, when desired, is used to indicate the form A = Table A property requirements,
5 = Inherent viscosity, min 0.85 dL/g,
or structure of the reinforcement and/or filler, but not used for 6 = Tensile strength, min 200 MPa,
functional mixtures. Thus, a letter designation G for glass, E 5 = Flexural modulus, min 6.5 GPa,
for beads or spheres or balls, and 33 for percent by weight, 7 = Izod impact, min 500 J/m,
7 = Deflection temperature, min 260°C, and
GE33, specifies a reinforced or filled material with 33 percent If no properties are specified, the designation would be PPA0121G33.
by weight in the form of glass beads, spheres or balls. The
reinforcement letter designations and associated tolerance 5. Suffixes
levels are shown in the previous table (1). Form and structure 5.1 When additional requirements are needed for the mate-
letter designations are shown in the following table (1A). rials covered in this classification system that are not covered
in Tables PPA, A, or B, then those requirements shall be
TABLE 1 Reinforcement-FillerA SymbolsB and Tolerances designated through the use of suffixes.
Symbol Material Tolerance (Based on 5.1.1 A list of suffixes found in Classification System D4000
the Total Mass) (Table 3) is useful for additional requirements as appropriate.
C Carbon or graphite fiber ±3 %
G Glass reinforced ±3 % 5.2 Flammability callouts were changed in 2007. Therefore
L Lubricants (for example, Depends upon the
PTFE, graphite) material and
callouts written before 2007 are different from those written in
process—To be 2007 and later.
specified 5.2.1 If the requirements for the polyphthalamide material
M Mineral ±3 %
R Combinations of ±3 % for the total
in 4.3.3 also included flammability requirements, the following
reinforcements or fillers, reinforcement or filler, example illustrates the call-out based on ASTM D4000-04:
or both or both
PPA0121G33A06577FL34
A
Ash content of filled and/or reinforced materials is to be determined using either
Test Method D5630 or ISO 3451-1 where applicable. PPA0121G33A06577 = Same as 4.3.3
B
Additional symbols will be added to this table as required. F = Flammability requirements
L = UL94 recognition required
3 = UL recognition at 0.80-mm min thickness
4 = UL rating 94V-0
TABLE 1A Symbols for the Form or Structure of Fillers and
Reinforcing Materials 5.2.2 The following example illustrates the call-out based
Symbol Form or Structure on ASTM D4000-07:
C Chips, cuttings
PPA0121G33A06577FF003
D Fines, powders
E Beads, spheres, balls
PPA0121G33A65770 = Same as 4.3.3
F Fiber
F = Flammability requirements
G Ground
F = Vertical burn rate by ASTM D3801 or UL 94V
H Whiskers
0 = Rating of designation V-0
K Knitted fabric
03 = 0.80 mm minimum specimen thickness
L Layer
M Mat (fabric, thick)
N Non-woven (fabric, thin) 6. General Requirements
P Paper 6.1 Basic requirements from Tables PPA and A or B, as they
R Roving
S Flake apply, are always in effect unless these requirements are
T Cord superseded by specific suffix requirements, which always take
V Veneer
W Woven fabric
precedence. Properties in Tables A and B supersede properties
Y Yarn in Table PPA when reinforced or filled materials are specified.
X Not specified
6.2 The material compositions shall be uniform and shall
conform to the requirements specified herein.
4.3.2 Tables A and B Detail Requirements—An identifying
number is made up of the letter “A” or “B,” depending on 7. Detail Requirements
whether ASTM or ISO test methods are used, and five digits 7.1 The materials shall conform to the requirements pre-
comprising the cell numbers in the order in which the proper- scribed in Tables PPA and A or B, and the suffix requirements
ties appear. as they apply.
4.3.2.1 Although the values listed in Tables A and B are 7.2 For the purpose of determining conformance, all speci-
necessary to include the range of properties available in fied limits for a specification (line callout) are absolute limits,
existing materials, this does not imply that every possible as defined in Practice E29.
combination of the properties exists or can be obtained. 7.2.1 With the absolute method, an observed value or a
4.3.3 An example of this classification system for a 33 % calculated value is not rounded, but is to be compared directly
glass-reinforced polyphthalamide material, using ASTM test to the specified limiting value. Conformance or nonconfor-
methods (Table A) is as follows: mance with the specification is based on this comparison.

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D5336 − 15a
8. Sampling NOTE 9—Test Method D648 and ISO 75-2 will probably yield different
heat distortion temperatures.
8.1 Sampling shall be statistically adequate to satisfy the
requirements of 12.4. A batch/lot of material shall be consid- 11.7 Inherent Viscosity (IV)—Test Method D2857 or D5225
ered as a unit of manufacture as prepared for shipment, and is with the following modifications:
permitted to consist of two or more “production runs” or 11.7.1 Solvent—Prepare a filtered solution containing a
batches. 60/40 weight percent of phenol/ tetrachloroethane (TCE).
(Warning—Phenol tetrachloroethane is a very dangerous sol-
9. Specimen Preparation vent. It is toxic by ingestion, inhalation, and absorption. Refer
to the appropriate material safety data sheet for information on
9.1 Mold test specimens by an injection molding process the proper handling of this material.)
(see Practice D3641 or ISO 294). Use the following conditions: 11.7.2 Sample Size—Use a sample size of 0.400 6 0.003 g
Class Grade Melt Temperature° C (°F) Mold Temperature min, °C (°F) of resin/100 mL of solvent. IV determinations are not recom-
1 1 325-335 (620-635) 135 (275)
2 335-345 (635-650) 135 (275)
mended for materials that contain fillers or reinforcements.
2 1 and 3 330-345 (625-650) 65 (150) However, if the sample does contain filler, select the appropri-
2 2 320-330 (605-625) 65 (150) ate sample size from the following table:
9.2 Materials used in the preparation of test specimens shall % Ash Sample Size, g
contain no more than 0.2 % moisture.
10 0.4444
NOTE 5—If the moisture content exceeds the limits previously stated, 20 0.5000
drying the material by methods such as at a temperature of 80 - 100°C in 25 0.5333
vacuum or in a stream, of nitrogen or in a desiccant bed dryer, or both, 30 0.5714
35 0.6154
until the moisture content is within the stated limits have been found to be
40 0.6666
satisfactory. 45 0.7273

10. Conditioning NOTE 10—A sample size to produce a resin concentration of 0.4
g/100mL shall be used. The sample sizes shown in the table were
10.1 Obtain test data using dry-as-molded specimens, de- calculated by the following equation:
fined as those that upon removal from the mold are immedi- 0.4
ately sealed in containers that are impermeable to water vapor. sample weight 5 3 100 (1)
100 2 % filler
Condition specimens a minimum of 2 h in sealed containers at
23 6 2°C prior to testing. 11.7.3 Dissolve the sample in the inherent viscosity (IV)
solvent by heating and stirring on a hot plate. Monitor the
NOTE 6—Physical properties of polyphthalamides are dependent upon
the moisture content of the molded item. Refer to the manufacturers’ temperature with a surface thermometer to be sure that it does
literature for details. not exceed 130°C.
10.2 Conduct tests, other than solution viscosity and those 11.7.4 If the sample contains a filler, it must be filtered to
conducted at elevated temperatures, in the standard laboratory remove the filler after all of the resin has dissolved.
atmosphere (see Practice D618) of 23 6 2°C and 50 6 10 % 11.7.5 Calculation:
relative humidity. Do not remove individual specimens from IV 5 ln~ S t /B t ! /C (2)
sealed containers until immediately before testing. where:
NOTE 7—The tolerance specified is the maximum allowed variation IV = inherent viscosity at 30°C, dL/g,
around the set points. It is not to be taken as the range of acceptable set St = average sample flow time, s,
points. Bt = average blank flow time, s, and
C = polymer concentration, g/dl.
11. Test Methods
11.8 Moisture—Test methods D6869 or ISO 15512, Method
11.1 Determine the properties enumerated in this classifica- B.
tion system by means of test methods referenced.
11.2 Tensile Strength—Test Method D638, using a Type I 12. Inspection and Certification
test specimen or ISO 527, using Type 1A specimens. A testing 12.1 Inspection and certification of the materials supplied
speed of 5 mm (0.2 in.)/min or 50 mm (2.0 in.)/min if with reference to a specification based on this classification
elongation exceeds 10 %. system shall be for conformance to the requirements specified
NOTE 8—ASTM D638 and ISO 527 could yield different results. herein.
11.3 Flexural Strength—Test Methods D790, using a testing 12.2 Lot acceptance inspection shall be the basis on which
speed of 1 mm (0.05 in.)/min. acceptance or rejection of a lot is made. The lot acceptance
11.4 Izod Impact—Test Methods D256, Test Method A. inspection shall consist of the following tests that ensure
process control during manufacturing as well as those neces-
11.5 Charpy Impact—ISO 179-1, Method 1eA sary to ensure certifiability in accordance with 12.4.
11.6 Deflection Temperature—Test Method D648, using a 12.2.1 Inherent viscosity only for unreinforced or unfilled
maximum outer fiber stress of 1.82 Mpa (264 psi), or ISO 75-2, polymer as described in Table PPA.
Method Af with a specimen height of 4.0 mm. 12.2.2 Moisture content, and

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D5336 − 15a
12.2.3 Filler content (see Test Method D5630 or ISO 3451), detailed information about statistical process control.
when applicable. 12.5 A report of test results shall be furnished when re-
12.3 A periodic check inspection shall consist of the tests quested. The report shall consist of results of the lot-acceptance
specified for all requirements of the materials under this inspection for the shipment, the percent by weight of recycled
classification system. Inspection frequency shall be adequate to plastic, as defined in 3.1.47 of Guide D7209, if requested, and
ensure the material is certifiable in accordance with 12.4. the results of the most recent periodic-check inspection.
12.4 Certification shall be that the material was 13. Packaging and Marking
manufactured, by a process in statistical control, sampled, 13.1 For packing, packaging, and practice marking, the
tested, and inspected in accordance with this classification provisions of Practice D3892 apply.
system, and that the average values for the lot meet the
requirements of the specification (line callout). 14. Keywords
NOTE 11—The ASTM publication, Manual on Presentation of Data and 14.1 inherent viscosity; line call-out; moisture analysis;
Control chart Analysis, 7th Edition, Stock number MNL7A, provides molding material; plastic; polyphthalamide

APPENDIX

(Nonmandatory Information)

X1. CALCULATION FOR VISCOSITY NUMBER (VN)

X1.1 Viscosity number (VN) is defined as the ratio of the To further elaborate on the situation where the IV is known
viscosities of the (dilute) solution of the polymer to the and the VN needs to be calculated, we note that 11.7.5 by the
viscosity of the solvent divided by the concentration of the equation: IV = ln (St / Bt) / C.
polymer in the solvent. In this instance efflux time (t) can be This can be re-arranged to: (St / Bt) = e(C × IV)
substituted for viscosity (ɳ). Substituting in the VN equation, this leads to:
VN = (e(C × IV) – 1 / C)
VN 5 ~~ t 2 t c ⁄ t o 2 t oc ! 2 1 ! ⁄C (0)
Using the above relation for C = 0.4 of PCTE as used in 11.7
VN = viscosity number, of this standard, leads to following correlation table (Table
t = flow time of the sample, X1.1).
tc = Hagenbach correction of the solution,
to = flow time of the solvent, TABLE X1.1 Correlation Table
toc = Hagenbach correction of the solvent, and
IV VN IV VN IV VN IV VN
C = polymer concentration. 0.70 81 0.82 97 0.94 114 1.06 132
0.71 82 0.83 98 0.95 116 1.07 134
Assuming the correction factors for the solution and solvent 0.72 83 0.84 100 0.96 117 1.08 135
approach zero the equation becomes, 0.73 85 0.85 101 0.97 119 1.09 137
VN = ((t / to) – 1) / C, or when using the symbols as in 11.7.5 0.74 86 0.86 103 0.98 120 1.10 138
0.75 87 0.87 104 0.99 121 1.11 140
of this standard, 0.76 89 0.88 105 1.00 123 1.12 141
0.77 90 0.89 107 1.01 124 1.13 143
VN 5 ~~ S t ⁄ B t ! 2 1 ! ⁄C (0)
0.78 92 0.90 108 1.02 126 1.14 144
0.79 93 0.91 110 1.03 127 1.15 146
VN = viscosity number, 0.80 94 0.92 111 1.04 129 1.16 148
St = average sample flow time, 0.81 96 0.93 113 1.05 130 1.17 149
Bt = average solvent flow time, and NOTE: Using a different concentration or a different solvent would change the
results.
C = polymer concentration.

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SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5336 - 15)
that may impact the use of this standard. (October 1, 2015)

(1) Added Guide D7209 to 2.1. (5) Added Table 1A.


(2) Revised Table 1. (6) Deleted 4.3.1.1, which is now included in 4.3.1.
(3) Added Note 3, Note 4, and Note 7, and subsequent notes (7) Revised 12.5.
were renumbered. (8) Added Appendix X1.
(4) Revised 4.3. (9) Some editorial changes were made.

Committee D20 has identified the location of selected changes to this standard since the last issue (D5336 - 09)
that may impact the use of this standard. (April 1, 2015)

(1) This five year review included editorial changes. (4) Deleted old Section 7. The requirements in old Section 7
(2) The title was changed. are now included in Section 6 and the new Section 7.
(3) Added Note 5 and renumbered subsequent notes. Renumbered subsequent sections.

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5364 − 14 (Reapproved 2019)

Standard Guide for


Design, Fabrication, and Erection of Fiberglass Reinforced
(FRP) Plastic Chimney Liners with Coal-Fired Units1
This standard is issued under the fixed designation D5364; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

INTRODUCTION

Federal and state environmental regulations have imposed strict requirements to clean the gases
leaving a chimney. These regulations have resulted in taller chimneys (600–1000 ft (183–305 m)) and
lower gas temperatures (120–200°F (49–93°C)) due to the use of Air Quality Compliance Systems
(ACQS). These regulations led to the development of fiber reinforced plastics (FRP) chimney liners
in the 1970’s.
Fiberglass-reinforced plastic liners have proven their capability to resist corrosion and carry loads
over long periods of time. Successful service has been demonstrated in the utility and general-process
industries for over 40 years. The taller FRP structures and larger diameters (10–30 ft (3–9 m)) imposed
new design, fabrication, and erection challenges.
The design, fabrication, and erection of FRP liners involves disciplines which must address the
specific characteristics of the material. Areas that have been shown to be of importance include the
following:
(1) Flue-gas characteristics such as chemical composition, water and acid dew points, operating and excursion temperature,
velocity, etc.
(2) Plant operation as it relates to variations in the flue-gas characteristics.
(3) Material selection and laminate design.
(4) Quality control throughout the design, fabrication, and erection process to ensure the integrity of the corrosion barrier and
the structural laminate.
(5) Secondary bonding of attachments, appurtenances, and joints.
(6) Installation and handling.
(7) Inspections and Confirmation Testing.
Chimney components include an outer shell, one or more inner liners, breeching ductwork, and miscellaneous platforms,
elevators, ladders, and miscellaneous components. The shell provides structural integrity to environmental forces such as wind,
earthquake, ambient temperatures, and supports the liner or liners. The liner or liners inside the shell protects the shell from the
thermal, chemical, and abrasive environment of the hot boiler gases (generally 120–560°F (49–293°C)). These liners have been
made of FRP, acid-resistant brick, carbon steel, stainless steel, high-alloy steel, shotcrete-coated steel, and shotcrete-coated shells.
The selection of the material type depends on the chemical composition and temperature of the flue gas, liner height, diameter, and
seismic zone. Also, variations in flue-gas characteristics and durations of transient temperatures affect material selection and
design. For FRP liners, the flue gas maximum operating temperature is generally limited to 200°F (90°C) for 2 hours and for
maximum transient temperatures to 400°F (204°C) for 30 minutes.

1. Scope terial selection, fabrication, erection, inspection, confirmatory


1.1 This guide offers direction and guidance to the user testing, quality control and assurance.
concerning available techniques and methods for design, ma- 1.2 These minimum guidelines, when properly used and
implemented, can help ensure a safe and reliable structure for
1
This guide is under the jurisdiction of ASTM Committee D20 on Plastics and the industry.
is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic Piping
Systems and Chemical Equipment. 1.3 This guide offers minimum requirements for the proper
Current edition approved May 1, 2019. Published May 2019. Originally design of a FRP liner once the service conditions relative to
approved in 1993. Last previous edition approved in 2014 as D5364 – 14. DOI:
10.1520/D5364-14R19. thermal, chemical, and erosive environments are defined. Due

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to the variability in liner height, diameter, and the environment, Other Operating and Service Environments 5.7
each liner must be designed and detailed individually. Static Electricity Build-Up 5.8
Flame Spread 5.9
1.4 Selection of the necessary resins and reinforcements, Materials 6
Raw Materials 6.1
composition of the laminate, and proper testing methods are Laminate Composition 6.2
offered. Laminate Properties 6.3
Design 7
1.5 Once the material is selected and the liner designed, Design 7.1
procedures for proper fabrication of the liner are developed. Assumptions 7.2
Dead Loads 7.3
1.6 Field erection, sequence of construction, proper field- Wind Loads 7.4
joint preparation, and alignment are reviewed. Earthquake Loads 7.5
Thermal Loads 7.6
1.7 Quality control and assurance procedures are developed Circumferential Pressure Loads 7.7
for the design, fabrication, and erection phases. The quality- Load Factors 7.8
Resistance Factors 7.9
assurance program defines the proper authority and Loading Combinations 7.10
responsibility, control of design, material, fabrication and Allowable Longitudinal Stresses 7.11
Allowable Circumferential Stresses 7.12
erection, inspection procedures, tolerances, and conformity to
Design Limits 7.13
standards. The quality-control procedures provide the steps Tolerances 7.14
required to implement the quality-assurance program. Deflections 7.15
Critical Deign Considerations and Details 7.16
1.8 Appendix X1 includes research and development sub- Fabrication 8
jects to further support recommendations of this guide. Fabrication 8.1
Reponsibility of Fabricator 8.2
1.9 Disclaimer—The reader is cautioned that independent Fabrication Facility 8.3
General Construction 8.4
professional judgment must be exercised when data or recom- Fabrication Equipment 8.5
mendations set forth in this guide are applied. The publication Resin Systems 8.6
of the material contained herein is not intended as a represen- Reinforcement 8.7
Fabrication Procedures 8.8
tation or warranty on the part of ASTM that this information is Handling and Transportation 8.9
suitable for general or particular use, or freedom from infringe- Erection Appurtenances 8.10
ment of any patent or patents. Anyone making use of this Tolerances 8.11
Erection of FRP Liners 9
information assumes all liability arising from such use. The Erection Scheme and Sequence 9.1
design of structures is within the scope of expertise of a Handling and Storage on Site 9.2
licensed architect, structural engineer, or other licensed profes- Erection Appurtenances 9.3
Field Joints 9.4
sional for the application of principles to a particular structure. Field Joints Lamination Procedure 9.5
Quality Assurance and Quality Control 10
NOTE 1—There is no known ISO equivalent to this standard. Quality Assurance and Quality Control 10.1
1.10 The values stated in inch-pound units are to be re- Quality-Assurance Program 10.2
Quality-Assurance Surveillance 10.3
garded as standard. The values given in parentheses are Inspections 10.4
mathematical conversions to SI units that are provided for Submittals 10.5
information only and are not considered standard. Operation Maintenance and Start-Up Procedures 11
Initial Start-Up 11.1
1.11 This standard does not purport to address all of the Operation and Maintenance 11.2
Annex
safety concerns, if any, associated with its use. It is the Typical Inspection Checklist Annex A1
responsibility of the user of this standard to establish appro- Appendix
priate safety, health, and environmental practices and deter- Commentary Appendix X1
References
mine the applicability of regulatory limitations prior to use.
Section
1.12 This international standard was developed in accor-
Introduction and Background dance with internationally recognized principles on standard-
Scope and Objective 1 ization established in the Decision on Principles for the
Referenced Documents 2
ASTM Standards 2.1
Development of International Standards, Guides and Recom-
ACI Standard 2.2 mendations issued by the World Trade Organization Technical
NFPA Standard 2.3 Barriers to Trade (TBT) Committee.
ASME Standards 2.4
Terminology 3
ASTM Standard General Definitions 3.1 2. Referenced Documents
Applicable Definitions 3.2
Descriptions of Terms Specific to This Standard 3.3
2.1 ASTM Standards:2
Symbols 3.4 C177 Test Method for Steady-State Heat Flux Measure-
Significance and Use 4 ments and Thermal Transmission Properties by Means of
Service and Operating Environments 5
Service Conditions 5.1
Environmental Severity 5.2
Chemical Environment 5.3 2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Erosion/Abrasion Environment 5.4 contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Operating Temperature Environment 5.5 Standards volume information, refer to the standard’s Document Summary page on
Abnormal Environments 5.6 the ASTM website.

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the Guarded-Hot-Plate Apparatus provided for reference:
C518 Test Method for Steady-State Thermal Transmission 3.2.1 accelerator—a material added to the resin to increase
Properties by Means of the Heat Flow Meter Apparatus the rate of polymerization (curing).
C581 Practice for Determining Chemical Resistance of 3.2.2 axial—in the direction of the axis (lengthwise center-
Thermosetting Resins Used in Glass-Fiber-Reinforced line) of the equipment.
Structures Intended for Liquid Service
3.2.3 Barcol hardness—measurement of the degree of cure
C582 Specification for Contact-Molded Reinforced Thermo-
by means of resin hardness. The Barcol impressor is the
setting Plastic (RTP) Laminates for Corrosion-Resistant
instrument used (see Test Method D2583).
Equipment
D638 Test Method for Tensile Properties of Plastics 3.2.4 binder—chemical treatment applied to the random
D648 Test Method for Deflection Temperature of Plastics arrangement of glass fibers to give integrity to mats. Specific
Under Flexural Load in the Edgewise Position binders are utilized to promote chemical compatibility with
D695 Test Method for Compressive Properties of Rigid various laminating resins used.
Plastics 3.2.5 blister—refer to Terminology D883.
D790 Test Methods for Flexural Properties of Unreinforced 3.2.6 bonding—joining of two or more parts by adhesive
and Reinforced Plastics and Electrical Insulating Materi- forces.
als
D883 Terminology Relating to Plastics 3.2.7 bond strength—force per unit area (psi) necessary to
D2393 Test Method for Viscosity of Epoxy Resins and rupture a bond in interlaminar shear.
Related Components (Withdrawn 1992)3 3.2.8 buckling—a mode of failure characterized by an un-
D2471 Practice for Gel Time and Peak Exothermic Tempera- stable lateral deflection due to compressive action on the
ture of Reacting Thermosetting Resins (Withdrawn 2008)3 structural element involved.
D2583 Test Method for Indentation Hardness of Rigid Plas- 3.2.9 burned areas—areas of laminate showing evidence of
tics by Means of a Barcol Impressor decomposition (for example, discoloration and cracking) due
D2584 Test Method for Ignition Loss of Cured Reinforced to excessive resin exotherm.
Resins 3.2.10 burn out (burn off)—thermal decomposition of the
D3299 Specification for Filament-Wound Glass-Fiber- organic materials (resin and binders) from a laminate specimen
Reinforced Thermoset Resin Corrosion-Resistant Tanks in order to determine the weight percent and lamination
D4398 Test Method for Determining the Chemical Resis- sequence of the glass reinforcement.
tance of Fiberglass-Reinforced Thermosetting Resins by
One-Side Panel Exposure (Withdrawn 2015)3 3.2.11 carbon veil—a nonwoven surface veil that is made of
E84 Test Method for Surface Burning Characteristics of carbon fiber or is coated with conductive carbon for purposes
Building Materials of providing static dissipation. This could be carbon veil, or
E228 Test Method for Linear Thermal Expansion of Solid polyester veil impregnated with carbon.
Materials With a Push-Rod Dilatometer 3.2.12 catalyst—an organic peroxide material used to acti-
2.2 American Concrete Institute (ACI) Standard: vate the polymerization of the resin.
ACI Standard 307 Specification for the Design and Con- 3.2.13 chopped-strand mat—reinforcement made from ran-
struction of Reinforced Concrete Chimneys4 domly oriented glass strands that are held together in a mat
2.3 NFPA Standard: form by means of a binder.
NFPA 77 Recommended Practice on Static Electricity5
3.2.14 chopper gun—a machine used to cut continuous
2.4 ASME Standards: fiberglass roving to predetermined lengths [usually 0.5–2 in.
Section X Fiberglass Reinforced Plastic Pressure Vessels6 (13–51 mm)] and propel the cut strands to the mold surface. In
RTP-1 Reinforced Thermoset Plastic Corrosion Resistant the spray-up process, a catalyzed resin is deposited simultane-
Equipment6 ously on the mold. When interspersed layers are provided in
3. Terminology filament winding, the resin spray is not used.
3.1 Definitions: 3.2.15 contact molding—process for molding reinforced
3.1.1 Terms used in this guide are from Terminology D883 plastics in which reinforcement and resin are placed on an open
unless otherwise indicated in 3.2. mold or mandrel. Cure is without application of pressure;
3.2 The following applicable definitions in this guide are includes both hand-lay-up and spray-up.
3.2.16 corrosion barrier—the integral inner barrier of the
3
laminate which is made from resin, veil, and chopped mat.
The last approved version of this historical standard is referenced on
www.astm.org. 3.2.17 coverage—see winding cycle.
4
Available from American Concrete Institute (ACI), P.O. Box 9094, Farmington
Hills, MI 48333-9094, http://www.concrete.org.
3.2.18 crazing—the formation of tiny hairline cracks in
5
Available from National Fire Protection Association (NFPA), 1 Batterymarch varying degrees throughout the resin matrix, particularly in
Park, Quincy, MA 02169-7471, http://www.nfpa.org. resin-rich areas.
6
Available from American Society of Mechanical Engineers (ASME), ASME
International Headquarters, Three Park Ave., New York, NY 10016-5990, http:// 3.2.19 cut edge—end of a laminate resulting from cutting
www.asme.org. that is not protected by a corrosion barrier.

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3.2.20 delamination—physical separation or loss of bond 3.2.40 gel time—time from the initial mixing of the resin
between laminate plies. with catalyst to gelation.
3.2.21 dry spot—an area where the reinforcement fibers 3.2.41 glass—see fiber(glass).
have not been sufficiently wetted with resin. 3.2.42 glass content—weight percent of glass-fiber rein-
3.2.22 edge sealing—application of reinforcement and forcement in the laminate.
resin, or resin alone, to seal cut edges and provide a corrosion- 3.2.43 gun roving—fiberglass roving designed for use in a
resistant barrier. The final layer should be paraffinated. chopper gun.
3.2.23 entrapped-air void—see void. 3.2.44 hand lay-up—see contact molding.
3.2.24 environment—state of the surroundings in contact 3.2.45 heat-deflection temperature (HDT)—temperature at
with the internal and external surfaces, including the which a specified bar specimen deflects 0.010 in. (0.25 mm)
temperature, pressure, chemical exposure, relative humidity, when loaded as a simple beam at a constant 264 psi (1820 kPa).
and presence of liquids or gases. Test Method D648 usually refers to a cured-resin casting, not
3.2.25 exotherm—evolution of heat by the resin during the a laminate.
polymerization reaction. 3.2.46 helical winding—filament winding where the angle
3.2.26 exotherm ply—that ply of chopped mat at which the at which the reinforcement is placed is other than 0 or 90°.
lamination process is stopped to allow gelation and exotherm 3.2.47 hoop winding—filament winding where the winding
of the existing laminate. angle is essentially 90°. The winding strands are applied
3.2.27 fabricator—the producer of the equipment who com- immediately adjacent to the strands applied on the previous
bines resin and reinforcing fibers to produce the final product. mandrel revolution.
3.2.28 fatigue—the change in properties of the laminate 3.2.48 intersperse—chopped fiberglass used in a filament-
over time under cycling of loads, including mechanical, wound laminate, usually in thin layers between winding
temperature, and other environmental exposures. coverages.
3.2.29 fiber(glass)—a fine, continuously formed thread of 3.2.49 isotropic—having uniform properties in all direc-
glass. E-glass is used for strength and durability, E-CR-glass is tions. The measured properties of the material are independent
a modified E-glass with improved corrosion resistance to most of the axis of testing. The opposite is anisotropic, which is the
acids, and C-glass is resistant to corrosion by most acids. case for FRP laminates.
3.2.30 fiberglass roving—see roving. 3.2.50 joint overlay—an overlay that joins the adjoining
3.2.31 fiberglass woven roving—heavy fabric woven from surfaces of two contacting parts or elements.
strands of glass fiber. 3.2.51 laminate—the total of the part constructed by com-
3.2.32 fiber wetting—coating of the fiberglass with resin by bining one or more layers of material (reinforcement and
means of rollout or immersion. resin). As used in this guide, the laminate consists of the
corrosion barrier on the inner surface, the interior structural
3.2.33 filament winding—a process for forming FRP parts
layer, and the outer surface.
by winding resin-saturated continuous-roving strands onto a
rotating mandrel. 3.2.52 laminate composition—the sequence of reinforce-
3.2.34 fillers—inert materials that are added to the resin to ment materials on a type, class, and category basis that make
increase density, increase viscosity, improve abrasion up a laminate.
resistance, enhance resin-application properties, decrease resin 3.2.53 lamination analysis—procedure by which, given the
shrinkage, and reduce cost. amount and properties of the resin and the properties and
3.2.35 fill picks—the rovings in a woven roving that run in orientation of the reinforcement, it is possible to calculate the
the transverse direction of the fabric, that is, across the fabric elastic physical and mechanical properties of the individual
roll width. layers of a laminate and using weighted-averaging techniques
to determine the elastic properties of the total laminate (see
3.2.36 flame-retardant resin—halogenated resins that can be section 2.4).
used with or without additives to provide a laminate having a
reduced flame-spread rating as measured in accordance with 3.2.54 lamination theory—see lamination analysis.
Test Method E84. The resins are not flame retardant in their 3.2.55 mandrel—mold around which a laminate is formed to
liquid state. fabricate a cylindrical section.
3.2.37 flame-spread rating—index number for any laminate 3.2.56 macro—denotes the properties of the laminate as a
of definite composition resulting from testing in accordance total structural element.
with Test Method E84. 3.2.57 matrix—resin phase of a fiberglass-reinforced lami-
3.2.38 gap filling—the filling of voids between joined parts, nate.
elements, or components with resin putty or resin. 3.2.58 micro—denotes the properties of the constituent ele-
3.2.39 gel—the initial jelly-like solid phase that develops ments of the laminate; that is, matrix and reinforcements and
during the polymerization of resin. interface only, and their effect on the laminate properties.

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3.2.59 mold—form over or into which resin and reinforce- 3.2.78 spray-up—method of contact molding where resin
ments are placed to form the laminate product shape. and chopped strands of continuous-filament glass fiber are
3.2.60 monomer—the basic polymerizing element for the deposited on the mold directly from a chopper gun.
formation of the matrix; in FRP-liner fabrication, this is mostly 3.2.79 strain—elongation per unit length.
styrene. 3.2.80 stress—load per unit area.
3.2.61 overlay—laminate applied over base FRP structures 3.2.81 structural layer—the portion of the laminate having
to secure a joint, seal a seam, or attach a nozzle. the primary mechanical strength.
3.2.62 paraffınated resin—resin containing a small amount 3.2.82 surface preparation—the act of roughening, priming,
of dissolved paraffin wax. This wax will come out of the or otherwise treating the laminate surface to achieve surface
solution during cure and bloom to the surface, preventing the conditions that are conducive to adhesion of a subsequently
normal air inhibition at the atmospheric exposed surface. applied laminate.
3.2.63 parting agents—compounds that assist in releasing 3.2.83 surfacing veil—a very thin (10 to 20 mils) mat of
the FRP part from its mold; also referred to as mold-release C-glass or synthetic material such as non-woven polyester
agents. fabric, used to reinforce the corrosion-resistant resin on the
3.2.64 pass—in filament winding, one “round trip” of the inside or outside surface of the FRP laminate.
carriage (which applies the winding strand to the mandrel) 3.2.84 unidirectional roving—continuous parallel roving
from one end of the mandrel to the other and return. held together with periodic stitching.
3.2.65 pit—crater-like area in the surface of the laminate. 3.2.85 vinyl ester resin—resin characterized by reactive
unsaturation, located predominately in terminal positions that
3.2.66 polyester resin—resin produced by the condensation can be compounded with styrene and reacted to produce
of dihydroxy glycols and dibasic organic acids or anhydrides. crosslinked copolymer matrices.
In FRP fabrications, the polyester plastic contains at least one
unsaturated constituent and is dissolved in styrene and subse- 3.2.86 void—unfilled space caused by air or gas in the resin
quently reacted to give a highly crosslinked thermoset matrix. mix or entrapment of such gases during lay-up of individual
plies of glass.
3.2.67 profile—the roughness (or smoothness) of a surface
that has been prepared for bonding. 3.2.87 warp ends—the strands in a woven roving that run in
the longitudinal direction of the fabric, that is, along the roll
3.2.68 promoter—a material which activates the catalyst length of the fabric.
that cures the resin.
3.2.88 winding angle—the angle between the winding
3.2.69 PVA—abbreviation for polyvinyl alcohol, a widely strand and the longitudinal axis of the cylindrical liner,
used parting agent. sometimes called the helix angle. The winding angle can be
3.2.70 reinforcement—glass fibers in the form of continuous determined by measuring the included angle along the longi-
strand, chopped-strand, or fabric. These fibers are added to the tudinal axis of the pipe at the intersection of strands and
resin matrix to give strength and other properties to the dividing this angle by two.
laminate. 3.2.89 winding cycle—the complete covering of the mandrel
3.2.71 release film—film used to facilitate removal of the surface by two bi-directional layers of filament winding. Hoop
fabricated part from the mold. Oriented polyester film, 3 to 5 winding will use one pass; in helical winding many passes are
mils thick has been found suitable for this purpose. required to complete one winding cycle.
3.2.72 resin putty—resin filled with clay, silica fume, milled 3.2.90 woven roving—a plain-weave reinforcement fabric
fibers, or other inert materials, or both, to yield a material for made of rovings. The standard configuration requires five
filling gaps, cracks, and fillets. rovings in the warp direction and four rovings in the weft
direction and a nominal weight of 24 oz/yd2 (814 g/m2).
3.2.73 resin richness—excessive amounts or uneven distri-
bution of resin in the laminate. Such areas are the result of 3.3 Definitions of Terms Specific to This Standard:
improper wetout or drainage and are prone to cracking. 3.3.1 can—an individual fabricated cylindrical liner section.
3.3.2 quality assurance (QA)—a system, employed by the
3.2.74 roll-out—densification of the laminate by working
owner or his designate, to monitor the manufacturer’s quality
reinforcement into and air out of the resin, using a serrated
control and to recognize and resolve any nonconformances.
thermoplastic or metal roller.
This system is administered by a quality-assurance represen-
3.2.75 roving—a number of strands or filaments gathered tative who is empowered to verify the QA and the resolution of
with little or no twist in a package called a roving ball. Also see all noncompliances.
woven roving.
3.3.3 quality-assurance program—a plan that documents
3.2.76 secondary bond strength—adhesive force that holds a the procedures or instructions used to ensure the quality control
separately cured laminate to the basic substrate laminate. of the manufacturing process.
3.2.77 sizing—surface treatment or coating applied to fila- 3.3.4 quality control (QC)—a system of measurements and
ments to improve the filament-to-resin bond. checks employed to monitor the manufacture of the FRP

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TABLE 1 Stress and Modulus of Elasticity Symbols, psi LL = total length of the continuous liner
Stress Type MRF = material resistance factor
Description Membrane Membrane P = external pressure, psi
Bending
Tension Compression p' = atmosphere pressure at plant grade level, psi
Calculated longitudinal fzt fzc fzb r = average radius of the liner wall, in.
Calculated circumferential fθt fθc fθb
Allowable longitudinal Fzt Fzc Fzb
R1 = displacement-induced seismic response (force,
Allowable circumferential Fθt Fθc Fθb displacement, or stress)
Ultimate longitudinal Fztu ... Fzbu R2 = inertia-induced seismic response (force,
Ultimate circumferential Fθtu ... Fθbu displacement, or stress)
Critical buckling, longitudinal ... Fzcr ...
Critical buckling, ... Fθcr ... Rc = radius of the liner to the centroid of the stiffener
circumferential Rs = radius of the stiffener
Modulus of elasticity, Ezt Ezc Ezb Rt = total seismic response (force, displacement, or
longitudinal
Modulus of elasticity, Eθt Eθc Eθb
stress)
circumferential RF = capacity-reduction factor = MRF × TTRF

Editorially corrected column alignment in March 2010. t = thickness of the liner (structural) wall, in.
T = normal temperature load,
Ta = ambient air temperature, Degrees Fahrenheit
tc = thickness of corrosion barrier, in.
chimney liner and to assess compliance of manufacture to the te = equivalent liner thickness, including stiffener
critical quality requirements. contribution, on basis of equal mass
3.4 Symbols: (see Table 1) Tg = flue gas temperature, Degrees Fahrenheit
Tm = mean liner temperature, (T1 + T2)/2, Degrees
a = winding angle (with respect to the longitudinal Fahrenheit
axis of the liner), degree Tn = annulus air temperature, Degrees Fahrenheit
Aθ = hoop membrane stiffness of the liner wall, lb/in. To = temperature at inside surface of corrosion
barrier, Degrees Fahrenheit
AT = abnormal temperature load T1 = temperature at interface between corrosion bar-
CP = circumferential pressure load, psi rier and structural layer, Degrees Fahrenheit
D = dead load T2 = temperature at outside surface of structural
Ds = theoretical draft (without losses), inches of layer, Degrees Fahrenheit
water ∆Tg = flue-gas temperature difference across the di-
Dx, Dθ = longitudinal and hoop bending stiffness, of the ameter of the liner, at height z, °F
liner wall, lb-in.2/in. (∆Tg)BASE = ∆Tg at top of breeching, °F (minimum Tg-
(EI)s = transformed flexural stiffness of ring stiffener, BASE = 25°F)
lb-in.2 ∆Tm = difference of temperature, Tm, across the diam-
EQ = earthquake load eter of the liner, °F
f = ovalling natural frequency, cycles per second ∆Tw = temperature differential across the structural
g = acceleration due to gravity, in/s2 layer, °F (T2 – T1)
H = total height of liner above breeching, ft TTRF = time and temperature reduction factor
h1 = flue-gas film coefficient of thermal W = wind load
conductivity, BTU/ft2/in/h/°F Wcm = compressive modulus of elasticity of the wind-
h3 = film coefficient of thermal conductivity outside ing material (glass), psi
of liner, BTU/ft2/in/h/°F WL = total weight of the continuous liner, including
I = center-line moment of inertia of liner section, corrosion barrier, and stiffeners
in.4 = πr3t Wtm = tension modulus of elasticity of the winding
Is = moment of inertia of one stiffener material (glass), psi
k = coefficient of thermal conductivity for FRP z = distance from top of breeching, in.
liner (in absence of data use k = 2), BTU/ft2/ α = coefficient of thermal expansion in the direction
in/h/°F specified by subscript, in./in./°F
kn = knockdown factor µ = average Poisson’s ratio
kR = ratio of thermal resistance from gas stream to 5 ~ µ zθ 3 µ θz ! 1/2
the middle of the liner wall to the total radial
thermal resistance of liner µθz = Poisson’s ratio of longitudinal strain to an
L = distance between lateral supports, ft imposed hoop strain
L1 = spacing between full circumferential stiffeners, µzθ = Poisson’s ratio of hoop strain to an imposed
in, determined as the sum of half the distance to longitudinal strain
adjacent stiffeners on either side of the stiffener γ = unit weight of liner, lb/in.3
under consideration γa = specific weight of ambient air, lb/ft3
LF = load factor γg = specific weight of gas, lb/ft3

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δ = longitudinal deflection, in. infrequent, such as when precipitator electric power is out or
when bag houses are bypassed. The duration should be
4. Significance and Use determined, as the plant may reduce load or shut down when
4.1 This guide provides information, requirements and rec- such a condition occurs.
ommendations for design professionals, fabricators, installers 5.4.3 Condition 3—High-velocity gas flow (higher than 100
and end-users of FRP chimney liners. FRP is a cost-effective fps (31 m/s)), by design, or at sharp corners, turning vanes, and
and appropriate material of construction for liners operating at struts. Erosion will likely occur at these locations.
moderate temperatures in a corrosive chemical environment. 5.5 Operating Temperature Environment:
4.2 This guide provides uniformity and consistency to the 5.5.1 Condition 1—Saturated flue gas, ambient to 140°F
design, fabrication, and erection of fiberglass-reinforced plastic (60°C). This is the usual operating condition for chimney liners
(FRP) liners for concrete chimneys with coal-fired units. Other on systems with wet scrubbers without reheat. Start-up condi-
fossil fuels will require a thorough review of the operating and tions are covered by the operating conditions. Where bypass of
service conditions and the impact on material selection. scrubbers is provided, conditions are described in 5.6.
4.3 This guide is limited specifically to FRP liners within a 5.5.2 Condition 2—Normal gas temperature from 140 to
supporting concrete shell and is not applicable to other FRP 200°F (60 to 93°C), with moisture content and acid condensa-
cylindrical structures. tion determined by the individual conditions. This is the usual
operating range for wet scrubber systems with reheat. Start-up,
5. Service and Operating Environments high-temperature, and by-pass conditions will be the same as
5.1 Service Conditions: described in 5.6.
5.1.1 To properly select the optimum design for an FRP 5.5.3 Condition 3—Normal gas temperature from 140 to
chimney liner, it is essential to define the operating and service 200°F (60 to 93°C), with temperatures high enough for
conditions and the effect they may have on the lining. The condensation not to occur during normal operation. This is the
chemical, erosion/abrasion, and temperature environments usual operating range for spray dryer-baghouse and spray
should be determined for the full height of the FRP liner. dryer-precipitator combinations. Condensation at start-up is
5.1.2 Owing to the variability in details of design and minimized by not introducing water to the spray dryers until
system configuration, each FRP liner design must be consid- coal firing is started. Temperatures during by-pass and for
ered individually. The information given is for coal-fired units, excursions are as described in 5.6.
but the general principles are applicable to units fired with 5.5.4 Condition 4—Normal gas temperature from 200 to
other fuels. 330°F (93 to 166°C). This is the usual operating range for
5.2 Environmental Condition—The environment for a chim- plants without scrubbers. This condition is also applicable to
ney liner is classified as to its chemical, erosion, and tempera- systems in which the particulate removal or flue-gas desulfu-
ture condition. Two chemical conditions, three erosion rization (FGD) system, or both, can be bypassed, with tem-
conditions, and four temperature conditions are identified, peratures determined by the gas flow that can be bypassed
together with the circumstances in which they usually occur. compared to the total gas flow of the system.
The combinations of circumstances applicable to a particular 5.5.5 This guide covers FRP liners for Conditions 1, 2, and
chimney liner should be determined. 3. Condition 4 is not covered in this guide, although applica-
tions over 200°F (93°C) operating temperature condition are in
5.3 Chemical Environment:
service. Condition 4 requires additional considerations in
5.3.1 Condition 1—Occasional exposure of certain areas to
evaluating materials and composite designs.
low pH from acid condensation, occurring with reheated gas or
un-scrubbed gas at localized cold areas, such as the liner hood 5.6 Abnormal Environments—Abnormal environments,
or during start-up. such as stoppage of an air preheater or malfunction of the
5.3.2 Condition 2—Constant exposure to low pH, acid scrubber sprays, or both, can result in short-term conditions
condensation with concentration based on equilibrium concen- more severe than those covered. The severity and duration of
tration of H2SO4, water vapor in the gas stream at temperatures the abnormal conditions depend on the design and operation of
above the water dew point. This operating condition is usually the plant and should be determined for each project. In many
for scrubber systems without reheat, with essentially saturated cases, these conditions are of short duration because a major
gas with temperatures from ambient to 140°F (60°C), or when upset in the boiler draft system, or in the FGD or particulate
there is insufficient reheat to raise the gas temperature above removal system, means a reduction in load or plant shutdown
the acid dew point. Start-up conditions are covered by the to protect the equipment or stay within the emission criteria.
operating conditions. 5.6.1 Condition 1—Flue-gas-temperature excursion of up to
5.4 Erosion/Abrasion Environment: 250°F (121°C) maximum, maintained by a quench system.
5.4.1 Condition 1—Normal-velocity gas flow (45–100 fps 5.6.2 Condition 2—Flue-gas-temperature excursion up to
(14–31 m/s)) with particulate removal equipment in service. 400°F (227°C) maximum.
Most particulate removal and flue-gas desulfurization (FGD) 5.6.3 FRP liners may be used for abnormal Condition 1, but
systems have velocities in this range. its use for Condition 2 is not considered in this guide.
5.4.2 Condition 2—Normal-velocity gas flow with particu- 5.6.4 The gas temperature shall be maintained by a quench
late removal equipment out of service. This condition would be system at or below a temperature of 250°F (121°C).

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5.6.5 In case of a gas-temperature upset 25°F (−4°C) above 6.1.3.1 Glass reinforcements shall be Type E or E-CR glass
the established operating temperature, an additional deluge fibers having a sizing compatible with the resin.
system should be used to bring the gas temperature back to 6.1.3.2 The surface veil used in the corrosion barrier should
normal operating temperatures. be Type C glass fibers, or a synthetic material as approved by
5.7 Other Operating and Service Environments: the owner. If specified by the purchaser, a carbon veil may be
5.7.1 Start-up of coal-fired units is usually accomplished added for static-charge dissipation as in section 6.3.6.
with fuel other than coal, such as diesel oil, natural gas, or 6.2 Laminate Composition—FRP chimney-liner laminates
liquefied natural gas. These fuels, which result in flue-gas consist of a corrosion barrier, a structural layer, and an exterior
compositions different from that produced by coal-firing, surface. The FRP composition shall include a thermoset
should be considered in the design of the liner. polyester or vinylester resin, reinforced with glass fiber and
5.7.2 The temperatures given are average temperatures of containing various other raw materials to provide specific
flue gases entering the chimney liners. Gas temperatures vary properties. The corrosion barrier provides primary corrosion
as the gas rises up the chimney and at breaching openings, and resistance, flame retardant, and shall follow laminate construc-
they vary with the start-up condition of the unit. tion described in Specification C582. The structural layer shall
5.8 Static Electricity Build-Up—FRP in a chimney-liner primarily provide the mechanical properties and strength of the
application is subject to the build-up of static electricity that design. The outer layer shall contain a paraffinated resin to
may be a consideration in some installations. A static-charge prevent air from inhibiting the cure process and shall provide
dissipation system must be provided where considered neces- weather or environmental protection, or both. Liner extending
sary (see 6.3.6). above the chimney cap shall be protected against ultraviolet
(UV) rays and in cold weather regions, against ice forming on
5.9 Flame Spread—FRP chimney liners are subject to con- the liner surfaces from freezing of water droplets in the gas
ditions that propagate flame spread. Specific requirements will phase.
vary, depending upon operating and maintenance conditions.
6.2.1 Corrosion Barrier—The corrosion barrier shall be as
However, all FRP liners shall have a flame-resistant resin as in
described in Specification C582. Additional plies of surfacing
6.3.5.
mat and chopped-strand mat may be used in particularly severe
chemical environments, but consideration shall be given to the
6. Materials effects of thermal and mechanical shock.
6.1 Raw Materials: 6.2.2 Structural Layer—The structural layer shall meet the
6.1.1 Resin: physical properties required by the design in Section 7. The
6.1.1.1 The selected resin shall be either a polyester or fabrication process is typically filament winding, as described
vinylester that provides the properties necessary to withstand in Specification D3299 and Section 8, but may include contact
the conditions of the operating environment described in molding, as described in Specification C582, or a combination
Section 5. Resins shall conform to the requirements of Speci- of both.
fication C582. 6.2.3 Outer Layer
6.1.1.2 FRP chimney liners are fabricated with a flame-
retardant resin and, when required, additional flame-retardant 6.3 Laminate Properties:
synergist added. The resin shall, at minimum, have been 6.3.1 Physical and Mechanical—The following physical-
demonstrated to withstand 25 % sulfuric acid at 180°F (82°C) property test methods are designed for use on entire laminates
for a duration of one year with a minimum retained strength of or individually on the corrosion barrier, the structural layer, or
50 %, in accordance with Practice C581, or under the actual repeating structural units, and external overlays. The following
anticipated environmental-service condition. test methods shall be used for determination of initial design
6.1.1.3 The resin in the corrosion barrier shall be chosen for data and QA/QC procedures:
its corrosion resistance and flame-retardant properties. Due to 6.3.1.1 Tensile Modulus (Axial Direction)—Test Method
physical and mechanical requirements, a different corrosion- D638 shall be used; or the test results used in conjunction with
resistant resin may be used in the corrosion barrier than in the laminate theory as in section 6.3.1.6.
structural layer. 6.3.1.2 Flexural Modulus (Axial and Hoop Directions)—
6.1.2 Other Additives—The resin may contain diluents such Test Method D790 shall be used; or the test results used in
as added styrene, fillers, dyes, pigments, or flame retardants conjunction with laminate theory as in section 6.3.1.6.
only when agreed upon between the fabricator and the owner. 6.3.1.3 Compressive Modulus—The compressive modulus
Such uses shall conform to the descriptions of diluents, resin shall be obtained in accordance with Test Method D695, with
pastes, and ultraviolet absorbers as explained in Specification the following modifications. The specimens shall be 2 in. (51
C582. Additionally, carbon filler may be added for static- mm) in the test direction by 0.5 in. (13 mm) thick with the
charge dissipation. corrosion barrier removed by machining. Strain shall be
6.1.3 Reinforcements—Reinforcements shall conform to the measured by the use of an extensometer or other strain gages
requirements of Specification C582 for contact molding and centered on the specimen in the 2-in. direction. The extensom-
Specification D3299 for filament winding. These specifications eter arms shall be spaced to 1.5 in. (38 mm) apart at their
require the sizing and binder systems to be compatible with the attachment points to the specimen. The test results may be used
resins selected. in conjunction with laminate theory as in section 6.3.1.6.

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6.3.1.4 Coeffıcient of Thermal Expansion—Coefficient of and thermal gradient through the laminate with the temperature
thermal expansion shall be measured in accordance with Test at the corrosion liner/structural layer interface.
Method E228, over an appropriate temperature range using 6.3.5 Flame Retardancy—Selection of the flame spread
specimens constructed with the same composition, resin, rating is governed by local building codes. The purchaser shall
construction sequence, glass content, type and weight of specify the rating for each location.
reinforcement, and cure conditions used in the actual liner. The 6.3.5.1 Flame spread is determined in accordance with Test
glass content of the test laminate should be within 5 % of the Method E84 (see Note 2) by using a standard laminate
glass content of the actual chimney-liner laminate. The direc- construction as determined in accordance with 4.1.2 of Speci-
tion of measurement in relation to the orientation of glass shall fication C582. The standard laminate is 0.125 in. (3 mm) thick,
be considered in interpretation of the results. Unidirectional flat, reinforced with all mat and has a glass content of 25 to
roving may be used to approximate filament winding. 30 % by weight. Flame-retardant synergists of the type and
6.3.1.5 Coeffıcient of Thermal Conductivity—The coeffi- level used in the actual laminate construction shall be used in
cient of thermal conductivity shall be determined by Test this test.
Method C177 or C518 on representative laminate for either the
NOTE 2—This flame-spread rating is based on a laboratory test, which
entire liner laminate to be used, or for each of the following is not necessarily predictive of product performance in a real fire situation,
laminate components; that is, corrosion barrier, structure layer, and is therefore not intended to reflect hazards presented by this or any
and exterior coating, if any. The representative laminate shall other material under actual fire conditions.
be a flat laminate constructed with the same resin, construction 6.3.6 Static-Charge Dissipation—Operation of FRP chim-
sequence, glass content, type and weight of reinforcements, ney liners can build up significant static charges. This may be
and cure conditions used in the actual laminate. The direction a safety hazard to personnel and appropriate grounding shall be
of measurement in relation to the orientation of glass shall be considered.
considered in interpretation of the results. Unidirectional rov- 6.3.7 Grounding System—Each can in the liner shall have at
ing may be used to approximate filament winding. least two proof tested grounding patches. The patches shall be
6.3.1.6 Laminate theory may be used instead of physical externally connected to a grounding system conforming to the
testing to determine axial tensile, flexural, and compressive requirements of NFPA 77 and 77-16. Patches should be
moduli only. In such a case, the axial tensile and hoop flexural approximately 2 feet square containing conductive carbon filler
moduli computed from laminate theory shall be verified by and carbon veil covering a 1⁄2 in. bolt that connects to the
comparison with the results obtained by physical testing. The grounding system. Every bolt patch shall be proof tested
test results shall be at least 90 % of the computed values. (ohmmeter) to assure it will provide an appropriate path to
6.3.2 Chemical—The corrosion resistance of the resins used ground.
shall have been characterized by either Practice C581 or Test
Method D4398. Resins may also be evaluated for vapor 7. Design
exposure in accordance with Practice C581, except that speci- 7.1 Design:
mens are exposed totally in the vapor space above the liquid 7.1.1 Standard guidelines and minimum requirements are
returning from the condenser. The resin shall have been provided for the structural design of fiber-reinforced plastic
deemed acceptable for long-term use in the environments (FRP) chimney liners, based on load and resistance-factor
described in Section 5 (Conditions 1 or 2, or both), by either of design procedures.
the above test methods or verifiable actual field environments.
7.1.2 The objective is to provide a uniform procedure for
6.3.3 Erosion/Abrasion—In areas where Condition 3 computing forces and displacements of the liner based on the
erosion/abrasion is expected, resin additives such as silicon present state of the art and science of design of fiber-reinforced
carbide may be considered. plastic liners.
6.3.4 Temperature: 7.1.3 The design is limited to FRP chimney liners supported
6.3.4.1 The material properties of the laminate shall be laterally and vertically by the concrete shell.
suitable for operating-temperature environments as defined by 7.1.4 The design of a fiber-reinforced plastic liner is an
normal Conditions 1, 2, and 3, and abnormal Condition 1. iterative process and similar to most engineering designs, but
These conditions define only typical temperature environ- with the following significant differences:
ments. It is essential for the owner to fully provide specific 7.1.4.1 Fiber-reinforced plastic is a composite material and
temperature conditions in order to properly select the optimum its behavior is different from isotropic materials.
resin. 7.1.4.2 The practical variation in the physical properties of
6.3.4.2 The maximum operating temperature at the interface the liner material in the thermal and chemical design environ-
between the corrosion barrier and the structural layer shall not ments are more than those encountered in most other structural
exceed the heat-deflection temperature (HDT) of the structural- materials.
layer resin. The HDT shall be determined in accordance with 7.1.5 The scope is limited to chimney liners designed to
Test Method D648. operate continuously in operating temperature environments
6.3.4.3 The temperature at the corrosion barrier/structural defined by Conditions 1, 2, and 3 in Section 5 under normal
layer interface may be determined by a thermocouple embed- operating conditions, and for Condition 1 for abnormal envi-
ded in the laminate or by correlating gas-stream temperature ronments defined in Section 5. The design of liners operating in

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normal-temperature environment, Condition 4, or abnormal 7.2.10 The minimum structural-wall thickness of the liner
Condition 2, is not covered. shall be 3⁄8 in. (10 mm).
7.2 Assumptions: 7.2.11 Wherever the design requirements for the concrete
7.2.1 The design procedure is based on the overall stress chimney are cited in accordance with ACI 307, it is implied
resultants acting on the wall and on the properties of the that requirements of ACI 307, or of the project specification,
laminate. whichever are more critical, shall be used.
7.2.12 Nothing in this section shall be deemed to prohibit
7.2.2 For the purpose of analysis, the cross section is
the use of other properly substantiated technical data and
considered to consist of the average diameter and structural
procedures for the analysis and design of fiber reinforced
layer thickness. The thickness of the corrosion barrier is
plastic liners.
excluded. For structure design, properties of the material are
based on centerline temperature of the section (that is, average 7.3 Dead Loads (D):
through-wall thickness), except where variation through the 7.3.1 The dead load shall include the estimated weight of all
thickness is being explicitly considered. permanent structures, including stiffeners and attachments. A
7.2.3 For analysis of the liner behavior due to dead load, unit weight of 140 lb/ft3 (2243 kg/m3) is recommended for the
wind, earthquake, and thermal loads, the liner may be treated calculation of the dead load of the liner (including stiffeners
as a beam column and beam theory used for calculating the and attachments) using its nominal dimensions.
resultant stresses and displacements. 7.3.2 Where fly-ash is expected to be deposited on the inside
7.2.4 For the beam-column analysis, the liner may be surface of the liner, the dead load of the fly-ash shall be
considered uncoupled (separate) or coupled (jointly) with considered in the design. Where a wet scrubber is in operation,
respect to the concrete column. or can be in operation upstream of the chimney liner, a fly-ash
7.2.4.1 For the uncoupled system, the liner is considered to deposit shall be considered to be attached to the inside of the
be rigidly supported by the concrete column and shall be liner. The variation of the thickness of the fly-ash deposit along
designed as a continuous beam column. The displacements at the height of the liner shall be as shown in Fig. 1. The dead
points of support or restraint shall equal the independently load of the wet fly-ash shall be based on a unit weight of 80
computed displacements of the concrete shell. lb/ft3 (1281 kg/m3).
7.2.4.2 For the coupled system, the coupling of the liner and 7.3.2.1 Where a wet scrubber is not in operation and no
the concrete column system is achieved by incorporating the quenching system is used, or used briefly or rarely, the dry
flexibility of the concrete column in the liner design. A larger
combined structure must be analyzed to obtain forces in the
liner member(s) as a beam column.
7.2.4.3 The flexibility of the supports and restraints between
the liner and the concrete column and the local flexibility of the
liner at lateral support points may be incorporated in the
analysis of the coupled system.
7.2.5 If the frequency of vibration of the liner, based on
beam theory, is within 620 % of the concrete column
frequency, a dynamic analysis of the coupled system shall be
made. A dynamic analysis of the coupled FRP liner/concrete
column system shall be made, unless it is demonstrated by
evaluation of the mass frequency ratios that coupling effects
are negligible.
7.2.6 At points of application of loads (that is, at supports
and restraints) on the liner beam-column, the liner may be
adequately stiffened locally so that the liner roundness is
maintained and the liner indeed functions as a beam-column.
7.2.7 Resultant forces are computed from linear elastic
analysis of the beam column.
7.2.8 Using the resultant forces from the analysis, the design
of the liner is checked against the appropriate material prop-
erties of the laminate. The resistance in a certain direction is
based on the strength of the laminate in that direction,
determined either experimentally or derived from known
properties of the constituents.
7.2.9 Most material properties used in the analysis and
design are results of short-duration tests at room temperature.
Factors are recommended to reduce these property values to a
design life of 35 years of the liner in the range of operating
temperatures given in Section 5. FIG. 1 Fly-Ash Deposit

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fly-ash load [65 lb/ft3 (1040 kg/m3) dry-unit weight] shall 7.6 Thermal Loads:
equal 0.5 lb/ft2 (2.5 kg/m2) on the entire inside surface of the 7.6.1 Uniform Temperature Loading (T)—The uniform tem-
liner, or as specified. perature across the cross section normally does not cause any
7.3.2.2 When a quench system is used frequently and a wet forces or stresses since the liner is not restrained in the
scrubber is not in operation, the moist fly-ash load [80 longitudinal direction. This load is used to calculate the total
lb/ft3 (1281 kg/m3) average moist-unit weight] shall equal 1.50 thermal expansion of the liner due to the difference between the
lb/ft2 (7 kg/m2) on the entire inside surface of the liner, or as installation and operating temperatures.
specified. 7.6.2 Non-Uniform Temperature Loading (∆T)—Thermal
7.3.3 The liner shall be designed to withstand the installa- loading on the liner is created by non-uniform temperatures
tion and handling stresses and the temporary loads during within the gas stream in both longitudinal and circumferential
construction. Such loads should include self dead weight when directions and by the variation of temperature through the liner
the can is resting on its side prior to the installation of bracing. wall thickness when combined with boundary restraint condi-
Temporary supports, lifting lugs, rigging, scaffolding, and tions.
other construction equipment shall be designed in accordance 7.6.3 Longitudinal Stress Due to Thermal Loads—The lon-
with accepted structural-engineering practices. gitudinal thermal stress shall be taken as the sum of the flexural
stress, the secondary stress, and the stress induced in the wall
7.4 Wind Loads (W)—The liner shall be designed for all
by the temperature differential through the wall.
forces induced by the displacements caused by wind on the
concrete column in accordance with ACI 307. The analysis for 7.6.3.1 Thermal Membrane Stress—A liner subject to cir-
the dynamic wind loads shall be for along-wind or across- cumferential temperature differential will rotate if free to do so.
wind, whichever gives higher relative displacements in accor- The resulting curvature may be expressed by 0.4 αz∆Tm/r.
dance with ACI 307. Thermal-membrane (direct) stresses result when rotational and
translational supports restrain the curvature of the liner. The
7.5 Earthquake Loads (EQ)—It is recognized that the liner equivalent moment to be applied to the liner is 0.4 EzIαz∆Tm/r.
and chimney column interact under earthquake motion. Proce- 7.6.3.2 Temperature differential of the liner across its diam-
dures for the dynamic analysis of the combined column liner eter is calculated as follows:
system are outlined in 7.5.1. An alternative empirical proce-
∆T m 5 ∆T g ~ 1 2 k R ! (1)
dure is outlined in section 7.5.2.
7.5.1 Dynamic Analysis: where:
7.5.1.1 The liner shall be designed for all forces or ∆Tg = flue-gas temperature difference across the diameter,
displacements, or both, resulting from a response spectrum and
analysis of the combined column liner system for the design kR = thermal resistance from gas stream to the middle of
response spectra in accordance with ACI 307. the liner wall relative to the total radial thermal
7.5.1.2 Other dynamic analysis, based on properly substan- resistance of liner.
tiated technical data for establishing the magnitude and distri- In these calculations, the insulation effect of the corrosion-
bution of lateral forces, is also acceptable. In such analyses, the barrier thickness shall be used.
dynamic characteristics of both the column and liner shall be 7.6.3.3 Temperature differential of flue gas across liner
considered. diameter is constant through the height of the breeching and
7.5.2 Empirical Method—The empirical method consists of attenuates with height as follows:
computing, separately, the liner earthquake responses due to
∆T g 5 ~ ∆T g ! basee 20.2z/r (2)
column deflections and due to liner inertia, and then combining
them to obtain the total liner earthquake response. The re- where:
straints between the liner and the concrete column are consid- z = distance from the top of breeching, and
ered rigid. The procedure is as follows: (∆Tg)base = minimum of 25°F (−4°C).
7.5.2.1 Calculate the response of the liner to displacements 7.6.3.4 Temperature differential across the structural layer,
induced by the concrete column due to earthquake. The column ∆Tw, should be considered in the design of the liner.
displacements shall be obtained from either method of earth-
7.6.3.5 Thermally induced longitudinal secondary mem-
quake analysis given in ACI 307, that is, from the design-
brane stress resulting from ∆Tg shall be computed from:
response-spectrum analysis or the equivalent static-lateral-
force analysis. f z ct 5 0.1E z ctα z ~ ∆T g ! (3)
7.5.2.2 Calculate the response of the liner due to its inertia where:
to the earthquake loads given in ACI 307 by either the Ezct = modulus of elasticity (compression or tension) in the
design-response spectrum or by the equivalent static-lateral- longitudinal direction, and
force method. αz = average coefficient of thermal expansion in the longi-
7.5.2.3 Calculate the total liner earthquake response from: tudinal direction.
R t 5 ~ R 1 2 1R 2 2 ! 1/2 7.6.3.6 Longitudinal bending stress due to temperature dif-
where R1 and R2 are the responses calculated from section ferential through the structural layer shall be computed from:
7.5.2.1 and 7.5.2.2, respectively. The response may be a
typical quantity such as force, displacement, or stress. f z b 5 0.5E z b α z ∆T w (4)

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where:
αz and Ezb = average material properties of the wall in the f5
3
πR 2c
Œ E bθ I s g
5L 1 γt e ~ 1 2 µ 2 !
(7)
longitudinal direction, and
∆Tw = total temperature differential through the struc- WL
te 5
tural layer. 2πrL L γ

7.6.4 Temperature differential, ∆Tw, also induces bending where:


stresses in the circumferential direction, which may be com- Rc = radius of the liner to the centroid of the stiffeners,
puted similarly using material properties in the circumferential Eθb = circumferential bending modulus of elasticity of the
direction. liner,
7.6.5 Reverse-thermal-gradient loading (that is, during shut- Is = moment of inertia of one (1) stiffener,
g = acceleration due to gravity,
down) where air temperature in the annulus is higher than
L1 = spacing between full circumferential stiffeners,
inside the liner, shall be considered in the design of the liner. γ = unit weight of liner,
7.7 Circumferential Pressure Loads (CP)—The circumfer- te = equivalent liner thickness, including stiffener
ential loads on the liner result from the positive or negative contribution, on basis of equal mass,
pressure inside the liner and pressure fluctuations due to µ = average Poisson’s ratio of the liner,
WL = total weight of the continuous liner, including corro-
turbulent gas flow.
sion barrier, and stiffeners,
7.7.1 Pressure in the Liner: r = radius of the liner,
7.7.1.1 The pressure within a liner is affected by changes in LL = total length of the continuous liner, and
the unit operation (air preheater malfunction, forced draft, or rs = radius of the stiffener
induced draft fan changes) as well as the changes in the unit 7.7.2.4 For other liners not covered by section 7.7.2.2 and
load. 7.7.2.3, rational procedures shall be used for computing the
7.7.1.2 When a liner is conveying hot flue gas of a specific lowest frequency.
weight less than that of the surrounding atmosphere, the
pressure on the outside of the liner may be greater than on the 7.8 Load Factors (LF)—The load factors in the limit design
inside. This negative pressure is commonly referred to as the approach are multiplicative factors used on dead, live, wind,
chimney draft. The amount of negative pressure depends on the earthquake, and temperature loads, as follows:
temperature and velocity of the flue gas, the height of the liner, LF = 0.9 or 1.2 for dead load (D),
as well as atmosphere pressure. When the flue-gas flow is = 1.3 for wind or earthquake load (W or EQ),
supplemented by induced-draft fans, a reduction of the net = 1.1 for temperature load (T or ∆T),
negative pressure will result. For cases when an induced-draft = 1.1 for circumferential pressure loads (CP).
fan is forcing the gas or cool air, or both, through the liner, the
7.9 Resistance Factor (RF)—Resistance factor is the prod-
liner may be operating under a net positive pressure.
uct of material resistance factor (MRF) and time-and-
7.7.1.3 The theoretical negative static pressure, neglecting temperature-reduction factor (TTRF) (RF = MRF × TTRF).
losses, shall be computed from:
7.9.1 Material-Resistance Factor (MRF)—The usable de-
D s 5 0.192H ~ γ a 2 γ g ! , inches of water (5) sign strength is a fraction of the nominal material strength in
where H = height from the center of breeching to top of the given mode.
liner.
7.9.2 The material-resistance factor for various types of
7.7.2 Liner Vibrations: loading is as follows:
7.7.2.1 There are situations where a liner may vibrate due to
MRF = 0.65 for direct tension or flexural, or both,
the movement of gas through it or due to resonance of the
= 0.40 for direct compression.
chimney column as a result of excitation by wind or earth-
quake. The lowest ovalling frequency of the liner, given in 7.9.3 Time-and-Temperature-Reduction Factor (TTRF)—
section 7.7.2.2 or 7.7.2.3 shall not be in the frequency range of The reduction in the mechanical properties of the liner material
the pressure fluctuation at the base of the liner. Where no under load subjected to the operating environment of the liner
specific data is available on the frequency range of pressure is reflected in the time-and-temperature-reduction factor
fluctuations, the lowest ovalling frequency shall not be less (TTRF). If no experimental data is available, the values of
than 2 Hz. TTRF in section 7.9.5 shall be used.
7.7.2.2 The lowest ovalling or ring frequency for an unstiff- 7.9.4 The TTRF is affected significantly by the duration of
ened liner is calculated as follows: the load. It is larger for short-term loads, such as those arising
in abnormal operations or upset conditions, as compared to
f5
t
2πr 2
Œ 3E θ b g
5γ ~ 1 2 µ 2 !
(6) those for the long-term loads such as normal operation and
dead loads.
7.7.2.3 For a stiffened liner with ring stiffeners, the lowest 7.9.5 The TTRF for the various types and durations of
frequency is calculated as follows: stresses at operating environments is given in Table 2.

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TABLE 2 Time-and-Temperature-Reduction Factors (TTRF) for 7.11.1.2 Lateral bracing such as stay rods or bumpers shall
Long-Term Operation and Short-Term Abnormal Environments be provided so that L/r does not exceed 20.
Type of Stress 7.11.2 Tensile Stress—Direct or membrane stress is that part
Duration Membrane Membrane
Bending of the total stress, which is uniform over the thickness of the
Tension Compression
structural layer, or which is almost uniform through the
Long-term 0.2 0.7 0.7 structural layer as in the case of beam bending of the liner. The
Short-term 0.6 0.8 0.8 remaining part of the total stress is caused by the bending of the
structural layer.
7.11.2.1 The maximum allowable longitudinal direct tensile
7.9.6 The values of the moduli used in sections 7.10 and stress in the liner shall be determined as follows:
7.11 shall correspond to results from short-duration tests under F z t 5 RF 3 F z tu (16)
the mean liner (Tm) temperature conditions. where:
7.10 Loading Combinations—Stresses shall be calculated RF = 0.13 for long-term loads,
for all three load combinations shown in sections 7.10.1 and RF = 0.39 for short-term loads, and
7.10.2. Fztu = ultimate longitudinal short-term tensile strength of the
7.10.1 Loading combination for the sustained or long-term structural layer at room temperature.
loading are as follows:
7.11.3 Bending Stresses—The allowable bending tension or
Load Combination No. 1: (8) compression in the longitudinal direction shall be determined
1.2D11.1T11.1CP
from the following equation:
F z b 5 RF 3 F z bu (17)
and where D reduces the effects of T and CP:
0.9D11.1T11.1CP (9)
where:
RF = 0.45 for long-term loads,
where: RF = 0.52 for short-term loads, and
D = dead loads, Fzbu = ultimate longitudinal short-term bending strength of
T = temperature loads, and the structural layer at room temperature.
CP = circumferential pressure effects.
7.12 Allowable Circumferential Stresses:
7.10.2 Short-duration-loading combinations are as follows: 7.12.1 Compressive Membrane Stress—Determine the
Load Combination No. 2:1.2D11.1T11.3W/EQ11.1CP (10) maximum allowable circumferential compressive membrane
stress in the liner by the following equation:
and where D reduces the effects of T, CP, and W or EQ :
F θ c 5 RF 3 F θ cr 5 0.28 F θ cr for long 2 term loads, and (18)
0.9D11.1T11.3W/EQ11.1CP (11)
where W/EQ = effects of wind or earthquake, not taken at F θ c 5 RF 3 F θ cr 5 0.32 F θ cr for short 2 term loads.
the same time.
Load Combination No. 3: (12) where Fθcr is calculated by:
@ ~ E z c ! 1/4 ~ E θ b ! 3/4 # ~ t/r ! 1.5
1.2D11.1AT11.1CP F θ cr 5 0.765 (19)
~ L 1 /r !
and where D reduces the effect of AT and CP:
7.12.2 Tensile Stress—Direct or membrane stress is that part
0.9D11AT11.1CP (13) of the total stress which is uniform over the thickness of the
where AT = effect of the abnormal temperature condition. structural layer. The remaining part of the total circumferential
tension stress is caused by the bending of the liner wall.
7.11 Allowable Longitudinal Stresses:
7.12.2.1 Determine the maximum allowable circumferential
7.11.1 Compressive Stress—Determine the maximum al-
direct tensile stress in the liner by the following equation:
lowable longitudinal compressive stress in the cylindrical liner
by the following equation: F θ t 5 RF 3 F θ tu (20)
c cr
F z 5 RF 3 F z (14) 50.13 F θ tu for long 2 term loads, and

50.28 F z cr for long term loads, and 50.39 F θ tu for short 2 term loads.
where Fθtu = ultimate hoop short-term tensile strength of the
50.32 F z cr for short term loads. structural layer at room temperature.
7.11.1.1 Fzcr in Eq 14 is calculated as follows: 7.12.3 Bending Stresses—The allowable bending tension or
k nt compression in the circumferential direction shall be deter-
F z cr 5 0.6
r
=E z b E θ c (15)
mined from the following equation:
~
k n 5 knockdown factor 5 1.00 2 0.91 1 2 e 20.06=r/t ! F θ b 5 RF 3 F θ bu (21)

(15A) 50.45 F θ bu for long 2 term loads, and

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50.52 F θ bu for short 2 term loads. 7.13.2 When either the longitudinal or circumferential stress
where Fθbu = ultimate circumferential short-term bending is compressive, the following requirements shall be satisfied:
strength of the liner wall, at room temperature.
f θc f zc
#1 and #1 (25)
7.12.4 Circumferential Stiffener Requirements: F θc F zc
7.12.4.1 General—Circumferential stiffening shall meet the
7.13.3 When the longitudinal and circumferential stresses
minimum requirements given in this section when the unstiff-
are both compressive, interaction shall be as follows:
ened liner shell is unable to structurely support the circumfer-
ential pressures as described herein. In addition to providing
structural resistance, stiffeners reduce the effect of imperfec-
f zc
F zc
1 S D
f θc
F θc
2
#1 (26)

tions built into the cross section. 7.13.4 The design limits in section 7.13 shall be applied,
7.12.4.2 The circumferential stiffeners shall be designed to separately, for long-term loads and for short-term loads.
resist the lateral loads arising from the positive or negative
pressure inside the liner, pressure fluctuations due to turbulent 7.14 Tolerances—The tolerances are based on those in
gas flow, liner vibrations (see section 7.7.2) and the lateral Section 8.
restraints such as stay rods and bumpers. 7.15 Deflections:
7.12.4.3 Stiffener Spacing—Spacing of stiffeners shall not 7.15.1 Short-Term Loads—The loading combinations de-
exceed 11⁄2 diameters of the liner or 25 ft (8 m), whichever is fined in section 7.10 with the loads defined in sections 7.3
less. through 7.7 shall be used to calculate deflections using the
7.12.4.4 Stiffener Size—The size of stiffeners shall satisfy short-term moduli of elasticity at room temperature.
the following requirements: 7.15.2 Long-Term Loads—The primary loads causing the
(a) The ring stiffener shall have a bending stiffness equal to long-term longitudinal deflection are the tension resulting from
or greater than that determined by the following equation: dead loads and the thermal growth of the liner.
PL r 3 7.15.2.1 The long-term longitudinal deflection shall be cal-
~ EI! s $ 1.15~1RF! (22)
culated from the following expression:
where: δ 5 @ f z t /E z t 1α z ∆T # 12H (27)
(EI)s = transformed flexural stiffness of the ring stiffener, 7.16 Critical Design Considerations and Details—The fol-
and lowing design considerations and details are critical to an FRP
RF = reduction factor for flexural tension or compression liner and will require careful consideration by the design
for short-term loads. The MRF, of the RF, shall be professional:
selected based on the stiffener material used (that is, 7.16.1 Shear parallel to laminate,
steel, plastic). 7.16.2 Support shoulders,
(b) In determining stiffener-section properties, a portion of 7.16.3 Lateral-restraint locations,
the structural layer of the liner equal in width to 1.56 =rt may 7.16.4 Construction joints,
be included, but the total area so added shall not exceed the
7.16.5 Reinforcement around openings,
transformed area of the stiffener.
(c) The stiffener shall be designed for the erection loads, 7.16.6 Breechings,
including deflection considerations. 7.16.7 Hoods, and
7.16.8 Expansion joints.
7.13 Design Limits—The liner shall be so proportioned that
the actual or computed stress in a given direction of the liner, 8. Fabrication
for a given loading condition, is less than the corresponding
allowable stress. Thus, when one of the two computed stresses, 8.1 Fabrication—This section addresses minimum require-
namely, longitudinal or circumferential, is tensile, the require- ments of facilities, tooling, laminate construction, and proce-
ment is expressed as follows: dures necessary for satisfactory fabrication of FRP chimney
liner components.
f zt f zb
1 #1 (23) 8.2 Responsibility of Fabricator—The responsibility of the
F zt F zb
fabricator shall be to construct the equipment in accordance
or with the complete designs and details set forth solely by the
f θt f θb design professional and shall warrant all workmanship to be in
1 #1 (24)
F θt F θb accordance with specified designs.
7.13.1 As an alternative method to the requirements of 8.3 Fabrication Facility:
section 7.13 for allowable tensile and bending stresses, the 8.3.1 The fabrication process is considered to be a “shop”
design professional may choose to use lamination analysis. If operation which can be performed in the “home-shop” of the
used then follow the procedure set forth in ASME RTP-1, a fabricator, or the process can be performed in a “temporary
standard for reinforced thermoset plastic corrosion-resistant shop” that is built at or near the project site.
equipment. The elastic constants and strain limits selected shall 8.3.2 The facility shall be enclosed and capable of main-
account for the thermal environment of the liner. taining a 60°F (16°C) minimum constant environment.

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8.3.2.1 The facility shall maintain all materials and equip- 8.5.3 Resin Apparatus—The resin-delivery equipment shall
ment during use at a minimum of 5°F (3°C) above dew-point be commercial internal-mixing units which will accurately
temperature to avoid moisture condensation. meter, dispense, and mix the proper ratio of catalyst to
8.3.3 Special care and conditioning is required when mate- promoted resin in adequate volume to properly wet out
rials are brought in from cold outside temperatures to warm (saturate) the glass reinforcement.
work areas. 8.5.4 Reinforcement Apparatus—The machine apparatus
8.3.4 If fabrication is not a continuous operation, provisions should deliver glass strand, and other reinforcements, in a
shall be made to assure that condensation does not develop on manner that is uniform, consistent and repeatable from part to
the surface of an incomplete part. part. Application of reinforcements that may cause gaps, voids
8.3.5 All mechanical systems (heating, lighting, and venti- or other structural impairments is not acceptable.
lation) shall be designed and operated for adequate safety of
8.6 Resin Systems:
materials and personnel.
8.3.5.1 The facility shall have adequate ventilation capacity 8.6.1 Resins shall be stored, promoted, catalyzed, and ap-
to constantly maintain the proper number of air changes per plied within the recommendations of the resin manufacturer.
hour, as required by OSHA (1).7 8.6.1.1 The resins shall be maintained at a minimum tem-
8.3.5.2 The styrene concentration at the working level shall perature of 60°F (16°C) during mixing and application.
not exceed that required by OSHA (1). Ventilation shall be 8.6.1.2 Resins can be supplied in drums or tank-car quan-
designed to draw fumes from the floor of the facility. Floor- tities. The mixing requirements apply equally to whatever
level exhaust fans are recommended. quantities are being mixed.
8.3.6 Open-flame heating units shall not be allowed. 8.6.2 Resin viscosity may be adjusted for manufacturing
Electric, steam, or closed-flame units are acceptable. The requirements by the addition of thixotropic agents such as
source of heat cannot generate any particles, moisture, or fumed silica or styrene, or both. The addition of thixotropic
organic vapor to the environment. agents or styrene shall be within the recommendation of the
8.4 General Construction: resin manufacturer and in no case shall these concentrations
8.4.1 The FRP chimney liners are normally constructed exceed 5 % by weight of the resin.
from individual cylindrical sections, called “cans,” of the 8.6.3 Resins containing dispersed solids shall be agitated
diameter set forth by the design. after mixing and continuously throughout use during applica-
8.4.2 The can should be fabricated in lengths to minimize tion.
the number of required erection joints. 8.6.4 Resins may be supplied with or without factory
promoters added. When promoters or other additives are added
8.5 Fabrication Equipment:
at the fabrication site, adequate equipment shall be provided to
8.5.1 Winding Machine:
assure accurate measurement and adequate mixing of resin.
8.5.1.1 The winding machine shall maintain a wind angle
within 61 1⁄2 ° throughout the length of the can. 8.6.5 Prior to application, a gel time test shall be performed
8.5.1.2 The machine shall deliver the reinforcing strands in on the resin. A suitable means shall be used to monitor the flow
a continuous uniform flat band saturated with resin. Unsatu- of catalyst to ensure that properly catalyzed resin is delivered
rated glass is not acceptable. to the mandrel.
8.5.1.3 The number of winding passes and the weight of 8.7 Reinforcement:
resin and reinforcement applied shall be recorded for each can. 8.7.1 Structural reinforcements shall be E or E-CR-grade
8.5.2 Mandrel: fiberglass rovings and mat with sizings and binder systems
8.5.2.1 The FRP cans shall be fabricated on mandrels with compatible with the specified resin, as stated in the requirement
uniform outer surface to minimize flat spots or indentations. in Section 6.
Mandrels may be of either collapsible or tapered design to 8.7.2 All reinforcement products shall be packaged, stored,
allow removal of the liner can. The extraction method shall and handled in such a manner that does not allow damage or
ensure safe removal without scratches. contamination (that is, dirt, moisture, etc.).
8.5.2.2 The mandrel shall have a diameter within 60.25 % 8.7.3 Winding rovings shall be continuous strands having
of the specified diameter anywhere along its length. nominal yield of 200 yd/lb, or greater.
8.5.2.3 The mandrel drive and related mechanisms shall be
8.7.4 Chopped-strand mat shall consist of random fibers
capable of maintaining the proper pattern(s) from can to can.
with a minimum length of 1 in. (25 mm) and maximum of 2 in.
8.5.2.4 Suitable polyester film, or other release agents such
(50 mm). A nominal weight of 1.5 oz/ft2 (458 g/m2) is required.
as polyvinyl alcohol, or both, shall be used to provide a glossy
Mat may be applied as roll goods or by use of a chopper gun.
inner surface to ensure extraction without damage to the inner
surface. 8.8 Fabrication Procedures:
8.5.2.5 Mandrel temperature must be 60°F (16°C) minimum 8.8.1 Mandrel Preparation:
during application of material. 8.8.1.1 Liner cans shall be constructed over a smooth
mandrel surface with a laminate consisting of: (1) a corrosion
barrier that consists of a resin-rich inner surface reinforced
7
The boldface numbers in parentheses refer to the list of references at the end of with one or more veil layers and interior layer(s) reinforced
this guide. with chopped-strand mat, both intended for optimum chemical

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resistance; (2) a structural layer reinforced with continuous- 8.8.3.2 Such deficiencies shall be removed or corrected by
strand rovings and mat layers for structured requirements; and grinding or sanding. Any pockets or depressions created by this
(3) an exterior outer surface for weather, erosion, and environ- operation shall be filled with chopped-strand laminate to a
mental protection. uniform flush surface.
8.8.1.2 The specific laminate sequence and number of layers 8.8.3.3 The structural reinforcement should be applied with
shall be determined by the design professional and detailed on 24 hours after completion of the corrosion barrier. The surface
the manufacturing drawings. of the corrosion barrier must be inspected for contamination
8.8.1.3 The mandrel and any molds shall be examined prior and condensation, and an acetone sensitivity test performed. If
to the start of fabrication to assure that their surfaces are clean no contamination or condensation is found, and the surface is
and free of defects. acetone sensitive, the structural reinforcement may be applied.
8.8.2 Corrosion Barrier: 8.8.3.4 If the surface does not become tacky with acetone,
8.8.2.1 The corrosion barrier shall be built-up on the man- or if the surface becomes contaminated by any cause, the
drel in a sequential operation to achieve the requirements of the surface shall be thoroughly sanded to remove the surface gloss.
specified laminate. The surface shall then be blown free of excessive dust. In no
8.8.2.2 A resin coat shall be applied to the rotating mandrel case shall the time between completion of the corrosion barrier
before application of any reinforcement. The mandrel shall be and application of the structural layer exceed 72 h without
wetted with resin and the specified veil applied. The veil should sanding.
be applied with sufficient overlap to ensure that no gaps are 8.8.3.5 The structural layer shall consist of continuous
present. Additional wetting of the veil may be required to wound strands at the specified winding angle. Strands shall be
achieve proper saturation. applied as a flat band in a helical pattern so as to provide full
8.8.2.3 The inner surface shall be 0.010-in. (0.25-mm) mandrel coverage of bi-directional layers without gaps or
nominal thickness reinforced with a minimum one-veil rein- overlays. Patterns that may not allow butting bands next to the
forcement. preceding band shall not be used.
8.8.2.4 The resin content of the inner surface shall be 8.8.3.6 As determined by the design professional, localized
approximately 85 % by weight. reinforcements may consist of circular wound rovings and weft
8.8.2.5 After a uniform wet-resin coat has been applied the unidirectional roving parallel to the axis and shall be detailed
veil shall be applied with a minimum overlap of 0.5 in. (13 on the manufacturing drawings.
mm) and no gaps shall be permitted. Another application of 8.8.3.7 The winding angle shall be as specified in the project
resin shall then be applied to assure complete wet-out of the specifications and drawings. Allowable variation from the
veil. specified angle is 63°.
8.8.2.6 The interior layers shall consist of chopped-strand 8.8.3.8 Immediately before start of the structural layer
mat or chopped rovings in one or more layers as specified. application, a wet layer of chopped strand shall be applied to
8.8.2.7 Chopped strand and resin shall be applied with “bed” the continuous strand and compensate for any minor
uniform thickness. If more than 1.5 oz/ft2 (458 g ⁄m2) is outer-surface irregularities.
required, it shall be applied in a minimum of two applications.
8.8.3.9 The first complete cycle (closed-pattern layer) of
8.8.2.8 Each pass shall be adequately rolled to ensure proper winding shall be applied with sufficient resin to fill in minor
wet-out and air pocket removal. surface irregularities to aid in and ensure good bedding onto
8.8.2.9 The resin content of the interior layer(s) shall be at the cured corrosion barrier.
least 70 %, but not more than 80 % by weight.
8.8.3.10 The glass content of the structural layer shall be
8.8.2.10 The mat shall be overlapped a minimum of 0.5 in.
within 63 % of that used to predict the design properties.
(13 mm) and no gaps shall be permitted.
8.8.3.11 Not more than 5 % of the winding strand or two
8.8.2.11 After completion of the corrosion barrier (inner
adjacent strands may be allowed to break out before the
surface and interior layers), the laminate shall be allowed to
operation is stopped and the strands retied.
exotherm and essentially cure prior to the application of the
structural wall. The structural wall shall not be allowed to 8.8.3.12 If the winding operation is not continuous to the
compress the thickness of the corrosion barrier. final thickness, or if equipment breakdown occurs that delays
8.8.2.12 After exotherm, the liner shall be inspected for completion, then the procedures in 8.8.3.3 and 8.8.3.4 shall be
rough spots, bumps, or depressions that may cause subsequent followed before the winding operation restarts.
bridging of the filament winding. 8.8.4 Outer Layer—The outer exterior surface shall be
8.8.2.13 The corrosion barrier shall be free of any coated with a layer of non-air-inhibited resin.
contamination, including moisture, and shall be acetone- 8.8.5 Fittings:
sensitive prior to start of filament winding. 8.8.5.1 Fittings shall be fabricated by hand lay-up construc-
8.8.3 Structural Layer: tion of alternate layers of mat and woven roving or by filament
8.8.3.1 Before starting the structural layer, the surface of the winding, or a combination of both. The precise sequence and
corrosion barrier shall be inspected for defects, air pockets, number of layers shall be specified by the design professional
protruding glass fibers, ridges at abutted reinforcement, or and detailed on the manufacturing drawings.
other conditions which could lead to deficiencies in subsequent 8.8.5.2 All fittings, regardless of structural layer design,
operations. shall have a corrosion barrier equal to the liner requirements.

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8.8.5.3 Flanges shall be fabricated by hand lay-up proce- points, or on the weight of the can, however, shall be between
dures. The stub wall reinforcing shall be continuous into the −5 and +10 %. When based on weight, there shall be no limit
flange face. on the tolerance on underweight as long as the thickness
8.8.6 Structural Joints: tolerances are achieved.
8.8.6.1 Structural joints for shop fabrication and field instal- 8.11.6 Control the total weight of the liner in order that the
lation shall be butt-and-strap type. The specific joint require- grillages not be overloaded.
ments shall be determined by the design professional.
8.8.6.2 Butt-and-strap joints may be on the inside only or 9. Erection of FRP Liners
inside and outside.
9.1 Erection Scheme and Sequence:
8.8.6.3 Butt-and-strap joints shall be constructed with alter-
9.1.1 Prior to liner erection, a construction plan shall be
nating layers of mat and woven roving to the thickness
formulated detailing the erection sequence and methods to be
specified.
employed by the contractor.
8.8.6.4 The first and last layers of butt-and-strap joints shall
9.1.2 Consideration shall be given to the loads imposed on
be mat.
the FRP liner during handling, storage, and erection. Stresses
8.8.6.5 All structural joints 24 in. (610 mm) in diameter and
resulting from these loads shall be accounted for during the
larger shall have an internal sealing laminate at least equal in
initial-design stage and incorporated into the final design.
construction to the specified corrosion barrier.
Conditions such as ovalling and localized stresses at lifting
8.9 Handling and Transportation: points are of particular importance.
8.9.1 All liner sections shall be properly handled in a safe 9.1.3 All rigging materials and hoisting equipment shall be
manner that will not allow damage, scuffing, or over-stressing. designed by a licensed engineer and made available to the
The FRP components shall not be allowed to impact on any owner for review, if requested.
hard objects as nonvisible impact damage may occur.
9.2 Handling and Storage on Site:
8.9.2 All shipments shall be adequately packaged, braced,
and cradled in order to prevent damage during transit. Ends and 9.2.1 Handling of liner cans shall be done with slings made
fittings shall be adequately protected from damage. of nylon or other similar materials to prevent damage to the
exterior surface.
8.9.3 All handling of cans shall be by means of non-abrasive
slings. The use of cables or chains is prohibited. 9.2.2 When repositioning the liner cans from the horizontal
to the vertical position, take care to avoid bottom edge point
8.10 Erection Appurtenances: loading conditions which may cause cracking of the interior
8.10.1 Lifting lugs or similar attachments shall be provided corrosion-barrier surface.
on each liner section for ease of handling and erection. 9.2.3 Liner cans shall be stored in a manner that will
8.10.1.1 The design of these attachments shall be incorpo- minimize ovalling.
rated into the overall design of the liner and shall take into 9.2.4 Stored liner cans shall be checked for wind effects and
account the method of handling and loads imposed. suitable anchorage or guy wires provided if required.
8.10.1.2 Location of the lifting attachments shall be deter-
mined by the fabricator and reviewed by the design profes- 9.3 Erection Appurtenances:
sional. Details of the attachments shall be furnished by the 9.3.1 The use of alignment lugs on each liner can is required
design professional. to ensure proper fit-up and liner orientation during the erection
phase. They shall be designed to accommodate any loads
8.11 Tolerances: imposed during erection.
8.11.1 The design professional is responsible to set consis- 9.3.2 When the liner installation utilizes a temporary FRP
tent tolerances for the manufacturing of the FRP cans and the lifting shoulder to support the liner during erection, it shall be
steel components that are attached to the cans. Tolerances shall similar in fabrication to any permanent support shoulders. The
take into account limitations with respect to methods of lifting shoulder shall be designed to accommodate all loads
manufacturing. imposed during erection.
8.11.2 The tolerance of can diameter, based on internal
measurement when the can is in the vertical position, including 9.4 Field Joints:
the out-of-roundness, shall be less than 1 %. 9.4.1 Field joints shall be connected as shown on the
8.11.3 Flat spots on a can shall not cause a change in erection drawings.
geometry in excess of that resulting in a radial offset of 0.2 in. 9.4.2 All field joints shall be designed to transmit the loads
(5 mm) over 2 ft (610 mm), 0.4 in. (10 mm) over 3 ft (915 from each liner can to the next. The joint shall be equivalent in
mm), and 0.8 in. (20 mm) over 4 ft (1219 mm) of the strength to the structural layer.
circumference of the can. 9.4.3 A butt-and-strap joint is preferred to other types. The
8.11.4 Tolerance on the overall can height shall be 61⁄2 % width of the joint shall be a minimum of 16 in. (406 mm) with
but shall not exceed 61⁄2 in. (13 mm). the sum of the exterior and interior overlay at least equal to the
8.11.5 Tolerance on the thickness of total structural layer full-wall thickness of the thinner can.
and of the corrosion-barrier layer at any point shall be −10 to 9.4.4 All joint types shall be cured to at least 25 Barcol
+20 %. The tolerance on the average thickness of a can, based hardness, read at eight places equally spaced on each surface
on thickness measurements of at least five randomly selected around the circumference, and averaged, eliminating the high

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and low readings, before moving the section. Barcol readings 9.5.2.6 If the patch begins to gel, (i.e. harden) prior to
shall be made for both the interior and exterior joint surfaces. placement on the liner can surface or prior to all the air removal
9.4.5 The contractor shall provide methods to ensure proper between the cans and the overlay, remove the patch and discard
alignment of joints, tolerances, and clearances to the design it.
professional for review prior to erection. 9.5.2.7 Allow laminate package to completely exotherm and
9.4.6 The contractor shall provide an inspection and testing cool to ambient temperature.
program, as well as safety recommendations, to the design 9.5.2.8 Repeat procedure from step 9.5.1.1 for each follow-
professional for review prior to erection. ing laminate sequence to apply the remainder of the overlay
material as defined in the overlay kit (glass layers).
9.5 Field Joint Lamination Procedure: 9.5.2.9 Visually inspect the weld overlay, remove and cor-
9.5.1 Joint Overlay Zone Preparation: rect with additional overlay material any deficiencies exceed-
9.5.1.1 The field weld overlay must be applied onto the ing the prescribed limit per square foot area Ishall not exceed
surface of an FRP Liner Can which has been abraded to the following. MoveMore][VB60] stringent requirements may
completely remove the glaze, and is clean and dry. The surface take precedence over these requirements.
glaze (external post coat or internal corrosion barrier), must be 9.5.3 Top Coat of Overlay Surface:
abraded in the overlay zone by grinding using a 24 grit 9.5.3.1 After application of all overlay laminate packages,
grinding disc, a 36 grit grinding disc can be used if it produces and all repairs have been completed prepare the overlay
the required surface profile. The abraded surface should not laminate for a final resin coat by grinding all loose edges and
have a polished finish appearance; it must remove the surface burrs. Use of a 36 grit grinding disc or higher is acceptable for
glaze exposing a clean abraded surface which has a roughened this step, as the intent is to provide a smooth finished laminate
finish approximately a 0.15 mm (0.006) mil minimum texture. surface profile.
9.5.1.2 The surface preparation should be done just prior to 9.5.3.2 Apply a coating or catalyzed resin to the entire
fabricating the weld overlay (no more than 12 hours maximum overlay joint area. This final topcoat is intended to provide a
prior to overlay placement). If the surface has been pre-ground resin rich surface, possibly with the addition of chemicals for
and left exposed to exterior environments (wet with dew or ultraviolet protection and wax for providing a tack free surface.
moisture) then acetone solvent wipe, allow to air dry, or dry
with a heat gun, and regrind the overlay zone. 10. Quality Assurance and Quality Control
9.5.1.3 If the grinding dust and dirt has not been removed 10.1 Quality Assurance and Quality Control:
from the overlay surface, this will cause the overlay not to have 10.1.1 Minimum quality-control criteria are stated for the
the proper bond adhesion. Clean, dry air or a clean cotton rag design, fabrication, erection, and inspection of the FRP
maybe used to remove the surface dust. chimney-liner system and accessories, and to ensure a system
9.5.1.4 If there is doubt about the surface preparation, of high-operating reliability.
re-prepare the surface for bonding. 10.1.2 Minimum quality requirements shall be ensured
through the entire process of design, fabrication, and installa-
9.5.2 Weld Overlay Placement:
tion. The components for the program may be defined by the
9.5.2.1 Verify the proper weld kit materials are available. fabricator or a designated representative of the owner. The
Overlay patches consist of multiple glass fabric plies; refer to procedures and practices shall be performed by persons with a
project drawings for the fabric ply order and quantities. demonstrated knowledge of FRP design and fabrication and the
9.5.2.2 Verify surface preparation is completed properly and specific requirements of chimney liners.
proceed with lamination.
10.2 Quality-Assurance Program:
9.5.2.3 If required, a bonding coat of catalyzed resin may be 10.2.1 The contractor’s organization shall be established in
applied to the section of the overlay zone to receive the such a manner that persons involved in the quality-assurance
overlay. This should be done before the application of the first program have sufficient authority and organizational freedom
plies. to identify quality nonconformances. The quality-assurance
9.5.2.4 Wet out the overlay plies on clean cardboard or non program shall define the method(s) to initiate, recommend, or
waxed Kraft paper. Be certain that all tools are clean and free provide solutions, as well as to verify implementation of
of liquid solvent before using. Begin to wet out overlay plies solutions.
starting with the widest ply first on the wet out table. Verify 10.2.2 The organization shall be established in such a
complete saturation of laminate plies with catalyzed resin. Do manner that the individual or group assigned the responsibility
not use an excessive amount of resin to wet overlay patches. for checking, auditing, inspecting, or otherwise verifying that
9.5.2.5 Apply the overlay material. Application in patch an activity has been correctly performed is independent of the
form is recommended. Apply the completed package of plies individual or group directly responsible for performing the
which have been wet out to liner can joint area. The overlay specific activity.
package should be centered on the liner can joint. Use a 10.2.3 The authority and responsibility of persons perform-
serrated roller tool to remove entrapped air from the laminated ing activities affecting quality shall be clearly established and
patch after it is placed on the liner can surface. Continue documented in the contractor’s quality-assurance manual.
applying overlay packages until the weld joint area has been 10.2.4 The contractor shall establish and maintain a quality-
closed completely. assurance program for the control over the quality of the

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specific items being supplied or the work to be performed. The 10.2.14 The contractor shall establish a program for in-
contractor shall require any subcontractors or suppliers to process and final inspection of activities affecting quality to
establish and implement a quality-assurance program for the ensure conformance with documented instructions, procedures,
work to be performed or the items to be supplied, or both. and drawings. Examinations, measurements, or tests shall be
10.2.5 The quality of all items under contract, whether performed for each activity, where necessary, to ensure quality.
supplied by the contractor or a subcontractor, shall be con- Inspection and test activities to verify that the quality of work
trolled at all points necessary to assure conformance with the shall be performed by persons other than those who performed
requirements of this guide and associated codes and standards. the work being inspected.
10.2.6 The quality-assurance program shall be documented 10.2.15 Sufficient records shall be prepared as work is
in detail in a quality-assurance manual, subject to the owner’s performed to furnish documentary evidence of the quality of
(or his designee’s) review. items and activities affecting quality. The records shall be
readily identifiable and retrievable for a period to be identified
10.2.7 The contractor’s quality-assurance manual shall in- by contract.
clude: written instructions, procedures, or drawings to direct
and control activities affecting quality. Job specifications, 10.3 Quality-Assurance Surveillance:
instructions, job tickets, planning sheets, operating or proce- 10.3.1 All activities performed by the contractor and sub-
dure manuals, test and repair procedures, or other relevant contractors are subject to quality-assurance surveillance or
documents shall be maintained to control quality. audit, or both, by the owner. Surveillance or audit, or both,
shall not relieve the contractor of any responsibility for the
10.2.8 The contractor’s quality-control system shall provide
requirements of his contract and shall not be considered as
procedures that will ensure that issued documents affecting
waiver of warranty or other rights.
quality, such as procurement documents, reports, drawings,
10.3.2 Compliance with the requirements of this guide does
calculations, procedures, and instructions, are adequately con-
not relieve the contractor of his responsibility to ensure that all
trolled. The control specified in the procedures shall assure that
other contract requirements are met.
the documents are reviewed for adequacy and approved for
10.3.3 The owner shall have the right to establish
release by authorized personnel. Changes to these documents
inspection-hold points and be given prior notice to all inspec-
shall be authorized and controlled in the same manner as the
tions designated as inspection-hold points.
original documents.
10.3.4 Prior to the start of fabrication activities, the owner
10.2.9 The design professional shall ensure that applicable may prepare a vendor-surveillance-check plan (VSCP) which
codes and standards have been included in his design. Mea- will be forwarded to the contractor. The VSCP shall establish
sures shall be established to ensure that appropriate quality those points in the fabrication cycle that the owner will
requirements are specified and included in the design docu- witness, verify, or perform.
ments. 10.3.5 The owner reserves the right to provide a quality-
10.2.10 Design-control measurements shall provide for assurance representative in the fabrication shop. A mutually
verifying or checking the adequacy of design by performance acceptable quality-assurance program that incorporates the
of design reviews and calculational or test programs. intent of the requirements of 10.2.1, 10.2.2, and 10.2.3 shall be
10.2.11 The design professional shall identify and control developed by the fabricator.
design interfaces, including coordination, review, and approval 10.4 Inspections:
with participating organizations of all interfaces with the 10.4.1 Inspections and approval of all critical, major, and
subject equipment. minor quality attributes shall be clearly defined in the quality-
10.2.12 The contractor shall ensure that purchased items assurance manual.
and services, whether purchased directly by him or through his 10.4.2 The acceptance and rejection criteria shall be clearly
subcontractors, conform to the requirements of the procure- defined for materials and laminate construction. Laminates
ment documents. The contractor’s procedures shall include, as shall be inspected for visual defects such as pits, voids, blisters,
appropriate: (1) provisions for source evaluation and selection cracks and other defects listed in Table 5 of Specification
by means of historical quality-performance data, source sur- C582. Special consideration shall be provided for entrapped air
veys or audits, or source qualification programs; and (2) in the bond area of the corrosion barrier as these may result in
objective evidence of quality furnished by the equipment eventual blistering. Appropriate acceptance and repair proce-
subcontractor, source inspection and audit, and inspection and dures shall be written in the Quality Assurance Manual.
test of item upon delivery. 10.4.3 The quality-assurance procedures shall address in-
10.2.13 The contractor shall maintain a system of receiving spections and approval of quality attributes which include, but
control which will assure that the material received is properly are not limited to the following:
identified and has documentation, including required material 10.4.3.1 Completeness of approved drawings and specifica-
certifications or material-test reports to satisfy code or standard tions;
requirements, as ordered. The material-control system shall 10.4.3.2 Material description of resins, reinforcements,
ensure that only acceptable material is used for fabrication or putty, and additives;
construction. These procedures shall also identify the methods 10.4.3.3 Surface Preparation:
of marking and maintaining control on applicable parts and (a) Mandrel.
materials. (b) Corrosion barrier to structural winding.

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(c) Ribs and shoulders. 10.5.4 Resin type with the type of catalyst and promotion
(d) Nozzles and joints. system intended and the location of its intended use.
(e) Secondary bonding of any discontinuous operations 10.5.5 The manufacturer’s general-arrangement drawings
that may occur. showing all dimensions, cross-sectional details of shell joints
10.4.3.4 Hand Lay-Up Laminate (Including Attachments or slip-mold-type joints, nozzles or manways, lugs and
and Appurtenances): supports, knuckles, pads, or other appurtenances. The width,
(a) Thickness control. minimum thickness, and composition of all laminates shall be
(b) Laminate sequences. included.
(c) Exotherm limit. 10.5.6 Description of the method of construction of flanges
(d) Critical ply intervals. detailing the method of connection between the flange face and
(e) Delay-and-restarting contingencies. neck.
(f) Reinforcement staggering. 10.5.7 The materials of construction and dimension of all
(g) Reinforcement overlap. weldments.
(h) Glass-to-resin ratios. 10.5.8 Identification of areas to receive abrasion-resistant
(i) Cure. laminates, for the purpose of resisting localized abrasion or
(j) Wax coat (where applicable). impingement.
10.4.3.5 Filament-Wound Laminate (Including Attachments 10.5.9 All major design criteria including laminate
and Appurtenances): physicals, maximum deflections, and safety factors.
(a) Thickness. 10.5.10 The plan for production of the equipment including
(b) Band width and strands per inch. the expected rate of production, number of shifts per day,
(c) Winding angle. names of the production manager, and leaders of each shift (if
(d) Laminate sequence. known).
(e) Exotherm limit. 10.5.11 Details of assembly and field installation of the
(f) Glass-to-resin ratio. equipment including edge preparations, end gap tolerances,
(g) Cure. and detailed joint-overlay laminate description including the
(h) Strand yield. width and composition of each ply. The method for protection
(i) Gapping tolerance. of the joint area during lamination shall be provided.
10.4.3.6 Environmental Constraints: 10.5.12 All inspection forms required to comply with this
(a) Temperature (air and resin). guide.
(b) Humidity. 10.5.13 Quality-assurance manual.
10.4.3.7 Mechanical Elements Non-FRP: 10.5.14 All design bases including calculations, laminate
(a) Welding and steel fabrication. design, and physical sample test data.
(b) Bolt torques.
10.5.15 Shipping, handling, and storage recommendations
(c) Equipment lifting and handling.
and instructions.
(d) Shipment to the job site.
(e) Storage of completed equipment.
11. Operation, Maintenance, and Start-Up Procedures
(f) Erection sequence.
10.4.3.8 Dimensions and Weights: 11.1 Initial Start-Up or Start-Up After a Long-Term Shut-
(a) Length. down:
(b) Thickness. 11.1.1 During start-up and shutdown, the temperature gra-
(c) Inside diameter. dients shall be gradual. Any sudden temperature changes shall
(d) Out-of-roundness. be avoided.
(e) Weight of finished part. 11.1.2 Prior to start-up, any temperature-moderation devices
10.4.4 A typical inspection checklist is contained in Annex (that is, spray quench systems) shall be checked and opera-
A1. tional.
10.5 Submittals—The following documentation shall be 11.1.3 Prior to start-up all expansion joints, counterweights,
submitted for review prior to fabrication by the contractor, if guides, etc. shall be checked, cleaned, and operating smoothly.
requested by the owner: 11.2 Operation and Maintenance:
10.5.1 The details of construction, including ply thickness 11.2.1 Inspections—Inspections of critical stress areas (that
and type of reinforcement, for all laminates. is, supports) shall be inspected at least annually. A vertical
10.5.2 The description of laminates shall include all plies of interior and exterior full-height inspection of the liner shall be
the corrosion barrier and structural wall, including the mini- performed at regular intervals (maximum two years).
mum allowable thickness for laminate sequences and the 11.2.2 Inspectors shall be qualified to inspect FRP materials
location of exotherm plies. The glass content of the corrosion and any areas of stress shall be noted and mapped.
barrier and structural wall of each laminate shall be provided. 11.2.3 All moving parts (that is, expansion joints), shall be
10.5.3 Filament-wound laminates shall be described includ- inspected regularly to ensure that all are operating satisfacto-
ing the thickness of each cycle, wind angle, and band density. rily. Additionally, any spray-quench system shall be tested. All
The yield of winding strand shall be listed. drains shall be kept clear.

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11.2.4 Written reports of inspections and unusual operating 11.2.6 Operation of the facility shall be such that buildup of
occurrences shall be recorded and a liner history maintained fly ash on the liner is minimized. The spray-quench system
over the life of the liner. shall not be operated continuously on a regular basis. Opera-
11.2.5 During operation of the liner, the difference in tion of the spray-quench system causes buildup of fly ash on
temperature between the ambient temperature surrounding the the liner.
liner shall be minimized. For instance, during cold weather,
exterior chimney-column vents shall not be opened unless
necessary.

ANNEX

(Mandatory Information)

A1. TYPICAL INSPECTION CHECKLIST

Inspection Item Inspection Inspection Reference Procedure Reference Remarks Documentation


Frequency Method Requirement

(1) Mandrel Prior to Start of


Carbon Veil
Application (Hold
Point)
Smooth each can visual ... ... ... not formally
documented
Clean each can visual ... ... ... not formally
documented
Other Items to Verify
Resin batch numbers each can visual ... ... ... quality assurance
manual (QAM)
Resin shelf life each batch visual (drums) ... 6 months resin if exceeds 6 months, not formally
supplier retest in documented
accordance
with procedure
Resin gel-time test each batch Test Method QC procedure resin supplier procedure ... QAM
daily D2471 specifications
Resin viscosity test each batch Test Method procedure resin suppliers procedure QAM
daily D2393 specifications
Glass receiving report each can visual procedure ... ... ... QAM
Air temperature in every day thermometer on ... 50°F (10°C), min fabricator material usage
work area mandrel form
Resin temperature in point each can visual ... min 60°F (16°C) fabricator material usage
of use max 95°F (32°C) form
(2) Carbon Veil (Witness
Application)
Smooth—no wrinkles which each can visual ... ... ... ... not formally
cannot be rolled documented
out before gel
Full wet-out each can visual ... ... ... ... not formally
documented
(3) Surfacing Veil (Witness
Application)
Smooth—no wrinkles which each can visual ... ... ... ... not formally
cannot be rolled documented
out before gel
Full wet-out each can visual ... ... ... ... not formally
documented
(4) Chopped Strand (Witness
First Layer At Least)
Smooth—no wrinkles which each can visual ... ... ... ... not formally
cannot be rolled documented
out before gel
Full wet-out each can visual ... ... ... ... not formally
documented
(5) Ready to Start Filament-
Winding (Witness
Point)
Chopped-strand used each can visual ... 3 oz/ft2 (915 g/m2), procedure material usage
min (2 layers
min)

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Inspection Item Inspection Inspection Reference Procedure Reference Remarks Documentation


Frequency Method Requirement
Chopped-strand layers each can visual ... ... ... ... not formally
gelled prior documented
to winding
Rough spots each can visual ... ... ... ... not formally
ground smooth documented
During winding:
Winding (helix) angle each can visual ... 55–65° specification QAM
(6) After Fabrication is
Complete, and Prior to
Removal from Mandrel
(Witness Point)
No gaps between glass each can visual ... ... ... ... not formally
strands documented
Proper number of filament- each can visual (check ... ... ... QAM
winding cycles based “counter”-
on specified wall passes/cycle)
thickness
All required stiffeners each can visual ... various requirements drawings ... QAM
etc . . . added
Outer surface coat applied each can visual ... U.V. stabilizer procedure QAM
(U.V. stabilizer/wax) and wax
Resin-glass ratio: interior each can Test Method procedure glass content 25 ± procedure QAM
layer (chopped strand) D2584 5 % by weight
Exterior layer (filament- each can Test Method procedure glass content 55 − 0 + procedure QAM
wound) D2584 15 % by weight
Total wall thickness each can cut-outs or ultra ... minimum thickness for procedure QAM
sonics, or both each can and
drawings
Corrosion barrier thickness each can cut-outs ... 0.096 in. (2.5 mm), specification QAM
(veil plus 2 mat) nominal
Barcol hardness (for each can Test Method procedure per resin manufacturer procedure Barcol hardness of QAM
surface cure) D2583 corrosion barrier
to be measured
after can removed
from mandrel
Visual inspection/repair each can visual ... visual specification Inspect corrosion grid preliminary inner
requirements barrier after can
is removed
from mandrel

APPENDIX

(Nonmandatory Information)

X1. COMMENTARY

X1.1 Reference 7.2—The information presented in the (2) The entire formulation may be developed in terms of
ASCE report (2) is used extensively. limiting lamina stresses and strains that constitute the design
criteria.
X1.1.1 Reference 7.2.3—The error introduced in the analy-
sis of cylindrical shells by the beam theory is the assumption X1.2 Reference 7.3.1—The recommended dead load is
that plane surfaces remain plane, or that the bending stresses based on a statistical analysis of some liners. See also X1.3.6.
are proportional to the distances from the neutral axis.
X1.2.1 Reference 7.3.3—The erection loads do not occur in
X1.1.2 Reference 7.2.9—If experimental data is available or conjunction with the thermal loads and hence will not normally
if other values of material properties are available, or both, they control the design of the liner. However, the circumferential
may be used, provided the various parameters defined in this stresses and stability shall be investigated for handling proce-
section can be substantiated (3). dures.
X1.1.3 Reference 7.2.12—It will be up to the user of the
alternative design procedures to properly substantiate the X1.3 Reference 7.4—The mass of the liner is usually not
rationality and the choice of the parameters used in the large enough to significantly affect the dynamic wind charac-
methods. Two examples of such design procedures are given as teristics of the concrete column.
follows: X1.3.1 Reference 7.6.2—An empirical method is presented
(1) Laminate theory may be used in arriving at the theo- in Ref (2). Field data was collected for temperature distribu-
retical properties of the laminate section based on the glass tions along and across steel liners with different geometric
ratio, angle of wind and the material properties of the resin and configurations and flow characteristics. Recommendations are
reinforcement. based on these measurements made in the early 1970’s. The

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operating conditions of some power plants have been altered
since then. Also, the thermal characteristics of uninsulated
fiber-reinforced liners are significantly different from the insu-
lated steel liners considered in the reports.
X1.3.2 The ASCE report remains a primary publicly avail-
able resource on the thermal distributions in liners. However,
caution is required in the present application of the ASCE
report recommendations.
X1.3.3 Reference 7.6.3—The temperature nonuniformity is
the result of incomplete mixing of different-temperature-level
flue-gas streams. The nonuniform temperature distribution
within the gas stream will impose a similar temperature
distribution on the inside of the liner, resulting in varying
temperatures around the centerline circumference of the liner.
These differentials produce unequal longitudinal thermal ex-
pansion causing lateral deflection of the liner. Longitudinal
stresses will develop when the liner is restrained.
X1.3.3.1 If the centerline temperature varies across the liner
as a linear function of the diameter, the resulting deformation
in the cylinder produces only beam-type stresses, if the liner is
restrained from bending freely. This idealized temperature NOTE 1—Curves are based on atmosphere at −20°F (−29°C) and sea
distribution along the centerline of the liner seldom occurs. level.
Secondary thermal stresses develop when nonlinear tempera- FIG. X1.1 External Pressure Curves (1)
ture variations are imposed across the liner.
X1.3.3.2 Reference 7.6.3.2—In the calculation of the total liners are as susceptible to vibration as steel liners. Measure-
thermal resistance, the temperature inside the liner may be ments of steel liners have shown pressure pulsation of 1⁄2 to 2
considered as the average gas temperature: in. of water and dominant frequencies of 1 to 2 Hz (cps). The

S T1
T0
2 D. (X1.1)
spectrum shown in Fig. X1.2 shows a peak at 1.8 cps.
Therefore, it is prudent to ensure a minimum natural frequency
of 2 cps to avoid resonance. Note that ovalling frequency of
X1.3.3.3 Reference 7.6.3.6—The calculations for obtaining liner is proportional to liner thickness, t, material factor
the temperature drop through the liner wall may be performed
in accordance with the procedure outlined in ACI 307. Other
substantiated heat-transfer models and the analysis thereof may
be used.
X1.3.4 Reference 7.7.1.3—Considering the variation of
pressure with elevation above sea level, the equation for Ds
becomes:

D s 5 0.52Hp' S 1
2
1
Ta Tg D inches of water (X1.2)
The negative pressure at the base of a chimney, computed in
accordance with Eq X1.2 under natural-draft conditions, is
shown in Fig. X1.1 in terms of average gas temperature for
various chimney heights. The negative static pressure at the
base of the stack is actually less than the plotted values be-
cause of flow losses, but for liner-design purposes, these val-
ues may be used.
X1.3.5 Reference 7.7.3—Gas movement through the liner is
turbulent and may cause significant pressure fluctuation. At the
present time there is little data available on the magnitude and
frequency of pressure fluctuations, or their spatial distributions
within the liner. The cause of the fluctuations may be associ-
ated with the uneven nature of the combustion process,
turbulence induced when the gas stream changes direction or
velocity, or both, and possible induced pulsation due to an
imbalance in an induced-draft fan. Ovalling vibration of steel NOTE 1—Pressure difference measured by transducers located 180°
liners due to gas turbulence has been observed at several apart.
locations, and is a design criterion for steel liners. The FRP FIG. X1.2 Pressure Difference Versus Frequency

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=2 E/ @ γ ~ 12µ2 ! #
, and 1/r2. For chimney liners of the same 2 =3 C =D x A θ
radius, the material factor for FRP is about 50 to 60 % of that F z cr 5 (X1.3)
rt
for steel; therefore, the thickness of the FRP liner must be 1.7
X1.4.1 For further explanation see Ref (6). For a uniform
to 2 times that of the steel liner to result in the same natural
thickness of the shell and neglecting the shear deflection, the
frequency.
equation reduces to the one given in 7.11.2, with kn = 1.0.
X1.3.5.1 Reference 7.7.2.2—The formula given for ovalling X1.4.2 The value of 0.6 in the equation in 7.11.1.2 corre-
frequency of an unstiffened shell is applicable to small diam- sponds to a Poisson’s ratio of about 0.3.
eter liners (approximately up to 6 ft (1.8 m)) in which the
thickness is not substantially increased. X1.4.3 The above equation is based on the “long-shell”
X1.3.5.2 Reference 7.7.2.3—If the shell is stiffened, appro- formulation. The longitudinal-buckling strength for the “short”
priate computation of natural frequency must be made. shells is higher than that for the long shells. The effect of the
X1.3.5.3 Reference 7.7.2.4—Although natural frequency length for“ intermediate” shells can be incorporated in the
for circumferentially stiffened shell is not given, there is knockdown factor kn in the equation. The additional term of 1.5
nothing that prevents the design professional from using an (r/L1)2 (t/r) in the more exact semi-empirical equation for kn is
appropriate equation. The design professional can reference omitted because its contribution is not significant for the
Forsberg for a discussion of natural frequency of a stiffened practical range of values of (r/L1) and (t/r) for liners. Thus, its
cylinder, or use the equations developed by Forsberg given in maximum value is estimated at about 0.03 when (r/L1) is at its
the steel chimney liner reference (2). practical maximum of 1.0 and t/r is 0.02. Furthermore,
dropping this term is more conservative.
X1.3.6 Reference 7.8—The upper load factor on dead load
was based on a statistical analysis of certain liners. A probabil- X1.4.4 As the value of r/t is increased from 24 to 1160, the
ity of failure of 1 × 10−5 was used with the normal distribution. value kn in the formula given in 7.11 varies from 0.768 to
The procedure given in Ref (4) was used in determining the 0.208. The latter value corresponds to the buckling stress of
load factor. 0.125 Et/r used in (2).
X1.3.6.1 Reference 7.9.1—The material-resistance factor X1.4.5 In addition to longitudinal buckling of the cylindri-
(MRF) accounts for the usual variability in the room- cal shell, the combined flexural and longitudinal compressive
temperature properties of the liner material manufactured stress should not be high enough to cause failure, local
under normal conditions of quality control, as specified in microbuckling, or delamination. Microbuckling occurs when
Section 10. It is based on a coefficient of variation of the fiber bundles buckle locally and delamination causes buckling
measured property of less than 10 %. If the level of quality of one or more laminate. Elastic buckling of a cylindrical shell
control is not sufficient to ensure a coefficient of variation of liner is a bifurcation phenomenon in which two adjacent
less than 10 %, then the MRF must be proportionally reduced. equilibrium configurations exist. The buckling occurs when the
X1.3.6.2 Reference 7.9.3—The time-and-temperature- strain energy required for deforming the liner into the buckled
reduction factor (TTRF) accounts for the loss of the mechani- configuration is less than the external work of the forces that
cal properties of the liner material when subjected to the maintain the liner in the unbuckled configuration. Therefore,
temperature and chemical environment of the liner for the the creep of the material in the unbuckled configuration does
duration of the load. When applied to long-term strength of not affect the buckling strength directly, although it magnifies
laminate in direct tension, it is the ratio of the average strength the imperfections and thus may affect the buckling strength
of a loaded specimen in the chemical environment and tem- indirectly.
perature of the liner that would cause creep rupture only after X1.4.6 High negative pressure can occur in the liner as a
the design life of the liner (35 years) to the strength of the result of the implosion effect following an explosion, or “puff”
specimen as determined by short-term tests at room tempera- in the boiler. Several coal-fired units have experienced explo-
ture. The TTRF should be distinguished from the retained sions during start-up which were severe enough to cause
strength of the laminate, which is the percent of the short-term extensive damage to steel liners. Nonuniform circumferential
strength of the laminate that is retained after exposure of the negative pressures were estimated to exceed 10 in. of water.
unloaded specimen to the combined thermal and chemical
environment of interest. The values of the TTRF presented in X1.4.7 The sudden closing of flue dampers can also create
Section 7 were selected based on the engineering judgment of a similar condition resulting in high negative pressures.
the members of Subcommittee D20.23 and the limited test X1.4.8 There are two significant considerations that suggest
results available (5). that the reduction factors for buckling strength of fiber-
X1.3.6.3 Reference 7.10.2—Wind loading is not considered reinforced plastic liners may be more than those for the steel
in the sustained or long-term loading because the contribution liners. The normal thickness of the former is generally more
of a factored-design wind load is very small, compared to other than that of the latter; thus the ratio of the magnitude of the
long-term loads on the liner. imperfections to the design thickness is likely to be less for
fiber-reinforced plastic. Secondly the method of fabrication of
X1.4 Reference 7.11.1.1—A more accurate longitudinal most liners makes it less likely to have the deviation from the
buckling strength of fiber-reinforced plastics may be deter- circular form, as compared to steel liners, where individual
mined from the following equation: plates are field-welded.

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X1.5 Reference 7.12.1—A more accurate analysis of the X1.5.3 If the test data for the material properties of the
circumferential buckling strength of fiber-reinforced plastics design laminate of the liner are not available, the moduli of
may be determined from the following equation: elasticity of the liner in circumferential compression may be
based on the following formula:
5.5k n ~ A x ! 1/4 ~ D θ ! 3/4
F θ cr 5 (X1.4) ~ E z c1/4 E θ b3/4 ! 5 W cm sin2 a (X1.5)
L 1 =rt
X1.5.4 Reference 7.12.4.4—The stiffness of the stiffener
X1.5.1 For further explanation, see Ref (6). For a uniform
should be large enough to resist ring buckling when subjected
thickness of the liner, Eq X1.4 reduces to the one given in
to radial load, even when the shell buckles and the pressure
7.11.1. The value of kn is taken as 0.9.
loads between stiffener rings are transferred to the rings. The
X1.5.2 The circumferential compressive stress should not factor of safety, FS, without the RF = 2.60. For a fiberglass
exceed the maximum compressive stress that causes mi- stiffener with an RF = 0.52, the FS against buckling = 5.0. For
crobuckling and delamination, as discussed in X1.4. a steel stiffener, an MRF = 0.85, the FS > 3.0.

REFERENCES

(1) Occupational Safety and Health Act (OSHA). Practice No. 63, ASCE, New York, NY, 1984.
(2) “Design and Construction of Steel Chimney Liners,” American (7) Robinson, James, “Utility FRP Chimney Liner Survey,” United
Society of Civil Engineers (ASCE), 1975. Discontinued; reproduc- Engineers and Constructors, Inc., Englewood, CO, May 1983.
tions at: UMI, 3009 N. Zeeb Rd., Ann Arbor, MI 48106. (8) Zarghamee, Mehdi, S., Brainerd, M. L., and Tigne, D. B., “On
(3) Nielsen, L. E., “Mechanical Properties of Polymers and Laminates,” Thermal Blistering of FRP Chimney Liners,” Journal of Structural
Vol 1, Dekar, 1974, pp. 8–83. Engineering, ASCE Vol 112, No. 4, April 1986, pp. 677-691.
(4) MacGregor, J. G., “Safety and Limit States Design for Reinforced (9) Nespoli, O., and Osborne, A. D., “Predicting Elastic Properties of FRP
Concrete,” Canadian Journal of Civil Engineering, Vol 3, 1976, pp. Laminates at Elevated Temperatures,” 1986 Canadian RP/C Corro-
481–513. sion Conference Proceedings, SPI, Canada.
(5) Kraus, H., Creep Analysis, John Wiley and Sons, Chapter 5 (“Creep
(10) Manual of Professional Practice, “Quality in the Constructed
Rupture”), p. 101, 1980.
Project,” American Society of Civil Engineers (ASCE), Vol 1.
(6) “Structural Plastics Design Manual,” ASCE Manual of Engineering

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5365 − 18

Standard Test Method for


Long-Term Ring-Bending Strain of “Fiberglass” (Glass-
Fiber-Reinforced Thermosetting-Resin) Pipe1
This standard is issued under the fixed designation D5365; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 3. Terminology
1.1 This test method covers a procedure for determining the 3.1 Definitions:
long-term ring-bending strain (Sb) of “fiberglass” pipe. Both 3.1.1 General—Definitions are in accordance with Termi-
glass-fiber-reinforced thermosetting-resin pipe (RTRP) and nology D883 and abbreviations are in accordance with Termi-
glass-fiber-reinforced polymer mortar pipe (RPMP) are “fiber- nology D1600 unless otherwise indicated.
glass” pipes. 3.2 Definitions of Terms Specific to This Standard:
1.2 The values stated in inch-pound units are to be regarded 3.2.1 end point—the failure of the test specimen. The failure
as the standard. The SI units given in parentheses are for mode may be catastrophic, characterized by a sudden fracture
information only. through the pipe wall in the area of greatest strain.
1.3 This standard does not purport to address all of the 3.2.2 fiberglass pipe—tubular product containing glass-fiber
safety concerns, if any, associated with its use. It is the reinforcements embedded in or surrounded by curing thermo-
responsibility of the user of this standard to establish appro- setting resin. The composite structure may contain aggregate,
priate safety, health, and environmental practices and deter- granular or platelet fillers, thixotropic agents, pigments, or
mine the applicability of regulatory limitations prior to use. A dyes; thermoplastic or thermosetting liners or coatings may be
specific warning statement is given in 9.5. included.
3.2.3 reinforced polymer mortar pipe (RPMP)—fiberglass
NOTE 1—There is no known ISO equivalent to this standard.
pipe with aggregate.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard- 3.2.4 reinforced thermosetting resin pipe (RTRP)—
ization established in the Decision on Principles for the fiberglass pipe without aggregate.
Development of International Standards, Guides and Recom-
4. Summary of Test Method
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 4.1 This test method consists of subjecting submerged-pipe
ring specimens to various increasing deflections induced by a
2. Referenced Documents constant load and monitoring the time to failure. A minimum of
18 samples are required. Test temperatures are obtained by
2.1 ASTM Standards:2
testing in a fluid environment where the temperature is
D883 Terminology Relating to Plastics
controlled.
D1600 Terminology for Abbreviated Terms Relating to Plas-
tics 4.2 The long-term ring-bending strain is obtained by an
D3567 Practice for Determining Dimensions of “Fiberglass” extrapolation to 50 years of a log-log linear regression line for
(Glass-Fiber-Reinforced Thermosetting Resin) Pipe and failure strain versus time.
Fittings NOTE 2—It is the consensus of Subcommittee D20.23 that the log-log
linear regression analysis of test data is a conservative approach and is
representative of standard industry practice.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.23 on Reinforced Plastic 5. Significance and Use
Piping Systems and Chemical Equipment.
Current edition approved Aug. 1, 2018. Published August 2018. Originally 5.1 This test method determines the long-term ring-bending
approved in 1993. Last previous edition approved in 2012 as D5365 - 12. DOI: strain of pipe when deflected under constant load and im-
10.1520/D5365-18.
2
mersed in a chemical environment. It has been found that
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
effects of chemical environments can be accelerated by strain
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on induced by deflection. This information is useful and necessary
the ASTM website. for the design and application of buried fiberglass pipe.

*A Summary of Changes section appears at the end of this standard


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D5365 − 18
NOTE 3—Pipe of the same diameter but of different wall thicknesses
will develop different strains with the same deflection. Also, pipes having
the same wall thickness but different constructions making up the wall
may develop different strains with the same deflection.

6. Apparatus
6.1 Loading Device—The testing apparatus shall be suitable
for maintaining a constant load on the test specimen.
6.2 Load Application—The load shall be applied to the test
specimens using any of three alternative pairs of parallel
loading surfaces; flat plates, rods or bars of a length at least as
long as the pipe ring and of sufficient strength and stiffness to
ensure a straight loading surface throughout the test. The same Side View Front View
type of loading device shall be used for each specimen in a test 1 Load-Application Guides 5 Submerged Test Specimen
series. In order to achieve uniform strain along the pipe, use 2 Load-Application Device 6 Test Solution
3 0.25 in (6 mm) Rubber Pad 7 0.25 in. (6 mm) Rubber Pad
0.25-in. (6-mm) thick elastomeric pads between the parallel 4 Test Enclosure 8 Load-Applicatiion Device
loading surfaces and the pipe ring (see Note 4).
6.2.1 Flat Plates—The plates shall have a minimum 6-in.
FIG. 1 Long-Term Ring Bending Test Apparatus
(152-mm) width.
6.2.2 Bars—The bars shall have a flat contact surface of
0.75 6 0.25 in. (19 6 6 mm). loading devices (plates, bars, or rods) of the apparatus as near
6.2.3 Rods—The rod diameter shall be 2 6 0.25 in. (51 6 6 parallel as practical. When the desired deflection is obtained
mm) for pipe rings 12 in. (305 mm) and greater in diameter. cease adding load to the apparatus.
For smaller pipes, the rod diameter shall be 1 6 0.25 in. (25 6
6 mm). NOTE 6—Alignment of the specimen within the loading devices is
critical. The loading devices should not only be parallel with the load
6.3 Environment Containment—A test enclosure of suffi- points 180° opposite, but the pipe ring should also be centered between the
cient size to fully immerse the test specimens shall be used to load-application guides. Additionally, the load-application guides should
contain the test solution. The enclosure shall not chemically permit complete vertical freedom of movement, so the specimen remains
affect the test solution. under constant load.
9.4 Measure the vertical inside diameter of the deflected
NOTE 4—Elastomeric pads with a hardness of Shore A40 to 70 have
been used successfully. pipe specimen at both ends to the nearest 0.01 in. (0.25 mm).
Average the measurements and determine the initial deflection
7. Test Specimens by subtracting the average vertical inside diameter after load-
ing from the measurement determined in 9.1.2.
7.1 The test specimens shall be ring sections taken from a
sample(s) of pipe selected at random from a normal production NOTE 7—Deflections in excess of 28 % of diameter may cause local
run. The test specimens shall have a minimum length of one flattening of the pipe and lead to erratic test results. For deflections
approaching 28 %, improved accuracy is obtained by use of strain gages
nominal pipe diameter or 12 in. (305 mm) 6 5 %, whichever is
or by establishing, for each pipe product, a calibration of deflection versus
less. Treat the cut edges of the specimens by the same measured strain. This calibration technique may also be useful at all
procedure as production products. deflection levels.
9.5 Introduce the test solution to completely submerge the
8. Test Conditions
pipe ring. The solution may be added prior to loading the pipe
8.1 The standard temperature shall be 23 6 5°C (73.4 6 ring and should be added within 30 min of loading the pipe
9°F). ring. Testing time commences only after both specimen loading
(deflection) and the addition of solution are complete.
9. Procedure (Warning—Since the failure mode could be catastrophic, take
9.1 Test Specimen Measurements: precautions to prevent or contain splashing or spilling of the
9.1.1 Wall Thickness—Determine in accordance with Test test solution or other damages resulting from the sudden
Method D3567. collapse of the pipe specimen.)
9.1.2 Inside Diameter—Determine in accordance with Test 9.6 Periodically check and maintain the test solution within
Method D3567 at both ends prior to deflection and average the 65 % of the specified strength or concentration for the
measurements. duration of the test. The test specimen must remain completely
NOTE 5—It is recommended that the inside diameter be measured with submerged.
the axis vertical.
NOTE 8—As some solutions become more concentrated with the
9.2 Place the test apparatus into the test enclosure. evaporation of water, care must be exercised in replenishment to prevent
a build-up in strength. It may be necessary, with some reagents, to
9.3 Place the pipe ring in the test apparatus (see Fig. 1) and periodically clean the deflected specimen and replace the test solution with
apply force to deflect the specimen at a rate not to exceed 10 % a fresh mixture. The use of plastic film, cut carefully to fit around the test
of its diameter per minute while keeping the top and bottom apparatus and floated on the top of the test solution, has been found

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D5365 − 18
helpful in reducing evaporation. where:
9.7 Continuously monitor the decreasing pipe-ring inside εf = failure strain in inches per inch (millimetres per
vertical diameter versus time or inspect the loaded specimen at millimetre),
least at the frequency given below and measure the pipe e = wall thickness in inches (millimetres) in accordance
specimen inside vertical diameter: with 9.1.1 (see Note 11),
D = mean diameter in inches (millimetres) (ID in accor-
Hours Inspect at Least
0 to 20 Every hour dance with 9.1.2 plus e in accordance with 9.1.1 or OD
20 to 40 Every 2 h minus e), and
40 to 60 Every 4 h ∆f = failure deflection in accordance with 10.1.
60 to 100 Every 8 h
100 to 600 Every 24 h 10.2.1.2 Springline failures:
600 to 6000 Every 48 h
After 6000 Every week 2.44~ e !~ ∆ f !
εf 5
Determine the deflection by subtracting the inside vertical ~ D1∆ f /2 ! 2
NOTE 11—The Sb calculations assume that the neutral axis is at the
diameter from the measurement determined in 9.1.2. pipe-wall midpoint. For pipe-wall constructions that produce an altered
neutral-axis position, it shall be necessary to evaluate results by substi-
NOTE 9—Decreasing diameter of the pipe ring (deflection change) may
tuting 2ȳ for e. (ȳ is the distance from the appropriate pipe surface to the
be monitored with an appropriate indicator on the apparatus above the
neutral axis.) Neutral-axis position shall be determined with strain-gage
solution and submerged specimen.
couples.
9.8 Calculate the end point (failure time and failure deflec- 10.2.2 Use for each specimen in the series, the log of the
tion) in accordance with 10.1. failure strain and the log of the failure time in hours as
9.9 Record the following data: described in A1.4.1. Calculate Sb, the strain at 50 years
9.9.1 Average pipe-wall thickness, (438 000 h).
10.2.3 If Sxy > 0 (see Annex A1.4.2.2), consider the data
9.9.2 Average inside pipe diameter before deflection, unsuitable.
9.9.3 Average inside pipe diameter after deflection, 10.2.4 Calculate r in accordance with A1.4.3.1. If r is less
9.9.4 Initial deflection, than the applicable minimum value given in Table A1.1,
9.9.5 Type of loading device, consider the data unsuitable.
9.9.6 Type, location and time of any distress of the pipe 10.2.5 Prepare a graph on a log-log diagram showing time
wall, to failure versus failure strain, with time plotted on the
9.9.7 Failure deflection and time at the end point, and horizontal (x) axis and strain on the vertical (y) axis.
9.9.8 Type of failure. 11. Reconfirmation of the Sb Regression Line
9.10 To determine the regression line and the lower confi- 11.1 When a piping product has an existing Sb regression
dence level, a minimum of 18 samples is required. Distribution line, any change in material, manufacturing process, construc-
of data points shall be as follows: tion or liner will necessitate a screening evaluation (reconfir-
Hours Failure Points
mation) as described in 11.2, 11.3, 11.4, and 11.5.
10 to 1000 At least 4 11.2 Calculate and plot the 95 % confidence limits and the
1000 to 6000 At least 3
After 6000 At least 3 95 % prediction limits of the original regression line in
After 10 000 At least 1 accordance with A1.4.6.2 using only data obtained prior to the
9.10.1 Those specimens that have not failed after more than change.
10 000 h may be included as failures to establish the regression NOTE 12—Prediction limits define the bounds for single observations,
line. Use of these data points may result in a higher or lower whereas confidence limits define the bounds for the regression line.
extrapolated value. NOTE 13—For 95 % confidence limits, there is a 2.5 % probability that
the mean value for the regression line may fall above the UCL and a 2.5 %
NOTE 10—Non-failed specimens may be left under test and the probability that the mean value for the regression line may fall below the
regression line recalculated as failures are obtained. LCL. For 95 % prediction limits, there is a 2.5 % probability that
individual data points may fall above the UPL and a 2.5 % probability that
individual data points may fall below the LPL.
10. Calculation
11.3 From the original regression line, select strain levels
10.1 Determine the failure time and deflection: for at least two sets of specimens. Each specimen set shall
10.1.1 The failure deflection and failure time shall be the consist of three or more specimens tested at the same initial
last values noted prior to the fracture occurrence. strain level, as follows:
Hours to Failure Failure Points
10.2 Long-Term Ring-Bending Strain: (Average of Set)
10.2.1 Compute the failure strain for each failed specimen 10 to 200 At least 3
More than 1000 At least 3
as given in 10.2.1.1 and 10.2.1.2. Total: At least 6
10.2.1.1 Crown and invert failures: For the purposes of reconfirmation it is permitted to include
4.28~ e !~ ∆ f ! as failures those specimens which have not failed after 1200
εf 5
~ D1∆ f /2 ! 2 hours provided they exceed the existing regression line.

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D5365 − 18
11.4 Consider any changes in material or manufacturing 11.6.2 The 95 % lower confidence limit of the original
process minor and permissible if the results of 11.3 meet the regression line at 50 years.
following criteria:
11.4.1 The average failure point for each specimen set falls 12. Report
on or above the 95 % lower confidence limit of the original 12.1 Report the following information:
regression line. 12.1.1 Complete identification of the pipe composition,
11.4.2 The earliest individual failure point falls on or above manufacturers code, size, and minimum wall thickness,
the 95 % lower-prediction limit of the original regression line. 12.1.2 Description of loading apparatus and monitoring
11.4.3 The failure points are distributed about the originally system,
determined regression line. No more than two-thirds of the 12.1.3 Data in 9.9,
individual failure points may fall below the original regression 12.1.4 Complete description of the test solution,
line. 12.1.5 If used, the type of strain gage employed and method
of mounting,
11.5 It is permitted to assume that data meeting the criteria 12.1.6 Temperature at which the test was run,
of 11.4 are part of the original data set and to determine a new 12.1.7 Graph of 10.2.5,
regression line using all failure points. Specimens which have 12.1.8 Calculations of 10.2.1, and
not failed after 1200 hours are not suitable for establishing a 12.1.9 Strain at 50 years for the mean and the value for r.
new regression line; however, it is permitted to use these points
for the purpose of reconfirmation. 13. Precision and Bias
11.6 If the data fails to satisfy the criteria of 11.4, the 13.1 No precision and bias statement can be made for this
changes are considered major and a new regression line must test method since controlled round-robin test programs have
be established. While the new test program is being conducted, not been run. This test method is generally used to evaluate
an interim Sb value for the material or process change may be large-diameter fiberglass pipe.
taken as the lower of the following calculations:
11.6.1 The 95 % lower confidence limit of the value ob- 14. Keywords
tained by extrapolating the failure points of 11.3 to 438 000 h 14.1 constant load; deflection; end point; fiberglass pipe;
(50 years) by the procedure in Annex A1. pipe-ring specimens; regression line; ring-bending strain

ANNEX

(Mandatory Information)

A1. LEAST SQUARES CALCULATION FOR LONG TERM RING-BENDING STRAIN

A1.1 General A1.2 Procedure for Analysis of Data


A1.1.1 The analysis is based on the following relationship: A1.2.1 Use a linear functional relationship analysis to
y 5 a1bx (A1.1) analyze n pairs of data values (as y and x) to obtain the
following information:
where: A1.2.1.1 The slope of line, b,
y = one variable, A1.2.1.2 The intercept on the y axis, a,
x = other variable, A1.2.1.3 The correlation coefficient, r, and
b = slope of the line, and A1.2.1.4 The predicted mean and the lower 95 % confi-
a = intercept on the y axis. dence and prediction intervals on the mean value.
A1.1.2 A linear functional relationship analysis (sometimes
called “covariance analysis”) is used, subject to tests for the A1.3 Assignment of Variables
sign (that is, “+” or “−”) of the slope and the coefficient of A1.3.1 Let x be log10t, where t is the time, in hours, and let
correlation for the quantity of data available. The relevant y be log10V, where V is the stain value.
equations are given together with example data and results, on
the basis of which any other statistical computing package may A1.4 Functional Relationship Equations and Method of
be used subject to validation by agreement with the example Calculation
results to within the indicated limits. A1.4.1 Basic Statistics and Symbols:
A1.1.3 For the purposes of this annex, a design service life A1.4.1.1 The following basic statistics and symbols are
of 50 years has been assumed. used:

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D5365 − 18

n = number of pairs of observed data values (Vi, ti), TABLE A1.1 Minimum Values for the Coefficient of Correlation, r,
for Acceptable Data From n Pairs of Data
yi = log10 of Vi, where Vi is the strain at failure of Observa-
tion i; i = 1, . . . n, n n-2 Minimum r
Number of variables Degrees of freedom
xi = log10 of ti, where ti is the time to failure in hours of 3 1 0.9999
Observation i; i = 1, . . .n, 4 2 0.9900
ȳ = arithmetic mean of all yi values: 5 3 0.9587
6 4 0.9172
1 7 5 0.8745
5
n (y i (A1.2) 8
9
6
7
0.8343
0.7977
10 8 0.7646
x̄ = arithmetic mean of all xivalues: 11 9 0.7348
12 10 0.7079
1 13 11 0.6835
5
n (x i (A1.3) 14 12 0.6614
15 13 0.6411
A1.4.2 Relevant Sums-of-Squares: 16 14 0.6226
17 15 0.6055
A1.4.2.1 Calculate the following sums-of-squares and 18 16 0.5897
cross-products: 19 17 0.5751
20 18 0.5614
1 21 19 0.5487
S xy 5
n ( ~ x 2 x̄ !~ y 2 ȳ !
i i (A1.4) 22 20 0.5368
23 21 0.5256
A1.4.2.2 If Sxy > 0, consider the data unsuitable for evalu- 24 22 0.5151
25 23 0.5052
ating the material; otherwise calculate also: 26 24 0.4958
1 27 25 0.4869
S xx 5
n ( ~ x 2 x̄ !
i
2
(A1.5) 32
37
30
35
0.4487
0.4182
42 40 0.3932
1
S yy 5
n ( ~y i 2 ȳ ! 2
(A1.6) 47
52
45
50
0.3721
0.3542
62 60 0.3248
A1.4.3 Correlation of Data: 72 70 0.3017
A1.4.3.1 Calculate the coefficient of correlation, r, from the 82 80 0.2830
92 90 0.2673
following relationship: 102 100 0.2540

2
~ S xy! 2
r 5 (A1.7)
~ S xx 3 S yy!
Yi, for true y and the error variance, σδ2, for x using Eq A1.12,
r 5 =r 2
Eq A1.13, and Eq A1.14, respectively:
A1.4.3.2 If the value of r is less than the applicable ξ i 5 $ λx i 1 ~ y i 2 a ! b % /2λ (A1.12)
minimum value given in Table A1.1as a function of n, reject Y i 5 a1bξ i (A1.13)
the data; otherwise, proceed to A1.4.4.
σδ 2 5 $ ( ~ y 2 Y ! 1λ ( ~ x
i i
2
i 2 ξ i! 2
%/$λ~n 2 2!% (A1.14)
A1.4.4 Functional Relationships:
A1.4.5.3 Calculate the following quantities:
A1.4.4.1 To find a and b for the functional relationship line,
y = a + bx (Eq A1.1), first set: τ 5 bσ δ 2 /2S xy (A1.15)

S D
2
S yy D 5 2λbσ δ /nSxy (A1.16)
λ5 (A1.8)
S xx B 5 2Dx̄ ~ 11τ ! (A1.17)
and then let: A1.4.5.4 Calculate the following variances: the variance,
C, of b using the formula:
b 5 2 =λ (A1.9)
C 5 D ~ 11τ ! (A1.18)
and then:
the variance, A, of a using the formula:
a 5 ȳ 2 bx̄ (A1.10)
NOTE A1.1—Since y = log10V and x = log10t, hence V = 10y, t = 10x and
the implied relationship for V in terms of t is therefore:
H
A 5 D x̄ 2 ~ 11τ ! 1
S xy
b J (A1.19)

V 5 10~ a1b3log 10 t ! the variance, σn2, of the fitted line at xL using the formula:
A1.4.5 Calculation of Variances: σ n 2 5 A12BxL 1CxL 2 (A1.20)
A1.4.5.1 If tL is the applicable time to failure, then set: the error variance, σε2, for y using the formula:
x L 5 log10t L (A1.11) σ ε 2 5 2λσ δ 2 (A1.21)
2
A1.4.5.2 Calculate, in turn, the following sequence of sta- the total variance, σy , for future values, yL, for y at xL using
tistics. For i= 1 to i = n, the best fit, ξi, for true x, the best fit, the formula:

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D5365 − 18
TABLE A1.2 Student’s “t” Value σy = value obtained in accordance with Eq A1.23, and
(Two-Sided 0.05 Level of Significance)
tv = applicable value for Student’s t for v = n − 2 degrees of
n n-2 Student’s freedom, as given in Table A1.2 for a two-sided 0.05
Number of variables Degrees of freedom t(0.05)
3 1 12.706 level of significance (that is, mean 62.5 %).
4 2 4.303
5 3 3.182 A1.4.6.2 Calculate the corresponding lower 95 % prediction
6 4 2.776 limit for V using the relationship:
7 5 2.571
8 6 2.447 V L 0.95 5 10Y L 0.95 (A1.26)
9 7 2.365
10 8 2.306
11 9 2.262
A1.4.6.3 The predicted mean value of V at time tL, that is,
12 10 2.228 VL, is given by the relationship:
13 11 2.201
14 12 2.179 V L 5 10Y L (A1.27)
15 13 2.160
16 14 2.145 where:
17 15 2.131 YL = value obtained in accordance with Eq A1.24
18 16 2.120
19 17 2.110
20 18 2.101
A1.4.6.4 Setting σy2 = σn2 in Eq A1.22 will produce a
21 19 2.093 confidence interval for the line rather than a prediction interval
22 20 2.086 for a future observation.
23 21 2.080
24 22 2.074
25 23 2.069
A1.5 Example Calculation
26 24 2.064
27 25 2.060 A1.5.1 Basic Data—The example data given in Table A1.3,
32 30 2.042 together with the example analysis given in this subsection, can
37 35 2.030
42 40 2.021
be used to validate statistical packages or procedures. Because
47 45 2.014 of rounding errors, it is unlikely that there will be exact
52 50 2.009 agreement, but acceptable procedures should agree within
62 60 2.000
72 70 1.994 60.1 % of the results given in A1.5.6.
82 80 1.990
92 90 1.987 A1.5.2 Sums of Squares:
102 100 1.984
Sxx = 0.7981093
Syy = 8.365498 × 10−4
σ y 2 5 σ n 2 1σ ε 2 (A1.22) Sxy = −0.024165
A1.4.5.5 Calculate the estimated standard deviation, σy, for A1.5.3 Coeffıcient of Correlation:
yL using the equation:
2
r = 0.935215
σy 5 ~σ n 1σ ε 2 ! 0.5 (A1.23)
A1.5.4 Functional Relationships:
and the predicted value, yL, for y at xL using the relationship:
y L 5 a1bxL (A1.24) λ = 1.048164 × 10−3
b = −3.237537 × 10−2
where a and b have the values obtained in accordance with a = 0.1372625
Eq A1.9 and Eq A1.10.
A1.5.5 Calculated Variances:
A1.4.6 Calculation and Confidence Intervals:
A1.4.6.1 Calculate the lower 95 % prediction interval, D = 4.84063 × 10−6
yL 0.95, predicted for yL using the equation: B = −1.470945 × 10−5
y L 0.95 5 y L 2 t v σ y (A1.25)
C (variance of b) = 5.01947× 10−6
A (variance of a) = 4.671877 × 10−5
where: σn2 (error variance for x) = 0.0515264
yL = value obtained in accordance with Eq A1.24 when xL is, σε2 (error variance for y) = 1.1157 × 10−4
as applicable, the value in accordance with Eq A1.11 A1.5.6 Confidence Limits—For N = 32 and Student’s t of
appropriate to a design life of, for example, 50 years 2.0423, the estimated mean and confidence and prediction
(that is, xL = 5.6415 (h)) or to a time at which it is intervals are given in Table A1.4.
desired to predict with 95 % confidence the minimum
value for the next observation of V,

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D5365 − 18
TABLE A1.3 Example Data For Example Calculation
Observation Number x(Time) Variable LOG x Variable y(Strain) Variable LOG y Variable

1 5184 3.714641 1 0
2 2230 3.348283 1 0
3 2220 3.346331 1.03 1.283708E-02
4 12340 4.091289 1.03 1.283708E-02
5 10900 4.037401 1.03 1.283708E-02
6 12340 4.091289 1.03 1.283708E-02
7 10920 4.038197 1.03 1.283708E-02
8 8900 3.949365 1.05 2.118911E-02
9 4173 3.620425 1.05 2.118911E-02
10 8900 3.949365 1.05 2.118911E-02
11 878 2.943476 1.05 2.118911E-02
12 4110 3.613819 1.07 2.938355E-02
13 1301 3.114257 1.07 2.938355E-02
14 3816 3.581585 1.07 2.938355E-02
15 669 2.825408 1.07 2.938355E-02
16 1430 3.155316 1.09 3.742624E-02
17 2103 3.322818 1.09 3.742624E-02
18 589 2.770098 1.09 3.742624E-02
19 1710 3.232975 1.09 3.742624E-02
20 1299 3.113589 1.09 3.742624E-02
21 272 2.434553 1.14 5.690446E-02
22 446 2.649318 1.14 5.690446E-02
23 466 2.668369 1.14 5.690446E-02
24 684 2.835038 1.14 5.690446E-02
25 104 2.01702 1.18 7.188151E-02
26 142 2.152274 1.18 7.188151E-02
27 204 2.309615 1.18 7.188151E-02
28 209 2.320131 1.18 7.188151E-02
29 9 0.9542362 1.25 9.690937E-02
30 13 1.113936 1.25 9.690937E-02
31 17 1.230441 1.25 9.690937E-02
32 17 1.230441 1.25 9.690937E-02

TABLE A1.4 Confidence Limits


Lower Confidence Lower Prediction
Time (hours) Mean Interval Interval

1 1.37 1.33 1.29


10 1.27 1.25 1.20
100 1.18 1.17 1.12
1000 1.10 1.09 1.04
10000 1.02 1.00 0.97
100000 0.94 0.92 0.89
438000 0.90 0.87 0.85

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D5365 – 12) that may impact the use of this standard (August 1, 2018).

(1) Clarified the intent and use of data for reconfirmation (3) Revised Tables A1.1 and A1.2 to unify range of variables
testing—Section 11. considered.
(2) Eliminated instances of non-mandatory language.

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D5365 − 18
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
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address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5418 − 15

Standard Test Method for


Plastics: Dynamic Mechanical Properties: In Flexure (Dual
Cantilever Beam)1
This standard is issued under the fixed designation D5418; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* priate safety and health practices and determine the applica-
1.1 This test method outlines the use of dynamic mechanical bility of regulatory limitations prior to use.
instrumentation for determining and reporting the viscoelastic NOTE 1—There is no known ISO equivalent to this standard.
properties of thermoplastic and thermosetting resins and com-
posite systems in the form of rectangular bars molded directly 2. Referenced Documents
or cut from sheets, plates, or molded shapes. The elastic 2.1 ASTM Standards:2
modulus data generated may be used to identify the thermo- D618 Practice for Conditioning Plastics for Testing
mechanical properties of a plastics material or composition. D4065 Practice for Plastics: Dynamic Mechanical Proper-
1.2 This test method is intended to provide a means for ties: Determination and Report of Procedures
determining the viscoelastic properties of a wide variety of D4092 Terminology for Plastics: Dynamic Mechanical
plastics using nonresonant, forced-vibration techniques as Properties
outlined in Practice D4065. In particular, this method identifies D5279 Test Method for Plastics: Dynamic Mechanical Prop-
the procedures used to measure properties using what is known erties: In Torsion
as a dual-cantilever beam flexure arrangement. Plots of the 3. Terminology
elastic (storage) modulus, loss (viscous) modulus, and complex
modulus, and tan delta as a function of frequency, time, or 3.1 For definitions applicable to this practice see Terminol-
temperature are indicative of significant transitions in the ogy Standard D4092.
thermomechanical performance of the polymeric material sys-
4. Summary of Test Method
tems.
4.1 This test method covers the determination of the elastic
1.3 This test method is valid for a wide range of frequencies,
modulus of plastics using dynamic mechanical techniques. A
typically from 0.01 to 100 Hz.
bar of rectangular cross section is tested as a beam in dynamic
1.4 Apparent discrepancies may arise in results obtained linear displacement or bending. The dual-cantilever beam
under differing experimental conditions. These apparent differ- specimen is gripped between two clamps. The specimen of
ences from results observed in another study can usually be known geometry is placed in mechanical linear displacement,
reconciled, without changing the observed data, by reporting in with the displacement strain or deformation applied at the
full (as described in this test method) the conditions under center of the dual-cantilever beam. The forced-strain displace-
which the data were obtained. ment is at either a fixed frequency or variable frequencies, and
1.5 Test data obtained by this test method are relevant and at either isothermal conditions or with a linear temperature
appropriate for use in engineering design. variation. The elastic or loss modulus, or both, of the polymeric
material system are measured in flexure.3
1.6 The values stated in SI units are to be regarded as
standard. 5. Significance and Use
1.7 This standard does not purport to address all of the 5.1 This test method provides a simple means of character-
safety concerns, if any, associated with its use. It is the izing the thermomechanical behavior of plastic compositions
responsibility of the user of this standard to establish appro- using a very small amount of material. Since small test

2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
and is the direct responsibility of Subcommittee D20.10 on Mechanical Properties. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 1, 2015. Published July 2015. Originally approved the ASTM website.
3
in 1993. Last previous edition approved in 2007 as D5418 - 07. DOI: 10.1520/ The particular method for measurement of the elastic and loss moduli and tan
D5418-15. delta depends upon the individual instrument’s operating principles.

*A Summary of Changes section appears at the end of this standard


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D5418 − 15
specimen geometries are used, it is essential that the specimens 6.2.3.1 The test specimen shall be held in such a way that
be representative of the material being tested. The data slippage relative to the grips is minimized as much as possible.
obtained can be used for quality control and/or research and 6.2.4 Deformation (Strain) Device—A device for applying a
development purposes. For some classes of materials, such as continuous linear deformation (strain) to the specimen. In the
thermosets, it can also be used to establish optimum processing force-displacement device the deformation (strain) is applied
conditions. and then released (see Table 1 of Practice D4065).
5.2 Dynamic mechanical testing provides a sensitive means 6.2.5 Detectors—A device or devices for determining de-
for determining thermomechanical characteristics by measur- pendent and independent experimental parameters, such as
ing the elastic and loss moduli as a function of frequency, force (stress), deformation (strain), frequency, and temperature.
temperature, or time. Plots of moduli and tan delta of a material Temperature should be measurable with a precision of 61°C,
versus these variables can be used to provide a graphic frequency, strain, and force to 61 %.
representation indicative of functional properties, effectiveness 6.2.6 Temperature Controller and Oven—A device for con-
of cure (thermosetting-resin systems), and damping behavior trolling the temperature, either by heating (in steps or ramps),
under specified conditions. cooling (in steps or ramps), or maintaining a constant specimen
environment, or a combination thereof. A temperature control-
5.3 This test method can be used to assess the following:
ler should be sufficiently stable to permit measurement of
5.3.1 The modulus as a function of temperature or aging, or
environmental chamber temperature to within 1°C.
both,
5.3.2 The modulus as a function of frequency, 6.3 Nitrogen, or other inert-gas supply for purging purposes
5.3.3 The effects of processing treatment, including if appropriate.
orientation, induced stress, and degradation of physical and
chemical structure, 7. Test Specimens
5.3.4 Relative resin behavioral properties, including cure 7.1 The specimens may be cut from sheets, plates, or
and damping, molded shapes or may be molded to the desired finished
5.3.5 The effects of substrate types and orientation (fabri- dimensions. Any rectangular specimen (representative of the
cation) on elastic modulus, material being tested and within the fixturing capabilities of the
5.3.6 The effects of formulation additives that might affect test equipment) is permitted as long as it is clearly stated in the
processability or performance, test report.
5.3.7 The effects of annealing on modulus and glass transi-
tion temperature, 8. Calibration
5.3.8 The effect of aspect ratio on the modulus of fiber 8.1 Calibrate the instrument according to procedures recom-
reinforcements, and mended by the manufacturer.
5.3.9 The effect of fillers, additives on modulus and glass
transition temperature. 9. Conditioning
5.4 Before proceeding with this test method, refer to the 9.1 Conditioning—Condition the test specimens at 23.0 6
specification of the material being tested. Any test specimen 2.0°C and 50 6 10 % relative humidity for not fewer than 40
preparation, conditioning, dimensions, or testing parameters, or h prior to test in accordance with Procedure A of Practice D618
combination thereof, covered in the relevant ASTM material unless otherwise specified by contract or relevant ASTM
specification shall take precedence over those mentioned in this material specification.
test method. If there are no relevant ASTM material
specifications, then the default conditions apply. 10. Procedure
6. Apparatus 10.1 Use an untested specimen for each measurement.
Measure the width and thickness of the specimen to the nearest
6.1 The function of the apparatus is to hold a rectangular
0.03 mm (0.001 in.) at the center of the specimen.
cross-sectional bar so that the material acts as the elastic and
dissipative element in a mechanically driven linear displace- 10.2 Clamp the test specimen between the movable and
ment system. Dynamic mechanical instruments described in stationary members; use shim stock, if necessary, to minimize
this standard generally operate in a forced, constant amplitude slippage within the clamp.
mode at either a fixed frequency or variable frequencies. 10.3 Pre-load the test specimen so that there is a positive
6.2 The apparatus consists of the following: force. The positive pre-load should be sufficient to maintain a
6.2.1 Fixed Grips—A fixed or essentially stationary fixture positive deflection during testing unless the test mode allows a
consisting of two grips to secure the rectangular specimen zero-displacement measurement.
horizontally in a dual cantilever configuration. 10.4 Measure the length of the specimen between the
6.2.2 Movable Grip—A movable grip applying the linear stationary end grips to the nearest 0.03 mm (0.001 in.).
displacement at the center of the rectangular beam.
6.2.3 Grip Alignments—The grips shall be mechanically 10.5 Select the desired frequency (or frequencies) for dy-
aligned or centered, that is, they shall be attached in such a namic linear displacement.
manner that they will move into alignment as soon as any load 10.6 Select the linear displacement amplitude within the
is applied. linear elastic region of the material being tested. If the linear

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D5418 − 15
elastic region is not known, perform a strain sweep at ambient 12.1.14 A plot of the modulus (moduli) and tan delta as a
temperature to determine an appropriate amplitude. function of temperature or of time as appropriate (see Fig. 1).
10.7 Temperature Sweep: 13. Precision and Bias
10.7.1 Temperature variations shall be controlled to 1 to
2°C/min for linear increases or to 2 to 5°C/min with a 13.1 The repeatability standard deviation has been deter-
minimum of 1-min thermal-soak time for step increases. mined for the following materials. A single laboratory evalu-
ated a polyurethane sample and the values in Table 1 were
10.8 The tan delta peak will coincide with a significant obtained with the same test method in the same laboratory by
decrease in the E' (elastic or storage) modulus, with increasing the same operator using the same equipment in the shortest
temperature, through the glass-transition region. Another indi- practical period of time using test specimens taken at random
cation of the glass-transition is a maximum value of the E" from a single quantity of homogeneous material. This labora-
(loss or viscous) modulus. tory tested the same polyurethane material used for the
11. Calculation precision and bias statement in Test Method D5279 and
obtained the results in Table 1.
11.1 The equations listed in Practice D4065 are used to TABLE 1 Dual Cantilever Beam, Elastic Modulus, E' (E9 Pa) or
calculate the important rheological properties measured in (E10 dynes/cm2) at Selected Temperatures
forced, nonresonant dynamic displacement where: –40°C 0°C
Mean 1.162 0.04953
E' = storage (elastic) modulus in bending, Standard deviation 0.004 0.00373
E" = loss (viscous) modulus in bending,
E* = complex modulus in bending, and 14. Keywords
Tanδ = tan delta. 14.1 dual cantilever; dynamic mechanical rheological prop-
erties; linear displacement; modulus storage; viscous; loss
12. Report
modulus; complex; tan delta; viscoelastic behavior
12.1 Report the following information:
12.1.1 Complete identification of the material tested, includ-
ing type, source, manufacturer’s code, number, form, principal
dimensions, and previous processing or thermal history, or
both, if available,
12.1.2 Description and direction of cutting and loading
specimen, including pre-load force,
12.1.3 Conditioning procedure,
12.1.4 Description of the instrument used for the test,
12.1.5 Description of the calibration procedure,
12.1.6 Identification of the sample atmosphere by gas
composition, purity, and rate used if appropriate,
12.1.7 Width and thickness of specimen,
12.1.8 Grip separation distance of the beam,
12.1.9 Frequency of dynamic displacement,
12.1.10 Amplitude of displacement,
12.1.11 Thermal gradient; heating rate, if appropriate,
12.1.12 Number of specimens tested,
12.1.13 Table of data and results, including moduli and tan FIG. 1 Dynamic Mechanical Modulus in Bending as a Function of
delta as a function of temperature or of time as appropriate, and Temperature at Different Frequencies

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D5418 − 15
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5418 - 07)
that may impact the use of this standard. (July 1, 2015)

(1) Added 5.3.7, 5.3.8, and 5.3.9. (3) Revised the title of Table 1.
(2) Revised 9.1, 11.1, and 12.1.11.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5419 − 14a

Standard Test Method for


Environmental Stress Crack Resistance (ESCR) of Threaded
Plastic Closures1
This standard is issued under the fixed designation D5419; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D2911 Specification for Dimensions and Tolerances for


1.1 This test method determines the susceptibility of Plastic Bottles
threaded plastic closures to failure due to environmental stress E145 Specification for Gravity-Convection and Forced-
cracking (ESC). Ventilation Ovens
E691 Practice for Conducting an Interlaboratory Study to
1.2 In use, threaded plastic closures can contact agents that Determine the Precision of a Test Method
appreciably reduce the stress at which cracks form. Examples
of such agents are: soaps, detergents, oils, and liquid bleaches. 3. Terminology
1.3 Major factors that influence environmental stress crack 3.1 Definitions—Except for those terms below, see Termi-
resistance (ESCR) of threaded plastic closures include the nologies D883 and D1600.
closure material(s), closure design, molded-in stress, and
applied stress. 3.2 Definitions of Terms Specific to This Standard:
3.2.1 assembly—closure applied to a bottle finish.
1.4 This procedure can be applied to all closures, but is
particularly applicable to closures made from plastics based on 3.2.2 failure—during this test, any visible crack.
polypropylene (PP) or polystyrene (PS). 3.2.2.1 Discussion—A crack does not have to penetrate the
closure wall to be considered a failure.
1.5 The values stated in inch-pound units are to be regarded
3.2.3 finish—fixture representing the threaded portion of the
as the standard. The values given in parentheses are for
bottle.
information only.
3.2.4 threaded closure—part applied to seal bottle as speci-
1.6 This standard does not purport to address all of the
fied in Specification D2911.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau- 4.1 This test method consists of applying closures at a
tionary statements are given in Section 8 and 6.2. specified application torque to rigid finishes (of polysulfone or
other appropriate resin), immersing the assembly in a potential
NOTE 1—There is no known ISO equivalent to this standard.
stress-cracking agent, and observing and reporting time-to-
2. Referenced Documents failure.
2.1 ASTM Standards:2
5. Significance and Use
D618 Practice for Conditioning Plastics for Testing
D883 Terminology Relating to Plastics 5.1 This test method compares closures for ESCR. Suitable
D1600 Terminology for Abbreviated Terms Relating to Plas- variables are: closure materials, closure designs, processes,
tics applied torque, and stress-crack agents.
5.2 Results can be used for estimating shelf life of closures
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics in terms of ESCR. This requires that the user has calibrated
and is the direct responsibility of Subcommittee D20.19 on Film, Sheeting, and failure time in this test to failure time in the field for actual
Molded Products. packaging systems.
Current edition approved Dec. 1, 2014. Published December 2014. Originally
approved in 1993. Last previous edition approved in 2014 as D5419 – 14. DOI:
10.1520/D5419-14A. 6. Apparatus
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1 Wide-Mount Gallon Jars, glass, PET, or other suitable
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on material. Must have lined closures to ensure air-tight seal. Use
the ASTM website. one jar per sample.

*A Summary of Changes section appears at the end of this standard


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D5419 − 14a

NOTE 1—Tolerances for Dimensions T, E, and S shall be in accordance with Specification D2911.
FIG. 1 Typical Fixture

6.2 Circulating-Air Oven, capable of maintaining a tem- 6.6 Plastic Test Closures, lined or unlined closure based on
perature of 50 6 1°C (critical in this application). See specifications.
Specification E145 for a procedure for confirming satisfactory NOTE 2—To ensure that full crystallization has essentially been
uniformity of temperature within the oven. There is no air-flow achieved, PP-based closures should condition for at least three weeks
requirement in this application. An environmental room with before testing and PS closures for at least 16 h.
these properties is also suitable. (Warning—A high- NOTE 3—To convert lbf-in. torque to Nm torque, multiply by 0.113.
temperature safety switch is highly recommended on this oven.
7. Reagents and Materials
Some test liquids can cause extreme pressure to build up upon
heating. Under these conditions it is possible that the test jars 7.1 Test Solution—Use solution for which the closure is
will rupture with explosive force. Set the override cutoff switch intended.
to turn off the oven if the test temperature is exceeded by 10°C 8. Hazards
or more.)
8.1 Always wear protective equipment, such as goggles,
6.3 Tongs, for sample removal and inspection. gloves, and aprons, appropriate to the product hazard when
6.4 Bottle Finishes, polysulfone or other material of equiva- setting up or inspecting closures.
lent stiffness and thermal coefficient of expansion, to which
closures are applied. These can be made by injection molding 9. Test Specimens
or by machining rod stock. See Fig. 1 for a drawing of a typical 9.1 Normal sample size is 20 closures, typical of lots to be
fixture. Use an appropriate size based on closure and bottle tested. It is strongly advisable to run the test in duplicate (two
specifications. sets of 20) or to sample more than one lot.
6.5 Torque Meter, with capacity of at least 5 torque Nm, 9.2 Visually inspect each closure to be tested. Replace any
calibrated or verified within the past 12 months. that appear defective or irregular.

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D5419 − 14a
10. Conditioning
10.1 Conditioning—After aging in accordance with 6.6,
condition closures and bottle finishes at 23 6 2°C and 50 6
10 % relative humidity for not less than 40 h prior to test, in
accordance with Procedure A of Practice D618 unless other-
wise specified by agreement or the relevant ASTM material
specification. Condition test solution at 50 6 1°C until it
reaches 50 6 1°C (16 h normally required).
10.2 Test Conditions—Conduct all tests at 50 6 2°C, unless
instructed otherwise.

11. Procedure
11.1 Apply closures to bottle finishes. Unless otherwise
specified, apply torque to a tolerance of 65 % using one of the
following values:
11.1.1 A value corresponding to the upper limit of immedi-
ate removal torque in production (rule of thumb: application
torque = 1.05 × immediate removal torque), or
11.1.2 A nominal value based on the closure diameter (rule
of thumb: torque, Nm = closure diameter, mm × 0.08), or
11.1.3 A value agreed upon between the laboratory and the
customer.
11.1.4 Firmly position the bottle finish between the four
posts on the torque tester in such a manner that the axis of
rotation of the cap is concentric with the center of the movable FIG. 2 F50 Failure Time
plate on which the bottle finish rests.
11.1.5 Grip the closure by hand, avoiding any contact with
the bottle finish, and twist clockwise while closely watching and a total of at least 11 out of 20 closures have failed. Record
the gauge. Apply torques smoothly and consistently, at a inspections even on days when there are no failures.
constant rate consistent with accurate reading of the gauge.
NOTE 5—If testing against an F50 specification, the test may be
11.1.6 Apply torque continuously until the desired torque as terminated if no more than 1 closure out of 20 fails by the specification
indicated by the needle on the gauge is reached. time.
11.2 Place 20 assemblies in jars. Fill jars with enough test
solution at 50 6 1°C to cover all assemblies. Wipe any test 12. Calculation
solution from jar-finish area. Cap jars and hand tighten. 12.1 Calculate closures predicted to fail at any given time
11.3 Place jars on test at 50 6 1°C. Check and record the by the following equation:
temperature of test area daily and maintain it within the failures, % 5 @ ~ n 2 0.5! /N # 3 100 (1)
specified limits. where:
11.4 Inspect the assemblies daily except on weekends. n = cumulative number of closures that have failed as of
Move jars from test condition to inspection area. Do not allow the given time, and
to be off test more than 60 min. Remove the assemblies N = number of closures tested (20 unless otherwise stated).
individually, using tongs on the bottle finishes, not the closures.
NOTE 4—It is recommended that the inspection frequency be increased 12.2 F25 Failure Time—Plot the data on Weibull probability
during periods of known high-failure rates. Delaying the start of the graph paper with days on the log scale and percent failure on
second duplicate sample facilitates this; however, frequency of torque
reapplication should remain at daily intervals except on weekends.
the probability scale. When more than one closure fails on a
given inspection, use the average % failing on that inspection
11.5 After inspection, set aside failures. Reapply initial for the plotting position (see the example in Appendix X1).
torque to nonfailing closures, return them to jars and move jars Draw the best fitting straight line for the plot. The days
back to test condition. Do not remove or loosen closures. If test indicated at the intersection of the data line with the 50 %
solution degrades with age, replace it often enough that the failure level probability line shall be reported as the F50 failure
failure rate is not significantly reduced. If closure cracks on time. See Fig. 2 for example.
retorqueing, count this as a failure on the next inspection.
NOTE 6—The plot or calculations, or both, may be made on computer
11.6 For each failure, note the time, description, and loca- with suitable software.
tion of failure.
11.7 Any sample (jar) can be removed and the test termi- 13. Report
nated when there have been failures on at least two inspections, 13.1 Report the following information:

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D5419 − 14a
TABLE 1 F50, Days precision of this test method. Do not apply the data in Table 1
Closures Tested
Average Sr A
SR B
r C
R D rigorously to the acceptance or rejection of material, as those
in Bleach data are specific to the round robin and are not necessarily
28 mm- 5.1 0.8 1.5 2.2 4.1
Polypropylene representative of other lots, conditions, materials, or laborato-
A
Sr is the within-laboratory standard deviation.
ries. Users of this test method need to apply the principles
B
SR is the between-laboratories standard deviation. outlined in Practice E691 to generate data specific to their
C
r is the within-laboratory repeatability limit = 2.8 Sr . laboratory and materials or between specific laboratories. The
D
R is the between-laboratory reproducibility limit = 2.8 SR .
principles of 14.1.1.1 – 14.1.1.3 would then be valid for such
data.)
13.1.1 Closure identification, specification number (if 14.1.1 Concept of r and R—if Sr and SR have been calculated
applicable), manufacturer, molding location, molding date, lot from a large enough body of data,
number, liner description (if applicable), molding machine, 14.1.1.1 Repeatability, (r)—(Comparing two test results for
resin, mold and cavity number(s), process conditions, the same material, obtained by the same operator using the
13.1.2 Test solution name and composition/analysis, same equipment on the same day.) Judge the two test results as
13.1.3 Application torque, not equivalent if they differ by more than the r value for that
13.1.4 Date and time of each inspection and location of each material.
failure, and 14.1.1.2 Reproducibility, (R)—(Comparing two test results
13.1.5 Failure time (F50 ). for the same material, obtained by different operators using
different equipment on different days.) Judge the two test
14. Precision and Bias3 results as not equivalent if they differ by more than the R value
14.1 Precision—Table 1 is based on a round robin con- for that material.
ducted in 1995 in accordance with Practice E691, involving 14.1.1.3 Any judgment determined in accordance with
one material tested by 12 laboratories. All of the samples were 14.1.1.1 and 14.1.1.2 would have an approximate 95 % (0.95)
prepared at one source. Each test result was based on 20 probability of being correct.
individual determinations. Each laboratory obtained two test 14.2 Bias—There are no recognized standards by which to
results for each material. (Warning—The following explana- estimate the bias of this test method.
tions of r and R (14.1.1.1 – 14.1.1.3) are only intended to
present a meaningful way of considering the approximate 15. Keywords
15.1 closures; environmental stress crack resistance
3
A research report is currently being written. (ESCR); failure; plastic; stress crack; threaded plastic closures

APPENDIX

(Nonmandatory Information)

X1. EXAMPLE OF GRAPHICAL DETERMINATION OF F50

TABLE X1.1 Data TABLE X1.2 Plotting Positions for n = 20


No. of Days No. of Closures Failing Total No. of Closures No. of Closures Failed Plotting Position, %
on Test on This Date Failed to Date 1 2.5
3 0 0 2 7.5
4 0 0 3 12.5
5 10 10 4 17.5
6 9 19 5 22.5
6 27.5
7 32.5
8 37.5
9 42.5
X1.1 Data (See Table X1.1): 10 47.5
11 52.5
X1.2 Plotting Positions for n = 20 (See Table X1.2): 12 57.5
13 62.5
X1.3 X-Axis Values for Example: 14 67.5
15 72.5
X1.3.1 First failures occurred at 5 days, so the first X value 16 77.5
17 82.5
is 5 days. 18 87.5
X1.3.2 The second X value is 6 days. 19 92.5
20 97.5
X1.3.3 The test terminated after 6 days (19 failures).
X1.4 Y-Axis Values for Example:

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D5419 − 14a
X1.4.1 For the first point, the Y value is the average of the X1.4.3 Graph (See Fig. 2):
plot position for 1 and 10 closures failed
5 ~ 2.5147.5! /2 5 25 % (X1.1)
X1.5 Determination of F50 —Interpolate the line at the
“percent failing” value of 50 on the Y-axis, and read of f “days
X1.4.2 For the second point, the Y value is the average of to failure” on the X-axis.
the plot position for 11 and 19 closures failed
5 ~ 52.5192.5! /2 5 72.5 % (X1.2)

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5419 - 14)
that may impact the use of this standard. (December 1, 2014)

(1) Deleted reference to ASTM D3198 since it was withdrawn.


(2) Added appropriate directions to Section 11 (Procedure) to
address application of closures to bottle finish.

Committee D20 has identified the location of selected changes to this standard since the last issue (D5419 - 09)
that may impact the use of this standard. (November 15, 2014)

(1) Editorially changed the wording of the warning note in 6.2. (3) Added units of measurement to Fig. 1.
(2) Clarified the standard units statement in 1.5.

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5420 − 16

Standard Test Method for


Impact Resistance of Flat, Rigid Plastic Specimen by Means
of a Striker Impacted by a Falling Weight (Gardner Impact)1
This standard is issued under the fixed designation D5420; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D5947 Test Methods for Physical Dimensions of Solid


1.1 This test method covers the determination of the relative Plastics Specimens
ranking of materials according to the energy required to crack E171 Practice for Conditioning and Testing Flexible Barrier
or break flat, rigid plastic specimens under various specified Packaging
conditions of impact of a striker impacted by a falling weight. E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
only. 3. Terminology
1.3 This standard does not purport to address all of the 3.1 Definitions—For definitions of plastics terms used in
safety concerns, if any, associated with its use. It is the this test method, see Terminologies D883 and D1600.
responsibility of the user of this standard to establish appro- 3.2 Definitions of Terms Specific to This Standard:
priate safety and health practices and determine the applica-
3.2.1 failure (of test specimen)—the presence of any crack
bility of regulatory limitations prior to use.
or split created by the impact of the falling weight that can be
NOTE 1—There is no known ISO equivalent to this standard. seen by the naked eye under normal laboratory lighting
conditions.
2. Referenced Documents
3.2.1.1 Discussion—Failure shall include the following:
2.1 ASTM Standards:2 (1) complete shattering of the plaque; (2) any crack radiating
D618 Practice for Conditioning Plastics for Testing out toward the edges of the plaque on either surface of the
D883 Terminology Relating to Plastics plaque; (3) any radial crack within or just outside the impact
D1600 Terminology for Abbreviated Terms Relating to Plas-
area of the striker; (4) any hole in the plaque, whether due to
tics
brittle or ductile puncture, where unobstructed light or water
D2794 Test Method for Resistance of Organic Coatings to
could pass through; (5) any brittle splitting of the bottom
the Effects of Rapid Deformation (Impact)
D3763 Test Method for High Speed Puncture Properties of surface of the plaque; and (6) any glassy-type chip dislodged
Plastics Using Load and Displacement Sensors from or loosened from the plaque.
D4066 Classification System for Nylon Injection and Extru- 3.2.1.2 Discussion—Since the interpretation of failure may
sion Materials (PA) be slightly different between material types, refer to the
D4226 Test Methods for Impact Resistance of Rigid Poly- appropriate material specification for guidance.
(Vinyl Chloride) (PVC) Building Products 3.2.1.3 Discussion—Cracks usually start at the surface op-
D5628 Test Method for Impact Resistance of Flat, Rigid posite the one that is struck. For example, in some cases
Plastic Specimens by Means of a Falling Dart (Tup or incipient cracking in glass-reinforced polymers is difficult to
Falling Mass) differentiate from the reinforcing fibers. In such cases, apply a
penetrating dye such as gentian violet to the stressed surface to
determine the onset of crack formation.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.10 on Mechanical Properties. 3.2.2 mean-failure energy (mean impact resistance)—the
Current edition approved May 1, 2016. Published May 2016. Originally energy required to produce 50 % failures, equal to the product
approved in 1993. Last previous edition approved in 2010 as D5420 - 10. DOI:
10.1520/D5420-16.
of the constant mass and mean failure height.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 3.2.3 mean-failure height (impact-failure height)—the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on height at which a standard mass, when dropped on test
the ASTM website. specimens, will cause 50 % failures.

*A Summary of Changes section appears at the end of this standard


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D5420 − 16
in velocity. Hagan, et al (2) found that the mean-failure energy
of sheeting was constant at drop heights between 0.30 and 1.4
m. Different materials respond differently to changes in the
velocity of impact.
5.2 The test conditions used in Geometry GA are the same
as those used in Geometry FA of Test Method D5628 (see
Table 1).
5.3 The test conditions of Geometry GB are equivalent to
the geometry used for the Gardner Variable Height Impact Test
(3).
5.4 The test conditions of Geometry GC cause a punch-
shear type of failure because the support-plate hole is close to
the diameter of the striker.
5.5 The test conditions of Geometry GD are the same as
those in Test Method D3763.
5.6 The test conditions of Geometry GE are the same as
those in Test Method D4226, impactor head configuration
H.25.
5.7 Because of the nature of impact testing, the selection of
a test method and striker must be somewhat arbitrary. Consider
the end use environment and requirements when choosing from
the available striker geometries. The selection of any one of the
striker geometries is permitted.
NOTE 2—Material processing can have a significant affect on the
FIG. 1 Impact Tester development of a plastic’s physical properties. Consult relevant material
standards for processing guidelines

4. Summary of Test Method 6. Interferences


4.1 In this test method, a weight falls through a guide tube 6.1 Falling-weight-impact test results are dependent on the
and impacts a striker resting on top of a supported specimen. geometry of the falling weight, striker, and the support. Thus,
The fixed weight is dropped from various heights (see Fig. 1). use impact tests only to obtain relative rankings of materials.
Impact values cannot be considered absolute unless the geom-
4.2 The procedure determines the energy (mass × grav-
etry of the test equipment and specimen conform to the end-use
ity × height) that will cause 50 % of the specimens tested to fail
requirement. Data obtained with different geometries, cannot,
(mean-failure energy).
in general, be compared directly with each other.
4.3 The technique used to determine mean-failure energy is 6.1.1 Falling-weight-impact types of tests are not suitable
commonly called the Bruceton Staircase Method, or the for predicting the relative ranking of materials at impact
Up-and-Down Method (1).3 Testing is concentrated near the velocities differing greatly from those imposed by these test
mean, reducing the number of specimens required to obtain a methods.
reasonably precise estimate of the impact resistance.
6.2 As cracks usually start at the surface opposite the one
4.4 This test method permits the use of different striker that is struck, the results obtained can be greatly influenced by
diameters and specimen support plate geometries to obtain the surface characteristics of the test specimens. Therefore,
different modes of failure, permit easier sampling, or test factors including surface features (flaws, texturing, and so
limited amounts of material. There is no known means for
correlating the results of tests made by different methods or
procedures. TABLE 1 Striker and Specimen-Support-Plate Dimensions
Striker Diameter, Support Plate Inside Diameter, mm
5. Significance and Use Geometry
mm (in.) (in.)
5.1 Plastics are viscoelastic and it is possible that they are GA 15.86 ± 0.10 76.0± 3.0
(0.625 ± 0.004) (3.00 ± 0.12)
sensitive to changes in velocity of weights falling on their GB 15.86 ± 0.10 31.75± 0.025
surfaces. However, the velocity of a free-falling object is a (0.625 ± 0.004) (1.25 ± 0.001)
function of the square root of the drop height. A change of a GC 15.86 ± 0.10 16.26 ± 0.025
(0.625 ± 0.004) (0.640 ± 0.001)
factor of two in the drop height will cause a change of only 1.4 GD 12.70 ± 0.10 76.0 ± 3.0
(0.500 ± 0.004) (3.00 ± 0.12)
GE 12.70 ± 0.10 16.26 ± 0.025
3
The boldface numbers in parentheses refer to the list of references found at the (0.500 ± 0.004) (0.640 ± 0.001)
end of this test method.

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D5420 − 16
forth), surface composition, orientation due to specimen
preparation, and so forth, are important variables and will
influence results.
6.3 Impact properties of plastic materials can be very
sensitive to temperature. This test can be carried out at any
reasonable temperature and humidity, thus representing actual-
use environments. However, this test method is intended
primarily for rating materials under specific impact conditions.
6.4 It is possible that the apparatus used in this test method
will not have sufficient energy available to cause failure of
some specimens under the conditions of this procedure.

7. Apparatus
7.1 Testing Mechanism—The apparatus is shown in Fig. 1.
Adapt the apparatus from Test Method D2794 for use in this
test method or obtain the apparatus commercially. The appa-
ratus shall consist of the following: suitable base to withstand
the impact shock; steel-rod impact mass, weighing 0.9 kg (2
lb), 1.8 kg (4 lb), or 3.6 kg (8 lb); a hardened steel striker
having a round nose with diameter described in 7.2.1 and 7.2.2
and Table 1; a slotted guide tube 1.0 m (40 in.) in length, in
which the impact mass slides, having graduations in newton-
metres (inch-pound increments) or multiples thereof. Use a
bracket to hold the tube in a vertical position by attaching it to
the base and also to hold the hand knob, which is a pivot arm
alignment for the striker, about 50 mm (2 in.) under the tube.
Mount this instrument firmly to a rigid table or bench. Round
the top edge of the opening in each specimen-support plate to
a 1.0 6 0.2-mm (0.039 6 0.008-in.) radius, except in Geom- FIG. 2 Specimen-Support Plate Used for Geometries GA and GD
etry GE which has a radius of 0.75 mm (0.031 in.).
7.1.1 The tester shall be mounted so that the axis of the tube
is plumb when measured with a spirit level at least 300 mm (12
in.) in length.
7.2 Striker Geometries:
7.2.1 For Geometries GA, GB, and GC, the striker shall
have a rounded nose with a diameter of 15.86 6 0.10 mm
(0.625 6 0.004 in.).
7.2.2 For Geometries GD and GE the striker shall have a
rounded nose with a diameter of 12.70 6 0.1 mm (0.500 6
0.004 in.).
7.2.3 With Geometries GA and GD, a specimen-support
plate with a hole 76.0 6 3.0 mm (3.00 6 0.12 in.) in diameter
is mounted in the apparatus. A suggested design is given in Fig.
2.
7.2.4 With Geometry GB, the specimen-support plate has a
31.75 6 0.025-mm (1.25 6 0.001-in.) diameter hole. This
geometry can be achieved by removing the removable support
ring on the standard Gardner instrument.
FIG. 3 Striker/Specimen/Support Plate Configuration for Geom-
7.2.5 With Geometries GC and GE, the standard removable
etries GB and GC (Geometry GC Shown)
specimen-support plate, with a hole 16.26 6 0.025 mm (0.640
6 0.001 in.) in diameter, is mounted in the specimen support
anvil (see Fig. 3 for Geometry GC and Fig. 4 for Geometry base shall have maximum dimensions of 16 by 30 by 30 in.
GE). (height by width by depth). Place this block or base at a height
7.3 Supporting Base—In order to minimize the energy suitable for ease of operation. It is not necessary to bolt blocks
absorption, compression, and deflection of the support, affix or bases of this weight to the floor. Alternatively, affix testers
the tester to a dense, solid block or base weighing a minimum directly to the floor. Use of rubber mats either directly under
of 375 lb (see Appendix X2). The main body of the block or the tester or supporting apparatus is prohibited.

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9.3 When the approximate mean-failure height for a given
sample is known, 20 specimens will usually yield sufficiently
precise results. If the approximate mean-failure height is
unknown, six or more additional specimens shall be used to
determine the appropriate starting point of the test.
9.4 Visually examine the specimens to ensure they are free
of cracks or other obvious imperfections or damages, unless
these imperfections constitute variables under study. For speci-
fication purposes, do not test samples known to be defective.
Production parts shall be tested in the as-received condition to
determine conformance to specified standards.
NOTE 1—Depth of penetration when fully seated shall be 12.2 6 0.1
mm (0.48 6 0.04 in.). 9.5 Select a suitable method for making the specimen that
FIG. 4 Striker/Specimen/Support Plate Configuration for Geom- will minimize the effect of specimen preparation on the impact
etry GE resistance of the material. Refer to the appropriate material
specification for requirements for specimen preparation.
NOTE 3—Such block dimensions conform to commercially available NOTE 5—As few as ten specimens often yield sufficiently reliable
butcher block tables. estimates of the mean-failure height. However, in such cases the estimated
7.3.1 Bolt supporting bases or tables lighter than 375 lb to a standard deviation will be relatively large (1).
concrete floor. For each different material tested, make com-
parisons between mean failure energy data generated using this 10. Conditioning
support and one where the tester is fixed directly to the 10.1 Unless otherwise specified by contract or relevant
concrete floor. If mean failure energy differences between two material specification, condition the test specimens in accor-
types of supports are found to be statistically nonsignificant, dance with Procedure A of Practice D618 or Specification
use of the lighter support shall be allowed. E171, for those tests where conditioning is required. Tempera-
7.3.2 If the weight of the butcher block that was originally ture and humidity tolerances shall be in accordance with
375 lb or greater decreases with time to less than 375 lb, Section 7 of Practice D618, unless otherwise specified by
increase the block weight to a minimum of 375 lb by adding a contract or relevant ASTM material specification.
suitable amount of weight to the bottom of the table. The 10.1.1 Note that for some hygroscopic materials, such as
weight shall be tightly affixed and in direct contact with the nylons, the material specifications (for example, Specification
bottom of the table and not cause any vibrations during the D4066) call for testing “dry as-molded specimens.” Such
impact test. requirements take precedence over the above routine precon-
NOTE 4—The weight of the butcher block can decrease over time due, ditioning to 50 % relative humidity and require sealing the
for instance to drying. specimens in water vapor-impermeable containers as soon as
7.4 Micrometer, for measurement of specimen thickness. molded and not removing them until ready for testing.
Ensure that the accuracy is 1 % of the average thickness of the 10.2 Conduct tests at the same temperature and humidity
specimens used. See Test Methods D5947 for descriptions of used for conditioning with tolerances in accordance with
suitable micrometers. Section 7 of Practice D618, unless otherwise specified by
contract or relevant ASTM material specification.
8. Sampling
8.1 Sample using a statistically acceptable procedure. The 11. Procedure
samples shall be representative of the lot under study. When 11.1 Determine the number of specimens for each sample to
taken from a commercial production process, the process shall be tested, as specified in 9.3.
be in a state of statistical control.
11.2 Mark the specimens and condition as specified in 10.1.
9. Test Specimens 11.3 Prepare the test apparatus for the geometry (GA, GB,
9.1 The diameter or width of flat test specimens shall be at GC, GD, or GE) selected.
least 25 mm (1.00 in.) greater than the diameter of the hole in 11.4 Measure and record the thickness of each specimen in
the support plate. The specimens shall be free of obvious the area of impact. In the case of injection molded specimens,
imperfections, unless the imperfections constitute a variable it is sufficient to measure and record thickness for one
under study. specimen when it has been previously demonstrated that the
9.2 The thickness of any specimen in a sample shall not thickness does not vary by more than 5 %.
differ by more than 5 % from the average specimen thickness 11.5 Choose a specimen at random from the sample. Use a
of that sample. However, if variations greater than 5 % are random numbers table if desired.
unavoidable in a sample that is obtained from parts, the sample
11.6 Position the specimen. Ensure that the same surface or
shall be permitted to be tested, but the data shall not be used for
area, or both, is targeted on all test specimens. (see 6.2).
referee purposes. Machining specimens to reduce thickness
variation is not permissible. NOTE 6—Normally the specimen is not clamped because the test

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D5420 − 16
apparatus does not have provision for clamping. However, the apparatus where:
can be modified to permit clamping, which should improve the precision
of the measurement.
h = mean-failure height, mm (or in.),
dh = increment of height, mm (or in.),
11.7 Place the test specimen on the tester anvil, after raising N = total number of failures or nonfailures, whichever is
the weight and striker foot. Be sure the specimen is flat against smaller. For ease of notation, call whichever are used
the specimen-support plate before the striker foot is brought in events,
contact with the top surface of the specimen. (Fig. 3 shows the ho = lowest height at which an event occurred, mm (or in.),
position of the test specimen.) Raise the weight in the tube to
the desired impact value, as shown on the appropriate scale, i = 0, 1, 2 ... k (counting index, starts at ho or wo),
and release it so that the weight drops on the striker. ni = number of events that occurred at hi or wi,
hi = ho + idh, and
11.8 As a result of the wide range of failure types that are
observed with different materials, the definition of failure k
defined in the material specification shall take precedence over A5 ( ini,
i50
the definition stated in 3.2.1. Other definitions of failure shall
be used if agreed upon between the supplier and the user.
In calculating h, the negative sign is used when the events
11.9 Remove the specimen and examine it to determine are failures. The positive sign is used when the events are
whether or not it has failed. Permanent deformation alone is nonfailures. Refer to the example in Appendix X1.
not considered failure, but note the extent of such deformation 12.2 Mean-Failure Energy—Compute the mean failure en-
(depth, area). For some polymers, for example, glass- ergy as follows:
reinforced polyester, it is difficult to assess incipient cracking
with the naked eye. In such cases, it is permissible to expose MFE 5 hwf (2)
the stressed surface to a penetrating dye, such as gentian violet, where:
to help determine the onset of cracking. MFE = mean-failure energy, J (or in.·lbf),
11.10 If the first specimen fails, decrease the drop height h = mean-failure height as applicable, mm (or in.),
while keeping the mass constant (see 11.11). If the first w = constant mass, kg (or lb), and
specimen does not fail, increase the drop height one increment, f = factor for conversion to joules.
as above. Then test the second specimen. Use f = 9.80665 × 10−3 if h = mm and w = kg; Use 0.11299
if h = in. and w = lb; Use f = 1.0 for inch-pound
11.11 In this manner, select the impact height for each test units (in.·lbf, in., lb).
from the results observed with the specimen just previously
12.3 Estimated Standard Deviation of the Sample—If de-
tested. Test each specimen only once.
sired for record purposes, calculate the estimated standard
11.12 At the start of a test, a continuous run of seven or deviation of the sample for variable height as follows:
more identical results (failure or nonfailure) is indicative of an s h 5 1.62d h @ B/N 2 ~ A/N ! 2 # 10.047d h (3)
improper starting heights and affects final results. Re-estimate
approximate starting height and restart the test. where:
sh = estimated standard deviation, height, mm (or in.), and
11.13 Keep a running plot of the data, as shown in Appen-
dix X1. Use one symbol, such as X, to indicate a failure and a k
different symbol, such as O, to indicate a nonfailure at each B5 ( i ni.
2

height level. i50

12. Calculation The above calculation is valid for [B/N − (A/N)2] > 0.3. If the
value is <0.3, use Table 1 from Ref (3).
12.1 Mean-Failure Height—If a constant-mass procedure
12.4 Estimated Standard Deviation of the Sample Mean—
was used, calculate the mean-failure height from the test data
Calculate the estimated standard deviation of the sample
obtained, as follows:
mean-failure height as follows:
h 5 h o 1d h ~ A/N60.5! (1)
s h¯ 5 Gsh / =N (4)

where:
sh̄ = estimated standard deviation of the mean height, mm
TABLE 2 Precision, Method GA
(or in.), and
Values Expressed as G = factor that is a function of s/d (see Table X1.2).
Material Mean, J Percent of the Mean
Vr r A sample computation of sw is found in Appendix X1.
33 % Glass-Reinforced Nylon (PA) 0.75 4.66 13.2
Acetal (POM) 2.12 6.90 19.5 NOTE 7—For values of G at other levels of s/d, see Fig. 22 in Ref (4).
Impact Polystyrene 15.1 2.20 6.23
12.5 Estimated Standard Deviation of the Mean-Failure
Vr = within-laboratory coefficient of variation of the mean Energy—Calculate the estimated standard deviation of the
r = 2.83 Vr mean-failure energy as follows:

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TABLE 3 Precision, Method GB laboratories. Data from only three laboratories were used in
Values Expressed as calculating the values in these tables. For each material, all
Material Mean, J Percent of the Mean samples were prepared at one source, but the individual
Vr r specimens were prepared at the laboratories that tested them.
33 % Glass-Reinforced Nylon (PA) 0.99 3.18 8.99 Each test result was the mean of multiple individual determi-
Acetal (POM) 2.57 11.6 32.8
Impact Polystyrene 10.3 12.3 34.7 nations (Bruceton Staircase Procedure) (1). Each laboratory
Acrylonitrile-Butadiene-Styrene (ABS) 26.9 6.56 18.6 obtained two test results for a material. Warning—The fol-
lowing explanations of r and R (14.2 – 14.2.3) are only
Vr = within-laboratory coefficient of variation of the mean
r = 2.83 Vr intended to present a meaningful way of considering the
approximate precision of this test method. Do not apply the
TABLE 4 Precision, Method GC data in Table 2 and Table 4 rigorously for acceptance or
Values Expressed as
rejection of a material. Data in these tables are specific to the
Material Mean, J Percent of the Mean round robin study and are not always representative of other
Vr r lots, conditions, materials, or laboratories. The principles of
33 % Glass-Reinforced Nylon (PA) 1.82 1.92 5.44
Acetal (POM) 4.56 7.02 19.9
14.2 – 14.2.3 are valid if users of this test method apply the
Impact Polystyrene 14.8 18.6 52.7 principles outlined in Practice E691 to generate data specific to
their laboratory and materials, or between specific laboratories.
Vr = within-laboratory coefficient of variation of the mean
r = 2.83 Vr 14.1.1 Glass-Reinforced Nylon (33 % Glass)—101 by 101
by 3.2 mm (4 by 4 by 1⁄8 in.) cut from injection-molded
S MFE 5 s h¯ wf (5) plaques.
14.1.2 Acetal (Homopolymer)—101 by 101 by 3.2 mm (4 by
where: 4 by 1⁄8 in.) cut from injection-molded plaques.
SMFE = estimated standard deviation of the mean-failure 14.1.3 Impact Polysytrene—101 by 101 by 3.2 mm (4 by 4
energy. by 1⁄8 in.) cut from extruded sheet.
13. Report 14.1.4 ABS—101-mm diameter by 3.2-mm (4-in. diameter
by 1⁄8-in.) injection-molded disks.
13.1 Report the following information:
13.1.1 Complete identification of the sample tested, includ- 14.2 Concept of r and R—If Vr and VR have been calculated
ing type of material, source, manufacturer’s code, form, from a large enough body of data, and for test results that were
principal dimensions, and previous history. means from testing multiple individual specimens, then the
13.1.2 Method of preparation of specimens. following concepts apply:
13.1.3 Means of clamping, if any. 14.2.1 Repeatability, r—In comparing two test results for
13.1.4 Statement of geometry (GA, GB, GC, GD, GE). the same material, obtained by the same operator using the
13.1.5 Thickness of specimens tested (average and range). same equipment on the same day, judge the two results as not
13.1.6 Number of test specimens employed to determine the equivalent if they differ by more than the r value for that
mean-failure height. material.
13.1.7 Mean-failure energy. 14.2.2 Reproducibility, R—In comparing two test results for
13.1.8 Types of failure, for example: (a) crack or cracks on the same material, obtained by different operators using differ-
one surface only (the plaque could still hold water), (b) cracks ent equipment in different laboratories, reproducibility statis-
that penetrate the entire thickness (water would probably tics were not calculated because data from only four and three
penetrate through the plaque), (c) brittle shatter (the plaque is laboratories do not justify making these calculations.
in several pieces after impact), or (d) ductile failure (the plaque
is penetrated by a blunt tear). Report other observed deforma- 14.2.3 Any judgement in accordance with 14.2.1 would
tion due to impact, whether the specimens fail or not. have an approximate 95 % (0.95) probability of being correct.
13.1.9 Date of test and operator name. 14.3 Bias—There are no recognized standards by which to
13.1.10 Test temperature. estimate bias of this test method.
13.1.11 In no case shall results obtained with arbitrary
geometries differing from those contained in these test methods 14.4 Efforts to form a task group to address between-
be reported as values obtained by Test Method D5420. laboratory reproducibility of this test method have been unsuc-
cessful. Persons interested in participating in such a task group
14. Precision and Bias4 need to contact ASTM Headquarters.
14.1 Table 2, Table 3, and Table 4 are based on a round
robin conducted in 1977 involving four materials tested by four 15. Keywords
15.1 dart impact; falling weight impact; Gardner impact;
4
Supporting data have been filed at ASTM International Headquarters and may impact; impact resistance; mean-failure energy; mean-failure
be obtained by requesting Research Report RR:D20-1060. height; rigid plastic

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APPENDIXES

(Nonmandatory Information)

X1. SAMPLE CALCULATIONS

X1.1 See Table X1.1 and Table X1.2 for sample calculations and values of G for obtaining the estimated standard deviation.

TABLE X1.1 Sample Calculations


Total Outcome of Test
Dart (X = failure; O = nonfailure) nx no i ni ini i2ni
Height,
mm 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
500 X 1 0 2 1 2 4
475 O X X X X 4 1 1 4 4 4
450 X O O X O O X X O 4 5 0 4 0 0
425 O O O O O 0 5
Totals 9 11 9 6 8
(Nx) (No) (N) (A) (B)

NOTE 1—
where:
ho = 450; N = Nx = 9; d = 25
h = ho + dh (A/N − 0.5)
= 450 + 25 (6/9 − 0.5)
= 454.2 mm
sh = 1.62dh [B/N − (A/N)2] + 0.047dh
= 1.62 (25) [8/9 − (6 ⁄ 9)2] + 0.047 (25)
= 19.2 mm
s/d = 19.2/25 = 0.77; G = 1.035 (from Table X1.2)
sh̄ = Gsh/ =N51.035 ~ 0.77! / =950.27 mm

TABLE X1.2 Values of G for Obtaining the Estimated Standard Deviation of the Mean
s/d 0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09
0.40 ... ... ... ... ... 1.18 1.175 1.17 1.16 1.155
0.50 1.15 1.145 1.14 1.135 1.13 1.125 1.12 1.11 1.105 1.10
0.60 1.095 1.09 1.085 1.08 1.075 1.07 1.07 1.065 1.06 1.06
0.70 1.055 1.055 1.05 1.05 1.045 1.04 1.04 1.035 1.035 1.03
0.80 1.03 1.025 1.025 1.02 1.02 1.02 1.015 1.015 1.015 1.01
0.90 1.01 1.01 1.005 1.005 1.005 1.00 1.00 1.00 0.995 0.995
1.00 0.995 0.99 0.99 0.99 0.985 0.985 0.985 0.985 0.98 0.98
1.10 0.98 0.98 0.98 0.975 0.975 0.975 0.975 0.975 0.975 0.97
1.20 0.97 0.97 0.97 0.97 0.97 0.97 0.965 0.965 0.965 0.965
1.30 0.965 0.965 0.965 0.965 0.96 0.96 0.96 0.96 0.96 0.96
1.40 0.96 0.96 0.96 0.955 0.955 0.955 0.955 0.955 0.955 0.955
1.50 0.955 0.955 0.955 0.95 0.95 0.95 0.95 0.95 0.95 0.95
1.60 0.95 0.95 0.95 0.95 0.945 0.945 0.945 0.945 0.945 0.945
1.70 0.945 0.945 0.945 0.945 0.945 0.945 0.94 0.94 0.94 0.94
1.80 0.94 0.94 0.94 0.94 0.94 0.94 0.94 0.94 0.94 0.935
1.90 0.935 0.935 0.935 0.935 0.935 0.935 0.935 0.935 0.935 0.935
2.00 0.935 0.935 0.935 0.93 0.93 0.93 0.93 0.93 0.93 0.93

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D5420 − 16

X2. TESTING SUMMARY

TABLE X2.1 Testing Summary, MFE versus Table Weight, 8 lb WeightA


MFE Averages
Plastic 57 lb Base 215 lb Base 440 lb Base Floor
ABS 273 256 239 240
HDPE 190 185 184 ...
HIPS 179 164 162 133
PP (0.077 in.) 121 120 110 ...
PP (0.0121 in.) 196 185 184 184
PVC 112 102 101 101
A
Test results are based on averages for three sets of operators, using two different testers fixed to each base. Twenty specimens were used for each sample calculation,
with a minimum of 120 specimens used for each averaged test result.

X2.1 See Table X2.1 for testing summary of mean failure


energy versus table weight using an 8 lb weight.

REFERENCES

(1) Brownlee, K. A., Hodgest, J. L., Jr., and Rosenblatt, M., “The ods for Plastics Parts Used in Appliances, Society of the Plastics
Up-and-Down Method with Small Samples,” American Statistical Industry, New York, NY, January 1965.
Association Journal, Vol 48, 1953, pp. 262–277. (4) Natrella, M. G., “Experimental Statistics,” National Bureau of Stan-
(2) Hagan, R. S., Schmitz, J. V., and Davis, D. A.,“Impact Testing of High dards Handbook 91, October 1966, pp. 10–22 and 10–23.
Impact Thermoplastic Sheet,” Technical Papers, 17th Annual Techni- (5) Weaver, O. R., “Using Attributes to Measure a Continuous Variable in
cal Conference of SPE, SPPPB, Vol VII, January 1961. Impact Testing Plastic Bottles,” Materials Research and Standards,
(3) “Test Method B—Gardner Impact, Proposed Method of Test for Vol 6, No. 6, June 1966, pp. 285–291.
Impact Resistance of Fabricated Plastics Parts,” Proposed Test Meth-

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5420 - 10)
that may impact the use of this standard. (May 1, 2016)

(1) Added 7.1.1 on plumbness of vertical tube. (3) Added new Note 4.
(2) Modified 7.2 based on commercially available butcher (4) Revised Section 8 on Sampling
block tables. (5) Added 11.12 on starting heights for testing.

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5421 − 15

Standard Specification for


Contact Molded “Fiberglass” (Glass-Fiber-Reinforced
Thermosetting Resin) Flanges1
This standard is issued under the fixed designation D5421; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents


1.1 This specification covers circular contact-molded fiber- 2.1 ASTM Standards:2
glass reinforced-thermosetting-resin flanges for use in pipe C582 Specification for Contact-Molded Reinforced Thermo-
systems and tank nozzles. Included are requirements for setting Plastic (RTP) Laminates for Corrosion-Resistant
materials, workmanship, performance, and dimensions. Equipment
D883 Terminology Relating to Plastics
1.2 Flanges (see Fig. 1) may be produced as integral flanges, D1599 Test Method for Resistance to Short-Time Hydraulic
Type A, or flange-on-pipe, Type B. Pressure of Plastic Pipe, Tubing, and Fittings
1.3 This specification is based on flange performance and D1600 Terminology for Abbreviated Terms Relating to Plas-
does not cover design. tics
D2996 Specification for Filament-Wound “Fiberglass”
1.4 These flanges are designed for use with pipe and tanks (Glass-Fiber-Reinforced Thermosetting-Resin) Pipe
that are manufactured to Specifications D2996, D2997, D3262, D2997 Specification for Centrifugally Cast “Fiberglass”
D3299, D3517, D3754, and D4097. (Glass-Fiber-Reinforced Thermosetting-Resin) Pipe
1.5 Selection of gaskets is not covered in this specification, D3262 Specification for “Fiberglass” (Glass-Fiber-
refer to the manufacturer’s recommendation. Reinforced Thermosetting-Resin) Sewer Pipe
D3299 Specification for Filament-Wound Glass-Fiber-
1.6 The values stated in inch-pound units are to be regarded Reinforced Thermoset Resin Corrosion-Resistant Tanks
as the standard. The SI units given in parentheses are for D3517 Specification for “Fiberglass” (Glass-Fiber-
information only. Reinforced Thermosetting-Resin) Pressure Pipe
1.7 The following precautionary caveat pertains only to the D3754 Specification for “Fiberglass” (Glass-Fiber-
test methods portion, Section 9, of this specification: This Reinforced Thermosetting-Resin) Sewer and Industrial
standard does not purport to address all of the safety concerns, Pressure Pipe
if any, associated with its use. It is the responsibility of the user D4097 Specification for Contact-Molded Glass-Fiber-
of this standard to establish appropriate safety, health, and Reinforced Thermoset Resin Corrosion-Resistant Tanks
environmental practices and determine the applicability of 2.2 ASME Standards:3
regulatory limitations prior to use. B 16.1 Cast Iron Pipe Flanges and Flanged Fittings
B 16.5 Pipe Flanges and Flanged Fittings
NOTE 1—There is no known ISO equivalent to this standard. B 18.21.1 Type “A” Narrow Washers
1.8 This international standard was developed in accor-
dance with internationally recognized principles on standard- 3. Terminology
ization established in the Decision on Principles for the 3.1 Definitions:
Development of International Standards, Guides and Recom- 3.1.1 Definitions are in accordance with Terminology D883.
mendations issued by the World Trade Organization Technical Abbreviations are in accordance with Terminology D1600,
Barriers to Trade (TBT) Committee.

2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This specification is under the jurisdiction of ASTM Committee D20 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Plastics and is the direct responsibility of Subcommittee D20.23 on Reinforced Standards volume information, refer to the standard’s Document Summary page on
Plastic Piping Systems and Chemical Equipment. the ASTM website.
3
Current edition approved May 1, 2015. Published June 2015. Originally Available from American Society of Mechanical Engineers (ASME), ASME
approved in 1993. Last previous edition approve in 2010 as D5421 – 05(2010). International Headquarters, Two Park Ave., New York, NY 10016-5990, http://
DOI: 10.1520/D5421-15. www.asme.org.

*A Summary of Changes section appears at the end of this standard


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D5421 − 15
TABLE 1 Pressure Categories
Pressure RatingA
Designation
psi MPa

A 25 0.173
B 50 0.345
C 75 0.517
D 100 0.690
E 125 0.862
F 150 1.034
A
Flanges with higher pressure ratings are available by agreement between the
purchaser and the manufacturer.

FIG. 1 Flange Types

unless otherwise indicated. The abbreviation for reinforced- 4.1.5 Short-term rupture pressure and sealing-test pressure
thermosetting-resin pipe is RTRP. limits shall be categorized by single arabic number designa-
3.2 Definitions of Terms Specific to This Standard: tions as indicated by the cell classification system of Table 2.
3.2.1 contact molding (CM)—a method of fabrication 4.2 Designation Code—The flange-designation code shall
wherein the glass fiber reinforcement is applied to the mold in consist of the abbreviation for contact molded (CM) followed
the form of all chopped-strand mat, or chopped-strand mat and by the type as a capital letter, grade as an Arabic numeral, class
woven roving, in alternate plies by hand with the resin matrix as a Roman numeral, and the pressure-rating category as a
applied by brush or roller and the laminate consolidated by a capital letter and two Arabic numbers identifying the cell-
roller. classification designations of the short-term rupture pressure
3.2.2 fiberglass pipe—a tubular product containing glass- and sealing-test pressure, respectively. Thus, a complete
fiber reinforcements embedded in or surrounded by cured flange-designation code shall consist of three letters, one
thermosetting resin; the composite structure may contain Arabic numeral, one Roman numeral, one letter and two
aggregate, granular or platelet fillers, thixotropic agents, pig- numerals.
ments or dyes; thermoplastic or thermosetting liners or coat- 4.2.1 Example—Contact molded fiberglass is CM-AlID-46.
ings may be included. This designation described a stub flange, made using glass-
fiber-reinforced epoxy resin for full-axial pressure thrust. The
4. Classification flange has a 100-psi (0.69-MPa) pressure rating, a short-term
4.1 General—This specification covers reinforced- rupture pressure of 400-psi (2.76-MPa), and a sealing-test
thermosetting-resin flanges defined by type (method of pressure of 225-psi (1. 55-MPa).
manufacture), grade (generic type of resin), class (pressure end 4.3 Attachment of Flanges to Pipe, Pipe Fittings, or Tanks:
thrust capability), and pressure rating. Flanges complying with 4.3.1 Type “A” flanges are to be butt and strap welded to
this specification are also given numerical classifications relat- pipe described in Specifications D2996, D2997, D3262,
ing to rupture pressure and sealing test pressure. D3517, and D3754, or using overlay joint into a tank as
4.1.1 Types: described in Specifications D3299 and D4097.
4.1.1.1 Type A—Integral flange, contact molded with the 4.3.2 Type “B” flanges are built onto elbows, reducers, or
stub integral with the flange. other parts where the use of an integral flange (Type “A”) is not
4.1.1.2 Type B—Flange on pipe, contact molded onto an practical or required.
existing pipe or fitting.
4.1.2 Grades: 5. Materials and Manufacture
4.1.2.1 Grade 1—Epoxy resin. 5.1 Flanges manufactured in accordance with this specifi-
4.1.2.2 Grade 2—Polyester resin. cation shall be composed of reinforcement embedded in or
4.1.2.3 Grade 3—Phenolic resin. surrounded by cured thermosetting resin.
4.1.2.4 Grade 4—Vinylester resin.
4.1.2.5 Grade 5—Furan resin. 5.2 The resins, reinforcements, and other materials, when
4.1.3 Classes: combined into composite structure, shall produce a flange that
4.1.3.1 Class I—Hoop and axial-pressure. will meet the performance requirements of this specification.
4.1.3.2 Class II—Hoop pressure only.
NOTE 2—All combinations of type, liner, grade, and class may not be TABLE 2 Short-Term Rupture Pressure and Sealing-Test
commercially available. Additional type, liner, grade, and class may be PressureA
added as they become commercially available. The purchaser should Property/Cell Classification 1 2 3 4 5 6
solely determine or consult with the manufacturer for the proper class,
type, liner, and grade to be used under the installation and operating Short-Term Rupture 100 200 300 400 500 600
conditions that will exist for the project in which the flange is to be used. Pressure, psi (MPa) (0.69) (1.38) (2.07) (2.76) (3.45) (4.14)
Sealing-test pressure, psi 37.5 75 112.5 150 187.5 225
4.1.4 Pressure Rating—Pressure rating shall be categorized (MPa) (0.26) (0.52) (0.78) (1.03) (1.29) (1.55)
by single-letter designation. Pressure designations are shown in A
Refer to Test Method D1599 for explanation of failure.
Table 1.

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D5421 − 15
NOTE 3—The term “other materials” does not include recycled or TABLE 3 Flange Dimensions
reprocessed thermosetting plastics which might otherwise be added as Drilling
Nominal Outside
fillers. Pipe Size, Diameter, Bolt Circle Number of Diameter of Diameter of
5.3 Flanges manufactured in accordance with this specifi- in.A min, in.A DiameterA Holes HolesA BoltsA
cation shall have an inner corrosion barrier fabricated with the
1 4 1⁄ 4 3 1⁄ 8 4 58⁄ 12⁄
same resin, reinforcement, ply sequence, and nominal glass/ 1 1⁄ 2 5 3 7⁄ 8 4 58⁄ 12⁄
resin ratio as required in the applicable ASTM standard for the 2 6 43⁄ 4 4 3 ⁄4 58⁄
tank or pipe on which the flange will be used. 2 1⁄ 2 7 5 1⁄ 2 4 3 ⁄4 5 ⁄8

3 7 1⁄ 2 6 4 3 ⁄4 5 ⁄8

6. Performance Requirements 3 1⁄ 2 8 1⁄ 2 7 8 3 ⁄4 5 ⁄8

4 9 7 1⁄ 2 8 3 ⁄4 5 ⁄8

6.1 The following performance requirements are intended to 5 10 8 1⁄ 2 8 7 ⁄8 3 ⁄4

6 11 9 1⁄ 2 8 7 ⁄8 3 ⁄4
provide classification and performance criteria for the purpose
8 13 1⁄2 11 3⁄4 8 7 ⁄8 3 ⁄4
of qualification testing and rating of prototype constructions 10 16 14 1⁄4 12 1 7 ⁄8

and periodic reevaluation of the manufacturer’s stated ratings. 12 19 17 12 1 7 ⁄8

14 21 18 3⁄4 12 1 1⁄ 8 1
They are not intended as routine quality assurance require- 16 23 1⁄2 21 1⁄4 16 1 1⁄ 8 1
ments for production runs of rated flanges: 18 25 22 3⁄4 16 1 1⁄ 4 1 1⁄ 8
6.1.1 Sealing—Flanges shall withstand a pressure of at least 20 27 1⁄2 25 20 1 1⁄ 4 1 1⁄ 8
24 32 29 1⁄2 20 1 3⁄ 8 1 1⁄ 4
1.5 times the pressure rating without leakage when tested in 26 34 1⁄4 31 3⁄4 24 1 3⁄ 8 1 1⁄ 4
accordance with 9.4. 28 36 1⁄2 34 28 1 3⁄ 8 1 1⁄ 4
6.1.2 Short-Term Rupture Strength—Flanges shall withstand 30 38 3⁄4 36 28 1 3⁄ 8 1 1⁄ 4
32 41 3⁄4 38 1⁄2 28 1 5⁄ 8 1 1⁄ 2
a hydrostatic load of at least four times their pressure rating 34 43 3⁄4 40 1⁄2 32 1 5⁄ 8 1 1⁄ 2
when tested in accordance with 9.5 using flat-faced steel 36 46 42 3⁄4 32 1 5⁄ 8 1 1⁄ 2
closure and using the gasket or “O” ring designated by the 38 48 3⁄4 45 1⁄4 32 1 5⁄ 8 1 1⁄ 2
40 50 3⁄4 47 1⁄4 36 1 5⁄ 8 1 1⁄ 2
flange manufacturer. 42 53 49 1⁄2 36 1 5⁄ 8 1 1⁄ 2
6.1.3 Bolt Torque—Flanges shall withstand, without visible 44 55 1⁄4 51 3⁄4 40 1 5⁄ 8 1 1⁄ 2
sign of damage, a bolt torque of two times that recommended 46 57 1⁄4 53 3⁄4 40 1 5⁄ 8 1 1⁄ 2
48 59 1⁄2 56 44 1 5⁄ 8 1 1⁄ 2
by the manufacturer. The use of a non-fluid thread lubricant is 50 61 3⁄4 58 1⁄4 44 1 7⁄ 8 1 3⁄ 4
recommended on all bolts. 52 64 60 1⁄2 44 1 7⁄ 8 1 3⁄ 4
54 66 1⁄4 62 3⁄4 44 1 7⁄ 8 1 3⁄ 4
7. Dimensions and Tolerances 60 73 69 1⁄4 52 1 7⁄ 8 1 3⁄ 4
66 80 76 52 1 7⁄ 8 1 3⁄ 4
7.1 Flange and Bolt Dimensions—Flanges of 24 in. (610 72 86 1⁄2 82 1⁄2 60 1 7⁄ 8 1 3⁄ 4
mm) or smaller diameter shall conform to the values for bolt 84 99 3⁄4 95 1⁄2 64 2 1⁄ 8 2
96 113 1⁄4 108 1⁄2 68 2 3⁄ 8 2 1⁄ 4
circle and number and size of bolt holes, for Class-150 cast 102 120 114.50 72 2.625 2.50
iron flanges in ASME B 16.5. Flanges larger than 24 in. (610 108 126.75 120.75 72 2.625 2.50
mm) in diameter shall conform to the values for bolt circle, 114 133.50 126.75 76 2.875 2.75
120 140.25 132.75 76 2.875 2.75
number and size of bolt holes, for Class-125 cast-iron flanges 126 147 139.25 80 3.125 3.00
in ASME B 16.1 as shown in Table 3. The tolerance for these 132 153.75 145.75 80 3.125 3.00
flange dimensions shall be the same as those contained in 144 167.25 158.25 84 3.375 3.25
ASME B 16.1 and B 16.5. A flat washer is to be used under all A
1 in. = 25.4 mm.
bolt heads and nuts.
NOTE 4—Interference between the hub and bolt spot face may occur,
especially in high-pressure flanges. The use of ASME B 18.21.1 narrow 24-in. (610-mm) inside diameter and ASME B 16.1 for larger
washers is suggested because of their smaller outside diameter. The flanges. It is accepted practice to increase all flange outside
customer should be notified when these washers with smaller outside diameters to provide greater strength at the bolt holes.
diameter are to be used.
NOTE 5—For special-design large flanges, it may be desirable to 8. Workmanship, Finish, and Appearance
provide the required bolt area by using smaller bolts spaced closer
together than is normally used for steel flanges. The minimum bolt size 8.1 Workmanship and appearance shall conform to Table 5
shall be 5⁄8 in. (16 mm). Flange dimensions shall be by purchaser- on visual acceptance criteria of standard C582 for the process
manufacturer agreement. side, and shall be as free as commercially practical of defects,
7.1.1 Flange Face for Full-Faced Gaskets— The flange face including indentations, delaminations, bubbles, pinholes, for-
shall be perpendicular to the axis of the fitting within 1⁄2 °, and eign inclusions, and resin-starved areas in the structural layer
shall be flat to 1⁄32 in. (1 mm) for sizes up to and including and outer surface as agreed upon between the purchaser and the
18-in. (457-mm) diameter and 1⁄16 in. (2 mm) for larger manufacturer.
diameters. For other sealing systems the tolerances must be
established to meet the requirements of 6.1.1. 9. Test Methods
7.1.2 Washer-Bearing Surface—Washer-bearing surface 9.1 Conditioning—When conditioning is required, and in all
shall be flat and parallel to the flange face within 1°. cases of disagreement, condition the test specimens at 73.4 6
7.1.3 Flange Outside Diameter—Outside diameter of 3.6°F (23 6 2°C) for not less than 40 h prior to test, in
flanges is to be at least equal to that of ASME B 16.5 for up to accordance with Procedure A of Test Methods D618.

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D5421 − 15
9.2 Test Conditions—The tests may be conducted at ambient in Fig. 3. For flanges with 20 or more bolts, similar alternating
temperature and humidity conditions. When controlled- bolt-tightening sequences shall be used. Increase the bolt
environment testing is specified, conduct test at 73.4 6 3.6°F torque uniformly until flange failure occurs, or until all bolts
(23 6 2°C). When elevated-temperature testing is specified, have been torqued to 2 times the level recommended by the
conduct the tests at the design operating temperature, with a manufacturer for field-installation practice to establish the bolt
tolerance of 63.6°F (2°C). torque cell classification of the flange. Any sign of flange
9.3 Dimensions and Tolerances—Measure flange dimen- damage (crumbling, flaking, cracking, or other breaking) shall
sions with a micrometer, vernier calipers, or other suitable constitute failure.
measuring devices accurate to within 50 % of the required NOTE 6—The torque limits determined by 11.6 apply only to flanges
tolerance. Determine diameters by averaging a minimum of bolted up against a flat sealing surface. Significantly lower bolt-torque
four measurements, equally spaced circumferentially. values will normally be allowed when contact-molded flanges are bolted
up against other than flat sealing surfaces. When fiberglass flanges must be
9.4 Sealing—Bolt together flanged components in general used against other than flat sealing surfaces, the flange manufacturer
agreement with Fig. 2 using the gasket and bolt torque should be contacted for his torquing and installation recommendations.
recommended for standard field installation by the flange
manufacturer. Then pressure test the assembly and require it to 10. Proof of Design
hold the test pressure for a period of 168 h without leakage. 10.1 Test one each of 150-psi (1.03-MPa) flanges 8, 12, and
Retorquing to the manufacturer’s specified level after initial 24 in. (203, 305, and 610 mm) as described in 6.1.2 and 9.5, to
pressurization is permitted. establish that the design calculations meet the test requirements
9.5 Short-Term-Rupture Strength—Hydrostatically test and to establish rating data for the particular construction for
flanged components in accordance with Test Method D1599 all sizes of 150 psi or lower pressure ratings. Any change in
with free-end closure for Class I flanges and fixed-end closure calculation or construction will require retesting.
for Class II flanges except as herein noted. Increase the 10.2 For individual orders conduct only those tests specifi-
pressure in the specimen until failure of the flange occurs. cally agreed upon between the purchaser and the manufacturer
Pressure testing in an atmospheric environment is permissible. prior to manufacture of flanges.
Minimum-failure time shall be 60 s; no restriction shall be
placed on maximum time-to-failure. Leaking past the gasket 11. Product Marking
interface is permissible during this test. Bolt torque may be 11.1 Flanges for use or installation by other than the flange
increased as necessary during the test in order to minimize manufacturer shall be marked with the following information:
gasket leaking and to achieve the pressure necessary to cause 11.1.1 The designation “ASTM D5421” with which the
flange failure. The assembly used for the test in 9.4 may be flange complies,
used for this test. (Warning—DO NOT TEST WITH AIR 11.1.2 Identification of the flange in accordance with the
PRESSURE.) designation code in 4.2,
9.6 Maximum Bolt Torque—Using the gasket and hardware 11.1.3 Nominal flange size, and
recommended by the flange manufacturer, bolt the flange 11.1.4 Manufacturer’s name (or trademark) and product
against a flat-face steel flange. Tighten the nuts by hand until designation.
they are snug. Prior to fit-up, the nuts, bolts and washers should 11.2 Flanges for use and installation by the flange manufac-
be well lubricated, using a non-fluid thread lubricant. Establish turer shall be identified on the fabrication and assembly
uniform pressure over the flange face by tightening bolts in drawings with the following information:
10-lb·ft (14-N·m) increments according to the sequence shown 11.2.1 The designation “ASTM D5421,” and
11.2.2 Pressure rating.
NOTE 7—Through a quality-assurance and surveillance program the
manufacturer shall ensure that the flanges used are of the designated grade
and pressure rating.

12. Precision and Bias


12.1 No precision and bias statement can be made for the
test methods outline in this standard since controlled round-
robin test programs have not been run. The wide variations in
A—End, plate, end cap, or quick closure with coupling for pressure source/vent raw materials and construction between manufacturers make
line. round-robin testing difficult to apply.
B—Reinforced thermosetting resin pipe (RTRP).
C—Test flange set. 13. Keywords
D—End plate, end cap, or quick closure.
13.1 butt weld; contact molded; flange on pipe; furan;
FIG. 2 Test-Assembly Configuration integral flange; polyester; vinylester

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D5421 − 15

FIG. 3 Bolt Torquing Sequence

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D5421 – 05(2010)) that may impact the use of this standard. (May 1, 2015)

(1) Extended to larger diameters as now covered in many (3) Removed references to ASTM D2310 and D3982 as not
“Fiberglass” pipe standards. applicable.
(2) Corrected referenced bolting standards from ANSI to (4) Corrected recommended bolt torqueing sequences in Fig. 3.
ASME.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5422 − 17

Standard Test Method for


Measurement of Properties of Thermoplastic Materials by
Screw-Extrusion Capillary Rheometer1
This standard is issued under the fixed designation D5422; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

INTRODUCTION

This test method uses capillary rheometry to measure the rheological properties of thermoplastics
and thermoplastic compounds. This test method utilizes a screw-extrusion-type capillary rheometer.

1. Scope* mendations issued by the World Trade Organization Technical


1.1 This test method covers the use of a screw-extrusion- Barriers to Trade (TBT) Committee.
type capillary rheometer for the measurement of flow proper-
2. Referenced Documents
ties of thermoplastics and thermoplastic compounds. The
measured flow properties, which are obtained through labora- 2.1 ASTM Standards:2
tory investigation, may help to describe the material behavior D618 Practice for Conditioning Plastics for Testing
that occurs in factory processing. D883 Terminology Relating to Plastics
D1238 Test Method for Melt Flow Rates of Thermoplastics
1.2 Since a screw-type capillary rheometer imparts shear
by Extrusion Plastometer
energy to the material during testing, the measurements will
D3835 Test Method for Determination of Properties of
usually differ from those obtained with a piston-type capillary
Polymeric Materials by Means of a Capillary Rheometer
rheometer (see Test Method D3835).
E691 Practice for Conducting an Interlaboratory Study to
1.3 Capillary rheometer measurements for thermoplastics Determine the Precision of a Test Method
and thermoplastic compounds are described in Test Method
D3835. 3. Terminology
1.4 The values stated in SI units are to be regarded as 3.1 Definitions: (See Terminology D883):
standard. 3.1.1 apparent shear rate (γ̇a)—shear strain rate (or velocity
1.5 This standard does not purport to address all of the gradient) of the thermoplastic or thermoplastic compound
safety concerns, if any, associated with its use. It is the extrudate as it passes through the capillary die.
responsibility of the user of this standard to establish appro- 3.1.1.1 Discussion—This velocity gradient is not uniform
priate safety, health, and environmental practices and deter- through the cross-section of the capillary die. The shear rate is
mine the applicability of regulatory limitations prior to use. calculated for the region of highest shear, which is at the wall
of the capillary. By selecting a die diameter and controlling the
NOTE 1—There is no known ISO equivalent to this standard. The scope volume flow per unit time through the die, a specific level of
of this standard is mentioned in ISO 11443:2014, Plastics—Determination
of the fluidity of plastics using capillary and slit-die rheometers,” Annex apparent shear rate is achieved. Alternately, the shear stress
C, “Uncertainties in the determination of shear viscosity by capillary (entrance pressure) is controlled, and the apparent shear rate
extrusion.” measured.
1.6 This international standard was developed in accor- 3.1.1.2 Discussion—Mathematically, the apparent shear rate
dance with internationally recognized principles on standard- at the wall of the capillary for a Newtonian fluid at the capillary
ization established in the Decision on Principles for the wall is given by the following:
Development of International Standards, Guides and Recom- 32·Q
γ̇ a 5 (1)
π·D 3
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.30 on Thermal Properties
2
(Section D20.30.08). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2017. Published January 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1993. Last previous edition approved in 2009 as D5422 – 09. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5422-17. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D5422 − 17
where: obtained by applying the Bagley Correction Factor (E) to the
γ̇a = apparent shear rate, s−1, apparent shear stress (see 3.1.7.1 and 3.1.7.2). The Bagley
Q = quantity of fluid extruded per time, mm3 /s, correction compensates for energy losses at the entrance and
π = 3.142, and exit of the die.
D = diameter of the measuring capillary, mm. 3.1.6.1 Discussion—This correction is often applied as
3.1.2 apparent shear stress (τa)—the measured resistance to though it were an additional length of capillary. The correction
the flow through a capillary die. It may be determined by is often termed “end effect.” Capillary entrance angle and
measuring the die entrance pressure for a specific die, then geometry have great influence on the magnitude of this
applying appropriate geometric factors. correction.
3.1.2.1 Discussion—Mathematically, apparent shear stress 3.1.6.2 Discussion—The Bagley correction will also remove
is given by the following: the influence of any static pressure in the system that does not
P vary with die length.
τa 5 (2)
4· ~ L/D ! 3.1.6.3 Discussion—Since the magnitude of correction is a
function of shear rate, data for this correction are obtained by
where:
using two or more dies of different length, but of the same
τa = apparent shear stress, Pa, diameter (and thus the same apparent shear rate, as calculated
P = pressure at the entrance of the measuring capillary, Pa, in 3.1.4.2). If the data from these additional dies are compared,
L = length of the measuring capillary, mm, and either graphically or mathematically, a linear relationship of
D = diameter of the measuring capillary, mm.
extrusion pressure with die geometry is usually obtained in the
3.1.3 apparent viscosity (ηa)—ratio of apparent shear stress following form:
to apparent shear rate, Pa·s.
3.1.3.1 Discussion—For an extrusion capillary rheometer,
the ratio is usually calculated at a given shear rate. At constant
P 5 c· F L
D
1E G (4)

temperature, the apparent viscosity of most polymers is not where:


constant, but varies with shear rate. The viscosity is generally E = the Bagley Correction Factor. (This term is often called
annotated with the shear rate at which the measurement was “end effect.” It is expressed as the equivalent length of
made. capillary necessary to extrapolate the pressure-line value
3.1.4 capillary rheometer—an instrument in which thermo- on the P versus L/D plot to zero, mm.)
plastics or thermoplastic compounds can be forced from a c = slope of the line.
reservoir through a capillary die. The temperature, pressure The Bagley Correction Factor (E) and the slope (c) are
entering the die, and flow rate through the die can be controlled functions of the thermoplastic compound and the shear rate.
and accurately measured. Corrected shear stress is therefore as follows:
3.1.5 corrected shear rate (γ̇w)—the actual shear rate at the P
wall of the capillary die determined by applying the Rabinow- τ 5 (5)
w
4· @ ~ L/D ! 1E #
itsch correction for non-Newtonian materials, s−1. 3.1.6.4 Discussion—Each value of corrected shear stress
3.1.5.1 Discussion—The Rabinowitsch correction math- must be annotated with the shear rate with which it is
ematically adjusts the shear-rate values to compensate for measured.
non-Newtonian behavior of the polymer. To obtain corrected
shear rate, at least two measurements of apparent shear stress 3.1.7 corrected viscosity (η)—the ratio of corrected shear
and apparent shear rate are made. This is generally accom- stress to corrected shear rate, Pa·s.
plished by increasing the rate of extrusion (Q) while using the 3.1.7.1 Discussion—Since both the material properties and
same measuring capillary. the correction equations are functions of shear rate, it is very
3.1.5.2 Discussion—As a first step, the Bagley correction important to state the particular value of shear rate at which
(as stated in 3.1.6) is made to the shear-stress values. Then, each measurement is made.
either by algebraic means (if only two measurements are 3.1.7.2 Discussion—Other corrections to measured values
made), or by a regression method (for a greater number of are often made in rheological research studies to compensate
points), the equation in 3.1.11 is solved for n, using the for the effects of pressure, viscous heating, compressibility,
corrected shear stress (τw). time effects, etc. The terms “true shear stress,” “true shear
3.1.5.3 Discussion—The corrected shear rate (γ̇ w) is deter- rate,” and “true viscosity” are often used for the results of such
mined by the following: exhaustive calculations. This test method addresses only the
γ̇ w 5 F 3 n 11
4n G ·γ̇ a (3)
two most important corrections, Bagley and Rabinowitsch.
3.1.8 die entrance pressure (P)—the pressure in the reser-
For most thermoplastics and thermoplastic compounds, voir at the die entrance.
the magnitude of shear sensitivity (n) will vary, depending 3.1.9 newtonian fluid—a material for which the measure-
on material composition. ment of viscosity is not changed by changing the shear rate.
3.1.6 corrected shear stress (τW)—the actual shear stress at Simple liquids, such as water, are considered Newtonian
the wall of the capillary die, Pa. The corrected shear stress is whereas most polymeric materials are not.

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D5422 − 17
3.1.10 power-law fluid—a material for which the viscosity shear stress, corrected shear rate, corrected viscosity, shear
varies with the shear rate in accordance with the following sensitivity, and entrance/exit effects.
known relationship:
τ a 5 K· ~ γ̇ a ! n (6) 5. Significance and Use
5.1 This test method is useful for the characterization of
where:
thermoplastics and thermoplastic compounds, in terms of
τa = apparent shear stress, Pa, viscosity, or resistance to flow.
γ̇a = apparent shear rate, s−1 ,
K = a material constant, often called “consistency index,” 5.2 The data produced by this test method has been found
and useful in both quality-control testing and compound develop-
n = shear sensitivity, dimensionless. ment. However, direct correlation with factory conditions is
Most non-Newtonian fluids follow this relationship for at not implied.
least short ranges of the shear rate variable. The power-law 5.3 Flow-performance data permits quality control of in-
equation is generally used in its logarithmic form as follows: coming thermoplastics and thermoplastic compounds because
log~ τ the flow parameters are sensitive to molecular weight and
a ! 5 log~ K ! 1n ~ log~ γ̇ a !! (7)
molecular-weight distribution. Therefore, this test method may
3.1.11 shear sensitivity (n)—a dimensionless material distinguish differences between lots.
parameter, also called the “power-law index,” that represents
the magnitude of the shear sensitivity of a polymer. It is equal 5.4 The shear viscosity or flow viscosity of thermoplastics
to 1.00 for Newtonian fluids, and generally less than 0.8 for and thermoplastic compounds will not only be sensitive to the
non-Newtonian fluids. raw-polymer molecular properties, but will also be affected by
3.1.11.1 Discussion—Mathematically, the shear sensitivity the type and amount of filler, additive, plasticizer, or stabilizer,
is given by the following: by the type of copolymer blend, and by the addition of other
compounding materials. This test method can serve as a
dlog~ τ w ! quality-control tool for either incoming materials or for in-
n5 (8)
dlog~ γ̇ a ! house quality-assurance checks on production mixing. This test
where: method is useful to the research and development of new
products in that the rheological behavior of a yet uncharacter-
d log(τw) = the change in log corrected shear stress over ized thermoplastic or thermoplastic compound can be mea-
varying extrusion rates, and sured and considered for comparative analysis.
d log(γ̇a) = the change in log apparent shear rate over
varying extrusion rates. 6. Interferences and Precautions
6.1 Since the flow properties of non-Newtonian materials
4. Summary of Test Method are not linear, capillary rheometers should be operated at
4.1 The thermoplastic material is fed into a laboratory conditions of flow (temperature, pressure, and rate) similar to
extruder, the barrel of which is equipped with a temperature those of selected commercial processes. These processes in-
control. The output end of the extruder is equipped with a clude mixing, calendering, molding, and extrusion of thermo-
capillary die containing an insert of specified dimensions. plastics and thermoplastic compounds.
Temperatures of the extruder barrel and capillary die are 6.2 Screw-extrusion-type rheometers impart significant
normally kept constant. (It may be necessary to alter the die-set amounts of energy to the thermoplastic or thermoplastic
temperature only to compensate for shear heating of the compound before the measurement is made. Interpretation of
material at different extrusion rates.) the data for factory operations such as production extrusion,
calendering, or injection molding is therefore more straightfor-
4.2 A suitable pressure transducer and temperature-
ward than for compression-molding operations, where factory-
measuring device, such as a thermocouple, are positioned in
work input is quite small.
the die just before the entrance to the insert.
6.3 Increasing the rate of extrusion will induce shear
4.3 The rate of material extrusion, or mass throughput (Q) is
heating, and therefore may alter the temperature of the material
determined by collecting extrudate over a timed interval and
flowing through the capillary die. It is essential to maintain a
then weighing it. The extrusion rate is controlled by adjusting
constant melt temperature in the die in order to perform
the drive speed.
accurate viscosity measurements. It may be necessary to
4.4 In order to calculate the flow properties of the material, compensate for shear heating by manually adjusting the
extrusion is performed at a minimum of two different drive die-heater set temperature.
speeds through an insert of specified dimensions (Die A). Then, 6.4 Extruder residence time and shearing actions at a
extrusion is performed again, at the same drive speeds, through particular melt temperature will often affect a material’s
at least one additional die insert of different specified dimen- viscosity. It is recommended that consideration be given to the
sions (Die B or Die C). temperature and shear-stability characteristics of each thermo-
4.5 This procedure allows for the determination of apparent plastic or thermoplastic compound before using this test
shear rate, apparent shear stress, apparent viscosity, corrected method.

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FIG. 1 Schematic of Screw-Extrusion-Type Rheometer Cross-Section

7. Apparatus assembly. The monitoring devices should have an accuracy of


7.1 A schematic diagram of a screw-extrusion capillary 61.0°C, and a precision of 60.2°C.
rheometer is shown in Fig. 1. Only those parts essential to the 7.3 The dies are firmly secured to the end of the barrel. A
measurement are depicted. Suitable supports, drive minimum of two die inserts are needed. A schematic of the die
components, and fixtures, such as devices for securing the die is shown in Fig. 2. The dimensions are given in Tables 1 and
to the barrel are essential, but are not shown. 2.
7.2 The screw-extrusion system controls both the rate of
NOTE 3—Refer to recommendations of the manufacturer when selecting
extrusion and the temperature of the stock at the die entrance. the proper diameter for the die nozzle. The 2.0 mm insert series is
7.2.1 A single-screw-type laboratory extruder having a bar- recommended for rigid PVC, glass-reinforced resins, and materials with
rel diameter of not greater than 31.7 mm nor less than 19 mm heat/shear sensitive properties.
is recommended. The length to diameter (L/D) ratio of the
7.4 For the purpose of calculation, the length of each insert
barrel should not be less than 20:1 nor more than 30:1.
shall be measured to 60.14 mm, and the diameter to 60.014
7.2.2 Compression of the stock is accomplished by transport
mm. The actual measured dimensions shall be used for these
action of the rotating screw. In some extruders, the volume
between the screw and the wall, occupied by the polymeric calculations. Calibration of the apparatus shall be carried out in
compounds, is less at the end of the barrel than at the feed accordance with the manufacturer’s recommendations.
section. The ratio of the volume in the feed section to the 7.4.1 Dies must be made of wear-resistant materials such as
volume at the end of the screw is referred to as the “compres- hardened steel, hardened stainless steel, or carbide. Calibration
sion ratio.” The compression ratio of the screw should not be of the pressure transducer generally requires removal of the
less than 2.0:1.0 nor greater than 5.0:1.0. The suggested transducer from its mounting, followed by the calibration in an
compression ratio is 3.0:1.0. appropriate testing apparatus, and then reattachment to the
extruder. Thermocouples are calibrated according to the rec-
NOTE 2—Refer to material specifications or to recommendations of the
manufacturer when selecting the proper compression ratio for the screw.
ommendations of the manufacturer.
7.2.3 Both the barrel and the screw should be constructed of 8. Sampling and Conditioning of Samples
hardened stainless steel with suitable surface treatments to
render them resistant to wear and chemical attack. 8.1 Many thermoplastics and thermoplastic compounds do
7.2.4 The extruder shall be equipped with instrumentation not require conditioning prior to testing. Materials that contain
capable of monitoring the wall temperature of each portion of volatile components, are chemically reactive, or have other
the barrel. The stock temperatures should also be measured at unique characteristics, are most likely to require special con-
the extruder head and at any inside surface of the capillary-die ditioning procedures. In many cases, moisture accelerates

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D5422 − 17
TABLE 3 Typical Screw-Flight Dimensions
Flight Channel Width, Flight Channel Depth,
Compression Ratio
mm mm
19.05 mm screw diameter 15.88 ± 0.14 1.91 ± 0.03
2:1 15.88 ± 0.14 1.27 ± 0.03
3:1 15.88 ± 0.14 0.95 ± 0.03
4:1 15.88 ± 0.14 0.76 ± 0.03
5:1
31.75 mm screw diameter 27.00 ± 0.14 3.18 ± 0.03
2:1 27.00 ± 0.14 2.12 ± 0.03
3:1 27.00 ± 0.14 1.59 ± 0.03
4:1 27.00 ± 0.14 1.27 ± 0.03
5:1

9.3 Equip the extruder with Die A if using the 1.0 mm insert
series, or Die D if using the 2.0 mm insert series (See 7.3).
9.4 Preheat the rheometer die and die holder to the test
temperature. This temperature should model that of the pro-
cessing operation. For material-processing temperatures, refer
to the supplier recommendations. The die and die holder shall
be preheated until thermal equilibrium of each heating zone has
been achieved, and then maintained at the test temperature for
at least 5 min.
9.5 Establish equilibrium extrusion conditions.
FIG. 2 Rheometer Die
9.5.1 To ensure that equilibrium-flow conditions prevail
before any viscosity measurements are taken, screw-extruder-
TABLE 1 1.0 mm Die Nozzle Dimensions
type capillary rheometers require an additional running period,
Item Die A Die B Die C generally referred to as “ line-out.” Sufficient sample must be
Capillary length, (L), mm 15.0 ± 0.13 20.0 ± 0.13 30.0 ± 0.13 fed to the turning screw to fill and maintain the volume in the
Capillary diameter, (D ), mm 1.0 ± 0.013 1.0± 0.013 1.0± 0.013
Total included entrance angle, 40° ± 0°30' 40°± 0°30' 40°± 0°30' screw, head, and die under equilibrium conditions.
(α),° 9.5.2 Check the rate of extrusion by cutting the extruded
Capillary length to diameter 15.0 ± 0.13 20.0 ± 0.13 30.0 ± 0.13 strand with a sharp knife, collecting the extrudate for precisely
ratio, (L/D)
2 min, and then cutting the strand. Weigh the collected
extrudate.
TABLE 2 2.0 mm Die Nozzle Dimensions NOTE 4—The apparent shear rate will increase or decrease by adjusting
Item Die D Die E Die F the extruder variable-speed drive.
Capillary length, (L), mm 20.0 ± 0.13 30.0 ± 0.13 40.0 ± 0.13
Capillary diameter, (D ), mm 2.0 ± 0.013 2.0 ± 0.013 2.0 ± 0.013
9.5.3 Monitor the barrel temperatures and the die-stock
Total included entrance angle, (α),° 40° ± 0°30' 40° ± 0°30' 40° ± 0°30' temperature for at least 5 min of continuous running. During
Capillary length to diameter ratio, 10.0 ± 0.13 15.0 ± 0.13 20.0 ± 0.13 this period, the pressures in the head and particularly in the
(L/D)
capillary-die assembly shall be in equilibrium before taking
readings for viscosity measurements.
9.6 Collect the extrudate for 2 min, again using a sharp knife
degradation or may otherwise affect reproducibility of flow- to cut the strand before and after the time period. Note the
rate measurements. If conditioning is necessary, see the appli- pressure and stock temperature in the die during extrudate
cable material specification and Test Method D618. collection. Weigh the extrudate to the nearest milligram, then
9. Procedure convert the mass to volume, using the melt density of the
material.
9.1 Determine the melt density of the thermoplastic or
thermoplastic compound being tested (see Test Method 9.7 Repeat the extrusion procedure of 9.5 and 9.6 at least
D1238). This is necessary since the throughput is measured as twice at different drive speeds to obtain an apparent shear-rate
a mass, but the calculations are based on volumetric flow. range. It may be necessary to adjust the die-set temperature in
order to compensate for the shear heating of the material (see
9.2 Prepare the sample for introduction into the extruder. 6.3).
9.2.1 To obtain equilibrium plastication and flow of thermo-
plastics or thermoplastic compounds, it is necessary to feed the 9.8 Change to Die B after using Die A when using the 1.0
material at a constant rate into the feed section of the screw. mm insert series. Change to Die E after using Die D when
Material should be supplied in either pellet or powder form. using the 2.0 mm insert series.
9.2.2 Typical screw-flight dimensions for the feed section of 9.9 Repeat the procedure in 9.5 – 9.7 using the same drive
the laboratory scaled extruders are shown in Table 3. speeds.

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TABLE 4 Repeatability Data
Corrected Shear Stress (KPa) at Fixed Corrected Shear Rate (s-1)
Mean Level in Ascending Order Within Laboratory
Material Shear Rate Avg. Stress (KPa) Sr r (r)
LDPE 1000 120.3 2617 7328 6.1 %
2500 157.3 1574 4409 2.8 %
5000 192.6 216 606 0.3 %
7500 216.9 884 2475 1.1 %
10 000 236.0 1831 5128 2.2 %
12 500 251.9 2676 7494 3.0 %
Pooled Values 1633 4573 2.5 %

Corrected Viscosity at Fixed Corrected Shear Rate (s-1) and Shear Stress (KPa)
Mean Level in Ascending Order Within Laboratory
Material Shear Rate Viscosity Sr r (r)
LDPE 1000 120.3 2.6 7.3 6.1 %
2500 63.0 0.6 1.8 2.8 %
5000 38.6 0.1 0.2 0.5 %
7500 28.9 0.1 0.4 1.4 %
10 000 23.6 0.1 0.4 1.7 %
12 500 20.2 0.2 0.6 2.9 %
Pooled Values 0.6 1.8 2.5 %

NOTE 5—If a third die insert is necessary, follow the procedures in 9.8
and 9.9, substituting Die C for Die B, or substituting Die F for Die E. Use
of three or more die nozzles of different lengths may better ensure the
3n11
γ̇ w 5
4nF ·γ̇ a G (15)
NOTE 7—Corrected shear stress (τW) is calculated first, and then used in
linearity of data required to calculate the Bagley Correction Factor. the determination of n.

10. Calculation 10.8 Corrected Viscosity (η):


NOTE 6—See Section 3 for terminology used in the following calcula- 10.8.1 The corrected viscosity is calculated as follows:
tions. For all calculations, it is advisable to use the actual measured values τw
of the die dimensions instead of the nominal values discussed in 7.3. η5 (16)
γ̇ w
10.1 Apparent Shear Rate (γ̇aA1 ):
10.1.1 Calculate the apparent shear rate of 9.5.2, 9.7, and 11. Report
9.9 as follows: 11.1 Report the following information:
γ̇ aA1 5 @ ~ 32·Q 3
A1 ! / ~ π·D A ! # (9) 11.1.1 Type of capillary rheometer used,
11.1.2 Dimensions of capillary-die inserts, mm,
10.2 Apparent Shear Stress (τaA1):
11.1.3 Entrance angle of capillary-die inserts, rad,
10.2.1 The apparent shear stress is calculated as follows:
11.1.4 Position of pressure transducer (distance from capil-
τ aA1 5 4· ~ P A1 /L A /D A ! (10) lary entrance), mm,
10.3 Apparent Viscosity (ηa): 11.1.5 Identity of sample,
10.3.1 The apparent viscosity is calculated as follows: 11.1.6 Pretreatment of sample, if any,
11.1.7 Temperature of test, °C or °K,
τ aA1
ηa 5 (11) 11.1.8 Shear sensitivity (n), dimensionless,
γ̇ aA1
11.1.9 End effect (E), mm,
10.4 Entrance/Exit Effects (Bagley): 11.1.10 Corrected shear stress values, Pa,
10.4.1 The Bagley Correction Factor (E) is calculated as 11.1.11 Corrected shear rate values, s−1, and
follows: 11.1.12 Corrected viscosity values, Pa·s.
@ P B1 · ~ L A /D A ! # 2 @ P A1 · ~ L B /D B ! # 12. Precision and Bias
E5 (12)
@ P A1 2P B1 #
12.1 Table 4 is based on a single laboratory repeatability
10.5 Corrected Shear Stress (τw): study conducted in 2002 involving one LDPE homopolymer
10.5.1 The corrected shear stress is calculated as follows: resin. The laboratory used a computerized torque rheometer
P A1 and a three zone electrically heated 19.0 mm single screw
τw 5 (13)
4· @ ~ L A /D A ! 1E # extruder, 3:1 metering extruder screw, electrically heated one
10.6 Shear Sensitivity (n): zone gear pump (1.16 cc/rev), and an electrically heated two
10.6.1 Shear sensitivity is calculated as follows: zone capillary rheology die to process the sample. The sample
was tested once on two separate days yielding two data points
dlog~ τ w ! per value. (Warning—The explanation of r (12.2.1 and 12.2.2)
n5 (14)
dlog~ γ̇ a ! is only intended to present a meaningful way of considering the
10.7 Corrected Shear Rate (γ̇w): approximate precision of this test method. The data in Table 4
10.7.1 The corrected shear rate is calculated as follows: should not be applied to acceptance or rejection of materials, as

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D5422 − 17
these data apply only to the materials tested in the round robin 12.2.2 Reproducibility (R)—The number of laboratories,
and are unlikely to be rigorously representative of other lots, one, participating in the round robin does not meet the
formulations, conditions, materials, or laboratories. Users of minimum requirement for inclusion of information on between
this method should apply the principles outlined in Practice laboratory variability. Because this method does not contain a
E691 to generate data specific to their materials and laboratory recognized round robin precision and bias statement, it shall
(or between specific laboratories). The principles of 12.2.1 and not be used as a referee test method in case of dispute. Anyone
12.2.2 would then be valid for such data.) wishing to participate in the development of precision and bias
NOTE 8—SYMBOLS ARE DEFINED AS FOLLOWS: data should contact the Chairman, Subcommittee D20.30
(Section D20.30.08) ASTM 100 Barr Harbor Drive, PO Box
Sr = within laboratory standard deviation C700, West Conshohocken, PA 19428-2959.
r = within laboratory repeatability, measurement units
(r) = within laboratory repeatability, % 12.3 Any judgment in accordance with 12.2.1 or 12.2.2
12.2 Concept of r and R in Table 4—If Sr has been would have an approximate 95 % (0.95) probability of being
calculated from a large enough body of data, and for test results correct.
that were averages from testing one point for each test result, 12.4 There are no recognized standards by which to esti-
then:
mate bias of this method.
12.2.1 Repeatability (r)—Two results obtained within one
laboratory shall be judged not equivalent if they differ by more
13. Keywords
than the r-value, where r = 2.8Sr. r is the interval representing
the critical difference between two test results for the same 13.1 capillary rheometer; flow properties; material proper-
material, obtained by the same operator using the same ties; molecular properties; rheological properties; rheology;
equipment on the same day in the same laboratory. screw extrusion

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5422 - 09)
that may impact the use of this standard. (December 1, 2017)

(1) Revised Note 1.

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of infringement of such rights, are entirely their own responsibility.

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Designation: D5436 − 15

Standard Specification for


Cast Poly(Methyl Methacrylate) Plastic Rods, Tubes, and
Shapes1
This standard is issued under the fixed designation D5436; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* D1003 Test Method for Haze and Luminous Transmittance


1.1 This specification covers poly(methyl methacrylate) of Transparent Plastics
rods, tubes, and other shapes produced by casting or machining D1600 Terminology for Abbreviated Terms Relating to Plas-
cast blanks. This specification does not apply to heat-formed tics
and molded or extruded parts and shapes, or sections that are D3892 Practice for Packaging/Packing of Plastics
made by assembling or joining two or more pieces. E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
NOTE 1—The properties included in this specification are those required
to identify the types and grades of materials covered. There may be other 3. Terminology
requirements necessary to identify particular characteristics.
3.1 The terminology used in this specification is in accor-
1.2 The values stated in SI units are to be regarded as dance with Terminology D883 and Terminology D1600.
standard.
1.3 This standard does not purport to address all of the 4. Classification
safety concerns, if any, associated with its use. It is the 4.1 Types—This specification covers two types of cast
responsibility of the user of this standard to establish appro- methacrylate plastics:
priate safety and health practices and determine the applica- 4.1.1 Type UVA—Material having ultraviolet-lightabsorbing
bility of regulatory limitations prior to use. properties as shown in Table 1.
NOTE 2—There is no known ISO equivalent to this standard. 4.1.2 Type UVT—Material not subject to the light-absorbing
properties shown in Table 1.
2. Referenced Documents 4.2 Finish—Castings may be specified with the following
2.1 ASTM Standards:2 finishes:
D542 Test Method for Index of Refraction of Transparent 4.2.1 Finish 1—Rods, tubes, and shapes having a smooth
Organic Plastics surface finish obtained either in the casting process or by
D570 Test Method for Water Absorption of Plastics highly polishing the surface.
D618 Practice for Conditioning Plastics for Testing 4.2.2 Finish 2—Rods, tubes, and shapes having a rough,
D638 Test Method for Tensile Properties of Plastics unfinished surface which may be frosted, abraded, sanded,
D648 Test Method for Deflection Temperature of Plastics machined, or as-cast.
Under Flexural Load in the Edgewise Position NOTE 3—The sawed ends of Finish 1 and Finish 2 rods, tubes, and
D792 Test Methods for Density and Specific Gravity (Rela- shapes are not polished.
tive Density) of Plastics by Displacement
D883 Terminology Relating to Plastics 5. General Requirements
5.1 Finish 1 and Finish 2 cast tubes are subject to the
following permissible variations from the specified dimen-
1
This specification is under the jurisdiction of ASTM Committee D20 on sions:
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic 5.1.1 Cast tubes shall be specified with either Type A or
Materials.
Current edition approved June 1, 2015. Published July 2015. Originally approved Type B wall thickness tolerances as listed in Table 2. Type A
in 1993. Last previous edition approved in 2013 as D5436 – 13. DOI: 10.1520/ tolerances are specified for applications where wall thickness is
D5436-15.
2
critical to performance, otherwise Type B is generally speci-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
fied.
Standards volume information, refer to the standard’s Document Summary page on 5.1.2 Cast tubes are subject to the outside-diameter toler-
the ASTM website. ances listed in Table 3.

*A Summary of Changes section appears at the end of this standard


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D5436 − 15
TABLE 1 Detail Requirements for Cast Methacrylate Rods, Tubes, TABLE 4 Sizes and Permissible Length Tolerances for Cut-to-
and Shapes Length Cast Rod and Tube
Type UVA Type UVT Nominal Outside Permissible Length
Index of refraction, n D, 23 °C Diameter, Tolerances,
min: 1.48 1.48 mm (in.) ±, mm (in.)
max: 1.50 1.50 up to 76 (3.0) 2 (0.079)
Specific gravity, 23/23 °C (73.4/73.4°F) up to 280 (11.0) 3 (0.118)
min: 1.18 1.18 greater than 280 (11.0) 6 (0.236)
max: 1.20 1.20
Spectral transmittance, %, max
270 nm: 5 ...
280 nm: 5 ... TABLE 5 Size and Permissible Tolerances for Diameter of Cast
290 nm: 5 ... Rods
310 nm: 5 ... Diameter Tolerances,
340 nm: 5 ... Size, Diameter, mm (in.)
±, mm (in.)
Luminous transmittance, %, min
up to 4.7 mm (0.187 in.) thickness: 91 91 up to 9.5 (0.375) 0.1 (0.005)
25.4 mm (1.00 in.) thickness: 89 89 up to 25.4 (1.00) 0.2 (0.010)
greater than 25.4 mm (1.00 in.) thickness: 87 87 up to 50.8 (2.00) 0.4 (0.015)
Haze, %, max 3.0 3.0 up to 76.2 (3.00) 0.8 (0.030)
Deflection temperature under load at 1820 up to 152.4 (6.00) 1.1 (0.045)
kPa (264 psi), °C (°F) min. up to 304.8 (12.00) 1.5 (0.060)
<12.0 mm (0.472 in.) 87 (188.6) 87 (188.6) greater than 304.8 (12.00) 2.5 (0.100)
>12.0 mm (0.472 in.)–24.0 mm (0.944 in.) 88 (190.4) 88 (190.4)
>24.0 mm (0.944 in.)–100 mm (3.937 in.) 93 (199.4) 93 (199.4)
Water absorption at 23 °C
Gain in weight, 3.2 mm (0.125 in.) thick, %, 0.8 0.8
max
5.3 Tolerances for shapes other than simple rods and tubes
Tensile strength at 23 °C (73.4°F), min, MPa 55 (8000) 55 (8000) depend upon the shapes themselves. Tolerances for these cast
(psi) shapes are to be specified independently.
Elongation at break, %, min 2 2
6. Detail Requirements
TABLE 2 Sizes and Permissible Tolerances for Wall Thickness of 6.1 The following applies to all specified limits in this
Cast Tube specification: For purposes of determining conformance with
Permissible Wall Thickness Tolerances, this specification an observed value or a calculated value shall
Nominal Wall Thickness, ±, mm (in.) be rounded to the nearest 1 MPa (100 psi) for tensile strength,
mm (in.)
Type A Type B and for all other properties shall be rounded to the nearest unit
up to 4.7 (0.187) 0.5 (0.020) not applicable in the last righthand place of figures used in expressing the
up to 6.4 (0.250) 0.6 (0.025) 1.1 (0.045)
limiting value, in accordance with the rounding method of
up to 9.5 (0.375) 0.9 (0.035) 1.4 (0.055)
up to 12.7 (0.550) 1.1 (0.045) 1.5 (0.060) Practice E29.
up to 19.0 (0.750) 1.5 (0.060) 2.3 (0.090)
up to 25.4 (1.00) 3.8 (0.150) not applicable
6.2 The physical and optical properties in this specification
greater than 25.4 (1.00) 6.4 (0.250) not applicable are based on Finish 1 material unless otherwise specified.
6.3 Rods, tubes, and shapes shall conform to the detail
requirements prescribed in Table 1 and, in addition, shall be so
TABLE 3 Sizes and Permissible Tolerances for Outside Diameter
of Cast Tubes prepared as to conform to the following properties:
6.3.1 Bubbles or inclusions in cast rods, tubes, and shapes
Difference Between
Nominal Outside Outside Diameter Maximum and Minimum shall not exceed 3.96 mm (0.156 in.) in any dimension. No
Diameter, Tolerances, Outside Diameter (One more than three such defects are permissible in any standard
mm (in.) ±, mm (in.) Tube), Not to Exceed,
mm (in.)
length greater than 122 cm (48 in.), or an outside diameter
up to 76.2 (3.0) 0.5 (0.020) 0.6 (0.025)
greater than 76.2 mm (3 in.). Bubbles or inclusions are not
up to 98.4 (3.875) 0.8 (0.030) 1.0 (0.040) permitted in rods, tubes, or shapes less than 122 cm (48 in.) in
up to 152.4 (6.00) 1.1 (0.045) 1.5 (0.060) length and less than 76.2 mm (3 in.) in outside diameter.
up to 304.8 (12.00) 1.6 (0.065) 2.0 (0.080)
greater than 304.8 (12.00) 3.2 (0.125) not applicable
Defects less than 1 mm (0.039 in.) shall be disregarded, unless
grouped to form an objectionable pattern.

7. Number of Tests
5.1.3 Cut-to-size lengths of cast tube are subject to the 7.1 The number of tests shall be consistent with the require-
length tolerances listed in Table 4. ments of Sections 8 and 10.
5.2 Finish 1 and Finish 2 cast rods are subject to the 8. Sampling and Specimen Preparation
following dimensions and tolerances.
5.2.1 Cast rods are subject to the diameter tolerances listed 8.1 Sampling shall be statistically adequate to satisfy the
in Table 5. requirements of Section 10.
5.2.2 Cut-to-size lengths of cast rod are subject to the length 8.2 In the case of rods, tubes, or special shapes from which
tolerances listed in Table 4. the required test specimens cannot be cut, the test specimens

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D5436 − 15
shall be prepared specially from the same raw materials and 9.1.7 Spectral Transmittance—Measure the spectral trans-
under conditions simulating the manufacture of the special size mittance at each specified wavelength with a suitable spectro-
or shape. Otherwise a unit of the manufactured product shall be photometer.
used for testing. 9.1.8 Light Transmittance—Test in accordance with Test
8.3 A batch or lot shall be constituted as a unit of manufac- Method D1003.
ture as prepared for shipment, and shall consist of product from 9.1.9 Haze—Test in accordance with Test Method D1003.
one or more production runs. 10. Certification and Inspection
9. Test Methods 10.1 When specified in the purchase order or contract, the
9.1 The properties enumerated in this specification shall be purchaser shall be furnished certification that samples repre-
determined in accordance with the following test methods: senting each lot have been either tested or inspected as directed
9.1.1 Test Conditions—Conduct the tests in the standard in this specification and the requirements have been met. When
laboratory atmosphere of 23 6 2.0 °C (73.4 6 3.6°F) and 50 6 specified in the purchase order or contract, a report of the test
10 % relative humidity, unless otherwise specified in the test results shall be furnished.
methods or in this specification. 10.2 Lot-acceptance inspection shall be the basis on which
9.1.2 Index of Refraction—Test in accordance with Test acceptance or rejection of the lot is made. The lot-acceptance
Methods D542, using one of the exposed surfaces of the test inspection shall consist of (1) thickness and dimensions, (2)
specimen that has been given any necessary polish without appearance, and (3) deflection temperature.
gross removal of material. 10.3 Periodic check inspection shall consist of the tests
9.1.3 Specific Gravity—Test in accordance with Method A specified for all requirements of the material under this
of Test Methods D792. specification. Supplier shall determine and use an inspection
9.1.4 Water Absorption—Test in accordance with Test frequency which shall be adequate to ensure that the material
Method D570, using the 24-h immersion procedure. Before is certifiable in accordance with 10.4.
testing and following immersion, condition the test specimens
for 24 h at 50 6 3 °C (112 6 5°F) in accordance with 10.4 Certification shall be that the material was
Procedure B of Practice D618. manufactured, sampled, tested, and inspected in accordance
9.1.5 Defection Temperature Under Flexural Load—Test in with this specification and that average values meet the
accordance with Test Method D648. Any square, rectangular, requirements at a confidence level of 95 %.
or cylindrical test specimen is allowed, but calculate the test 10.5 Any report made in accordance with 10.1 shall consist
load used on the basis of a center-loaded beam in which the of the results of the lot-acceptance inspection of the shipment
outer fiber stress produced is 1820 kPa (264 psi). Stack and and the results of the most recent periodic-check inspection.
bind together pieces of thin sheet, 12.7 mm (0.500 in.) in
width, to form a test specimen approximately 12.7 by 12.7 mm 11. Packaging and Marking
(0.500 by 0.500 in.). Load the specimen parallel to the faces 11.1 All packing, packaging, and marking provisions of
containing the original surfaces of the material. Specimens Practice D3892 shall apply to this specification.
12.7 by 12.7 mm (0.500 by 0.500 in.) machined from the face
of thick material shall be loaded parallel to the face containing 12. Keywords
the original surface. 12.1 acrylic; acrylic plastic; cast acrylic; clear weatherable
9.1.6 Tensile Strength and Elongation at Break—Test in plastics; plastic; plastic materials; plastic rods; plastic shapes;
accordance with Test Method D638 using Type I or Type II plastic tubes; PMMA; poly(methyl methacrylate); rods;
specimens at a cross-head speed of 5 mm/min (0.2 in./min). shapes; transparent; tubes

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5436 –
13) that may impact the use of this standard. (June 1, 2015)

(1) Updated tolerances on temperature and humidity in 9.1.1 to


be consistent with Practice D618, Table 1.

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D5436 − 15
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5477 − 18

Standard Practice for


Identification of Polymer Layers or Inclusions by Fourier
Transform Infrared Microspectroscopy (FT-IR)1
This standard is issued under the fixed designation D5477; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope D1600 Terminology for Abbreviated Terms Relating to Plas-


1.1 This practice describes the techniques used for detecting tics
two different polymer entities such as: E131 Terminology Relating to Molecular Spectroscopy
1.1.1 Abnormal specks or spots on a surface or in the film E168 Practices for General Techniques of Infrared Quanti-
that are objectionable as defects and tative Analysis
1.1.2 Layers of different polymeric sheets commonly used E2015 Guide for Preparation of Plastics and Polymeric
as barrier films made by coextrusion. Specimens for Microstructural Examination
IEEE/ASTM SI-10 Standard for Use of the International
1.2 This practice utilizes through-transmittance optical and System of Units (SI):The Modern Metric System
infrared techniques.
1.3 The values stated in SI units are to be regarded as the 3. Terminology
standard. The values given in parentheses are for information 3.1 Definitions:
only. 3.1.1 For definitions of the terms used in this practice, refer
1.4 This standard does not purport to address all of the to Terminologies D883 and D1600.
safety concerns, if any, associated with its use. It is the 3.1.2 For units, symbols, and abbreviations used in this
responsibility of the user of this standard to establish appro- practice, refer to Terminology E131 or IEEE/ASTM SI-10.
priate safety, health, and environmental practices and deter-
4. Significance and Use
mine the applicability of regulatory limitations prior to use.
Specific hazard statements are given in Section 7. 4.1 A speck will ultimately cause a failure to occur by virtue
of its appearance in a film or by the decrease in electrical or
NOTE 1—There is no known ISO equivalent to this standard.
mechanical properties in the polymer substrate (see Specifica-
1.5 This international standard was developed in accor- tion D1248).
dance with internationally recognized principles on standard-
4.2 The analysis of composite layers for barrier purposes by
ization established in the Decision on Principles for the
microscopic Fourier transform infrared spectroscopy (FT-IR)
Development of International Standards, Guides and Recom-
can indicate the adequacy of the barrier tape or indicate why a
mendations issued by the World Trade Organization Technical
barrier may be defective (a missing layer or hole in the layer or
Barriers to Trade (TBT) Committee.
poor coextrusion practice). Fig. 1 represents a typical multi-
layer film.
2. Referenced Documents
2.1 ASTM Standards:2 5. Apparatus
D883 Terminology Relating to Plastics 5.1 FT-IR Spectrophotometer, with nominal 4-cm−1 resolu-
D1248 Specification for Polyethylene Plastics Extrusion tion (see Practices E168).
Materials for Wire and Cable
5.2 Microsampling Accessory, accommodated into the
FT-IR for microscopic infrared analysis, with nominal 6.25-µm
resolution in the infrared mode.
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and
is the direct responsibility of Subcommittee D20.70 on Analytical Methods. 5.3 Optical Microscope, equipped with cross-polarized light
Current edition approved Aug. 1, 2018. Published August 2018. Originally and phase contrast accessories. May be incorporated into the
published as D5477 – 93. Last previous edition approved in 2011 as D5477 – 11. infrared microsampling accessory.
DOI: 10.1520/D5477-18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5.4 Hot-Stage, with temperature readout, is accommodated
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM into the optical microscope or microsampling accessory.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 5.5 Microtome, capable of <25 µm slices 62.5 µm.

*A Summary of Changes section appears at the end of this standard


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D5477 − 18

FIG. 1 Position and Function of Materials in a Typical Multilayer Film

6. Material 8. Specimen Preparation


6.1 Stiff plastic at 25°C, 1.25 mm thick and large enough to 8.1 It is necessary to microtome a thin cross section at right
hold sample (for example, ABS, boPET). angles to the surface of the film or sample in order to
6.2 Cyano-acrylate adhesive. conveniently observe the individual layers or the interior of the
speck.
6.3 Thermoset material for encapsulating sample (for
example, 2-part epoxy, acrylic). 8.2 Samples that do not deflect can be microtomed into the
required thin sections as received.
6.4 Glass microscope slide to support sample slice during
8.3 Flexible samples must be supported during sectioning.
inspection.
Two common support techniques are shown, for flexible
7. Hazards samples, in Fig. 2. On the left, a stiff, flat plastic is used for the
support. A cyano-acrylate adhesive quickly bonds the flexible
7.1 The FT-IR spectrophotometer contains a laser. To avoid sample to the flat plastic support. On the right of Fig. 2, the
eye injury, do not stare directly into the laser beam. sample is supported and cured inside a thermoset compound,
7.2 Use gloves when samples are prepared. The cyano- such as a two-part epoxy. (See Guide E2015.)
acrylate adhesive will attach itself to the fingers and skin. Take 8.4 The entire sandwich is then microtomed in a direction
care to prevent this from occurring. normal to the sample surface. Slice thickness typically of 25-50
7.3 Avoid burns when handling microscopic slides with the µm provide satisfactory transmission of optical and infrared
hot-stage. light.

FIG. 2 Sandwich for Thin Films

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D5477 − 18
9. Procedure The areas of interest may then be photographed and measure-
9.1 Optical Microscopy ments made to quantify the dimensions of inhomogeneities or
9.1.1 The first step is to observe the sample visually in an layers.
optical microscope. The fundamentals of optical microscopy 9.1.4 Since differences in contrast may arise from factors
and sample preparation have been discussed in detail else- other than chemical differences, it is necessary to conduct a
where.3 hot-stage microscopic analysis. In the hot-stage, each of the
9.1.2 The key to optical microscopy analysis is the sample different materials is located when their birefringence disap-
preparation. A 25 to 50-µm thick section allows the visible and pears in the microscope under cross-polarized light, in accor-
IR radiation to go through the section. A section with very few dance with their melting temperature. The hot-stage is heated
knife marks is required. A knife mark is a gouge created in the at a rate of up to 10°C/min. It is advisable to recrystallize the
section by a defect in the microtome knife. Under cross- polymers and recheck the melting points since processing
polarized light, knife marks will confuse and distort the history may influence softening point upon first melting in the
boundaries of an inhomogeneity or layers in a multilayer hot-stage.
specimen. 9.2 Infrared Microscopy—
9.1.3 Once suitable sections have been collected, they are 9.2.1 The infrared microscope permits the identification of
viewed in the optical microscope under cross-polarized light. inclusions and multilayer films down to diameters of 10 µm.
In pigmented materials, it is also necessary to view the 9.2.2 This procedure uses the microscope to locate and
materials in uncrossed polarized light. Differences in contrast analyze small areas of a specimen. The microscope mates with
between inhomogeneities of layers develop in these situations a FT-IR spectrometer. Infrared spectra may then be obtained
due to differences in the intrinsic birefringence of the resins, for each small area of interest.
thermal and stress history, and pigment concentration. The 9.2.3 A schematic of an instrument capable of performing
differences in contrast generally define material boundaries. these tasks is shown in Fig. 3. This microscope accessory is
very useful for locating and then identifying small
3
inhomogeneities, such as a particle, oxidized zone, or layer in
Chamot, E. M., and Mason, C. W., Handbook of Chemical Microscopy, John
Wiley and Sons, Inc., New York, NY, 1985. a plastic film. Its use is unique for the identification of the

FIG. 3 Schematic of An Infrared Microsampling Accessory with Viable Lenses and Polarizers Built In

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D5477 − 18
layers in a multilayer film or sheet. The area of interest is 10. Report
chemically identified by the interpretation of the infrared
10.1 Report the following information:
spectra obtained for that area.
9.2.4 The infrared microscope is focused on the area of 10.1.1 Preparation method,
interest within the section. This typically requires using aper- 10.1.2 Material(s) identification,
tures to isolate the area. All spectra are recorded at 4 cm–1 10.1.3 Method(s) of determination,
resolution. Acceptable signal-to-noise ratios are obtained by 10.1.4 The date of the test.
the co-adding at least 100 spectra.
9.2.5 Many unresolved peaks in the spectrum indicate
11. Keywords
sections need to be thinner, assuming apertures, gain, and other
parameters optimized. 11.1 Fourier transform infrared spectroscopy; microscopy;
9.2.6 A well-resolved spectrum, along with the estimated microsampling; cross-polarized
melting point, may now be used to aid in chemical identifica-
tion.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5491 − 08 (Reapproved 2014)

Standard Classification for


Recycled Post-Consumer Polyethylene Film Sources for
Molding and Extrusion Materials1
This standard is issued under the fixed designation D5491; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* D1600 Terminology for Abbreviated Terms Relating to Plas-


1.1 This document provides for the classification of post- tics
consumer polyethylene (PE) film derived from specific D7209 Guide for Waste Reduction, Resource Recovery, and
sources. It also identifies characteristics useful in determining Use of Recycled Polymeric Materials and Products
the acceptability of the film for recycling into molding and
extrusion materials. It is neither the intent nor the purpose of 3. Terminology
this classification to specify the suitability of the recycled 3.1 Definitions—The definitions used in this classification
material for specific applications. are in accordance with Terminology D883 and Guide D7209.
1.2 This classification provides that the source of the mate- 3.2 Definitions of Terms Specific to This Standard:
rial be listed as an aid in identification. The separation by 3.2.1 bubble packaging film, n—clear or tinted LDPE or
source also improves the usefulness of the material. Sources LLDPE film with little or no print, used to cushion or to protect
are post-consumer PE films from shrink wrap, dry cleaning surfaces, or both.
film, merchandise bags, grocery sacks, stretch wrap, recycle 3.2.2 commercial/industrial liners/bag, n—clear LDPE,
bags, redemption bags, bubble packaging film, and LLDPE, or MDPE film with light or no print, used for the
commercial/industrial liners/bags and overwrap. Other post- shipment of industrial parts, mattresses or textile products, dry
consumer PE films shall be added to this classification when nonputrescible foods, nonhazardous chemicals, etc.
such material streams are defined.
3.2.3 commercial overwrap, n—clear LDPE, LLDPE, or
1.3 It is not the function of this classification to provide data MDPE film with light or no print, used to cover finished
for specific product design or process-performance purposes. products such as carpeting, furniture, yarn, and other interme-
1.4 The supplier shall provide a written certification with diate or retail items during shipment to the distribution outlet or
each shipment stating that the material is derived from post- final consumer.
consumer PE film sources described within this classification. 3.2.4 dry-cleaning film, n—clear or pigmented film made
1.5 The values stated in SI units are to be regarded as the from LDPE, LLDPE, or their blends, with light or no print,
standard. The values given in parentheses are for information used as the outer protective wrap by dry-cleaning establish-
only. ments.
NOTE 1—There is no known ISO equivalent to this standard. 3.2.5 grocery sacks, n—pigmented or unpigmented blends
of polyethylene with or without print, used to carry groceries
2. Referenced Documents from a food market.
2.1 ASTM Standards:2 3.2.6 merchandise bags, n—pigmented LDPE, LLDPE,
D883 Terminology Relating to Plastics MDPE, HDPE, or a combination of these resin types, with
print, used to carry dry goods from a retailer.
3.2.7 nominal density, n—the density of the unpigmented
1
polyethylene resin. The nominal density differs from the
This classification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic apparent density of the material due to the addition of fillers or
Materials. pigments to the resin.
Current edition approved Dec. 1, 2014. Published December 2014. Originally
approved in 1993. Last previous edition approved in 2008 as D5491 - 08. DOI:
3.2.8 recycle bags, n—blue tinted LLDPE or LDPE film
10.1520/D5491-08R14. with light or no print, used to transport items to a recycling
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or facility.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 3.2.9 redemption bags, n—clear or tinted LLDPE or LDPE
the ASTM website. film with little or no print, used to transport beverage bottles

*A Summary of Changes section appears at the end of this standard


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D5491 − 08 (2014)
and cans to a recycler in a “bottle bill” state where beverage 5.1.9 Commercial/Industrial Liners/Bags—Clear LDPE,
containers require a refundable deposit upon purchase. LLDPE, or MDPE film with light or no print, used for the
3.2.10 shrink wrap, n—pigmented or unpigmented film shipment of industrial parts, mattresses or textile products, dry
made from LDPE, LLDPE, or their blends, clear or pigmented, nonputrescible foods, nonhazardous chemicals, etc.
with light or no print, that is typically used to unitize an item 5.1.10 Commercial Overwrap—Clear LDPE, LLDPE, or
or items for stability. MDPE film with light or no print, used to cover finished
products such as carpeting, furniture, yarn, and other interme-
3.2.11 source, n—the original end use of the PE materials
diate or retail items during shipment to the distribution outlet or
described in this specification.
final consumer.
3.2.12 stretch wrap, n—clear or tinted LLDPE film, with no
print, used to unitize an item or items for stability. 6. Ordering Information
6.1 The purchase order or inquiry for these recycled post-
4. Significance and Use consumer PE materials shall state this ASTM specification
4.1 This classification identifies sources of PE film. The number, year of issue, and source.
separation by sources also improves the usefulness of the 6.2 Further definition for the sources listed in 5.1 shall be by
material. Sources are post-consumer PE films from shrink agreement between user and supplier.
wrap, dry cleaning film, merchandise bags, grocery sacks,
stretch wrap, recycle bags, redemption bags, bubble packaging 7. Contamination
film, commercial/industrial liners/bags, and commercial over- 7.1 Contamination by non-polymeric materials, non-
wrap. polyethylene films, and non-film plastics shall not exceed 2 %
4.2 This classification is useful in characterizing post- by weight and must be identified by type.
consumer film to be used as a feedstock for recycling. 7.2 Shipments shall contain minimal contamination (see
4.3 It is neither the intent nor the purpose of this classifica- Note 3) from dirt, mud, stones, grease, glass, metals, and paper.
tion to specify the suitability of the recycled material for 7.3 Materials contaminated with agricultural chemicals,
specific applications. hazardous materials, flammable liquids, and medical wastes are
prohibited.
5. Basis of Classification
7.4 All polymeric materials that present a health hazard, or
5.1 The basis of classification is solely by source. safety hazard, or both, due to their decomposition products at
5.1.1 Shrink Wrap—Pigmented or unpigmented film made polyethylene processing conditions are prohibited.
from LDPE, LLDPE, or their blends, clear or pigmented, with
light or no print, that is typically used to unitize an item or 7.5 The material shall be free of any free-flowing liquid.
items for stability. 7.6 The plastic shall not have visible evidence of damage by
5.1.2 Dry-Cleaning Film—Clear or pigmented film made ultraviolet exposure, that is embrittled, flaky film.
from LDPE, LLDPE, or their blends, with light or no print,
NOTE 2—It is recognized that certain contaminants result in an odor
used as the outer protective wrap by dry-cleaning establish- being present in the recycled material. The acceptability of the type and
ments. level of odor shall be agreed upon between the user and supplier. Methods
5.1.3 Merchandise Bags—Pigmented LDPE, LLDPE, to evaluate odors in recycled materials are being developed elsewhere in
MDPE, HDPE or a combination of these resin types, with the plastics industry.
NOTE 3—It is recognized that despite all efforts to completely prevent
print, used to carry dry goods from a retailer. the presence of contamination, it still does occur. The term “minimal
5.1.4 Grocery Sacks—Pigmented or unpigmented blends of contamination” shall mean film that has been inspected and is visually
polyethylene with or without print, used to carry groceries acceptable for use in good commercial practice. Carefully collect and pack
from a food market. the film for accumulation and shipment.
5.1.5 Stretch Wrap—Clear or tinted LLDPE film, with no 8. Inspection and Certification
print, used to unitize an item or items for stability. Tackifiers
are an acceptable constituent of the wrap. 8.1 The supplier shall provide a written certification with
5.1.6 Recycle Bags—Blue tinted LLDPE or LDPE film with each shipment that the material is derived from post-consumer
little or no print, used to transport items to a recycling facility. sources. The source of these materials, as specified in 5.1, shall
5.1.7 Redemption Bags—Clear or tinted LLDPE or LDPE also be identified in the certification.
film with little or no print, used to transport beverage bottles 8.2 Certification shall be that the material is in accordance
and cans to a recycler in a “bottle bill” state where beverage with this classification and meets the contamination require-
containers require a refundable deposit upon purchase. ments of Section 7.
5.1.8 Bubble Packaging Film—Clear or tinted LDPE or
LLDPE film with little or no print, used to cushion or to protect 9. Keywords
surfaces, or both. Barrier resin or tie layers are acceptable 9.1 plastic films; polyethylene; post-consumer material; re-
components of the construction. covered material; recycled

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SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5491 - 08)
that may impact the use of this standard. (December 1, 2014)

(1) Reapproved with no changes.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5492 − 17

Standard Test Method for


Determination of Xylene Solubles in Propylene Plastics1
This standard is issued under the fixed designation D5492; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 3. Terminology
1.1 This test method is to be used for determining the 25°C 3.1 Definitions:
xylene-soluble fraction of polypropylene homopolymers and 3.1.1 For definitions of plastic terms see Terminology D883
copolymers. and for abbreviations see Terminology D1600.
1.2 This standard does not purport to address all of the 3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the 3.2.1 soluble-fraction (SS)—the percentage of the polymer
responsibility of the user of this standard to establish appro- mass that does not precipitate out when the polymer solution is
priate safety, health and environmental practices and deter- cooled from reflux temperature to +25 6 0.5°C and held at that
mine the applicability of regulatory limitations prior to use. temperature for a specified period of time.
NOTE 1—This test method is technically equivalent to ISO 16152.
4. Summary of Test Method
1.3 This international standard was developed in accor-
dance with internationally recognized principles on standard- 4.1 A weighed amount of sample is dissolved in xylene
ization established in the Decision on Principles for the under reflux conditions. The solution is cooled under con-
Development of International Standards, Guides and Recom- trolled conditions and maintained at a +25°C equilibrium
mendations issued by the World Trade Organization Technical temperature so that the crystallization of the insoluble fraction
Barriers to Trade (TBT) Committee. takes place. When the solution is cooled the insoluble portion
precipitates and is isolated by filtration. The xylene is evapo-
2. Referenced Documents rated from the filtrate, leaving the soluble fraction in the
residue. The percentage of this fraction in the plastic is
2.1 ASTM Standards:2 determined gravimetrically.
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plas-
5. Significance and Use
tics
E456 Terminology Relating to Quality and Statistics 5.1 The results of this test provide a relative measure of the
E691 Practice for Conducting an Interlaboratory Study to total soluble fraction of polypropylene homopolymers and
Determine the Precision of a Test Method copolymers. The soluble fraction approximately correlates to
E2935 Practice for Conducting Equivalence Testing in the amorphous fraction in the polypropylene. Xylene is widely
Laboratory Applications used for determining the soluble fraction in polypropylene as it
is more specific to the atactic fraction than other solvents. The
2.2 ISO Standard:
concentration of a soluble fraction obtained with a specific
ISO 16152 Plastics—Determination of Xylene Solubles of
solvent has been found to relate closely to the performance
Polypropylene3
characteristics of a product in certain applications, for example
film and fiber. Data obtained by one solvent and at one
precipitation time cannot be compared with data obtained by
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics another solvent or precipitation time, respectively.
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materi-
als.
Current edition approved Aug. 1, 2017. Published August 2017. Originally 6. Interferences
approved in 1994. Last previous edition approved in 2010 as D5492 - 10. DOI:
10.1520/D5492-17. 6.1 It is possible that materials with solubilities similar to
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or the soluble fraction, such as additives, can interfere with the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM measurement of solubles. When present in concentrations that
Standards volume information, refer to the standard’s Document Summary page on
are judged to impart a significant error to the soluble-fraction
the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., data, the level of interference must be determined and correc-
4th Floor, New York, NY 10036. tions made.

*A Summary of Changes section appears at the end of this standard


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D5492 − 17
6.2 It is possible that small-particle fillers and pigments and 8. Reagents
insoluble gels present in the polymer can pass through the filter 8.1 Reagent-Grade Ortho-Xylene (o-Xylene)—Assay gas
and cause errors in the measurement. chromatography (GC) = 98 % min; less than 2 % ethylbenzene
6.3 The polymer flakes and spheres must be dried before as established by GC; evaporation residue at 140°C less than
testing to eliminate moisture that can influence the initial 0.002 g/100 mL; boiling point 144°C.
weight of sample added to the flask. 8.2 Reagent-Grade Para-Xylene (p-Xylene)—Assay gas
chromatography (GC) = 98 % min; less than 2 % ethyl-
7. Apparatus benzene as established by GC, evaporation residue at 140°C
7.1 Reflux-Condenser Apparatus, minimum 400 mL, with less than 0.002 g/100 mL; boiling point 138°C.
24/40 glass joint. NOTE 2—Mixed xylene may be used within a laboratory if the ratio of
7.1.1 The use a teflon seal sleeve around the glass joint is an para-xylene to ortho-xylene remains constant and the level of ethyl-
acceptable option provided it has been determined that com- benzene is less than 2 %.
ponents from the sleeve or tape are not extracted by the xylene. 8.3 Reagent grade ortho-xylene shall be used as the refer-
7.1.2 The use of silicone greases or other greases shall be ence solvent whenever there is a dispute between laboratories
avoided. on test results, unless the laboratories agree otherwise.
7.2 Flat- or Round-Bottom Boiling Flask, with one or two 9. Reagent and Specimen Preparation
necks, minimum 400 mL with 24/40 joint, Erlenmeyer flask, or 9.1 Preparation of the Xylene:
flat-bottomed cylindrical bottle. 9.1.1 Stabilization of the xylene is not required.
7.3 Insulation Disk, made of fiberglass or rock wool. NOTE 3—When testing non-stabilized polypropylene powders, (that is,
7.4 Electromagnetic Stirrer Unit, with temperature- unstabilized reactor products) it is recommended that antioxidants be
added to prevent degradation. This addition is optional if previous testing
controlled heating plate, oil bath, heater block, or heating
has shown there is no significant change in xylene soluble level.
mantle capable of maintaining 145 to 150°C. NOTE 4—Butylated hydroxyl toluene (BHT), 4,4 thiobis (6-tert-butyl-
7.5 Stirring Bar. m-cresol), or tetrakis (3,5-di-tert-butyl-4-hydroxy-hydrocinnamate) meth-
ane at an approximate concentration of 0.02 g/L of xylene have been
7.6 Pipet, Class A, 200 mL or equivalent. found to be effective stabilizers. Agitate with a magnetic stirring bar and
heat for a minimum of one hour at 80°C to 90°C to ensure the thorough
7.7 Pipet, Class A, 100 mL or equivalent. mixing of the antioxidants and the xylene. This is a suitable heating
temperature for BHT, which is highly volatile.
7.8 Glass-Stoppered Volumetric Flask, 250 mL.
9.1.2 Degas the xylene. Using nitrogen gas, purge the
7.9 Thermostatically Controlled Water Bath, at +25 6 xylene for a minimum of 1 h every 24 h.
0.5°C.
9.2 Determine the Level of Contamination in the Xylene
7.10 Electromagnetic Stirrers. (Solvent Blank):
7.11 Filter Paper, fluted, Whatman No. 4, No. 541,4 or 9.2.1 The purpose of the solvent blank is to determine
equivalent, at least 125 mm in diameter. whether the xylene to be used contains significant amounts of
evaporation residue or foreign components. A solvent-blank
7.12 Funnel, 60°, or equivalent, at least 125 mm in diam-
test for residue shall be run on every new lot of xylene. Test
eter.
and average the solvent-blank results, for three aliquots per
7.13 Heated Vacuum Oven. bottle or lot of xylene. Each aliquot shall be 200 mL.
7.14 Aluminum or stainless steel pans or beaker at a 9.2.2 If the xylene is an extra pure grade (minimum 99.5 %)
minimum 125 mL capacity, but not larger than 300 mL, with and is used within three days after being opened, the determi-
smooth sides or other suitable container of similar design. nation of the blank is not required. If used more than three days
after being opened, a solvent blank must be run.
7.15 Temperature-Controlled Heating Plate.
NOTE 5—It is recommended that xylene be purchased in glass or
7.16 Analytical Balance, with minimum weighing sensitiv- glass-lined containers and of a size such that the xylene is used within
ity to 0.0001 g (a sensitivity of 0.00001 g is preferred). three days, once opened. Containers of larger size may be used if the
xylene is used up within a short period of time. The purpose of the short
7.17 Desiccator, containing appropriate desiccant. time period is to ensure purity and minimize moisture pickup and other
contaminants.
7.18 Timer, preferably with an alarm, in minutes.
9.2.3 Pipet 200 mL of unstabilized or stabilized xylene into
7.19 Oven, conventional forced air or gravity. a clean empty flask.
9.2.4 Place a 125-mm diameter or larger No. 4 filter paper
or equivalent in a 125-mm diameter of larger funnel in a funnel
4
The sole sources of supply (EU/U.S.) of the apparatus known to the committee rack over a 250-mL glass-stoppered flask.
at this time are Whatman Int’l. Ltd., Maidstone, England or from Fisher Scientific, 9.2.5 For each sample blank, pour the contents from the
711 Forbes Ave., Pittsburgh, PA 15219. If you are aware of alternative suppliers,
please provide this information to ASTM International Headquarters. Your com-
flask into a funnel and allow the filtrate to drip into a second
ments will receive careful consideration at a meeting of the responsible technical flask. Continue the filtration until all the filtrate has been
committee,1 which you may attend. collected.

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D5492 − 17
TABLE 1 Sample Size
Expected Solubles Initial Sample Mass, gA
<8 % by mass 4.0000 ± 0.1000 or 2.000 ± 0.1000
8.0 to 30.0 % by mass 2.0000 ± 0.1000
>30.0 % by mass 2.0000 ± 0.1000 or 1.0000 ± 0.1000
A
See 10.2.

9.2.6 Dry the aluminum or stainless steel vessel (or other


suitable container) for 30 min in an oven at 200°C. Cool the
pans in a desiccator until ready to use. For each sample weigh
a clean, dry vessel on the analytical balance to the nearest
0.0001 g.
9.2.7 With a Class A pipet, pipet a 100-mL aliquot of the
filtered xylene into the weighed vessel.
9.2.8 Place the vessel on a temperature-controlled heating
plate maintained at 145 to 150°C. Allow the aliquot to obtain
a rolling boil to prevent splashing. Blanket the pan with a slow
stream of nitrogen. Continue heating the vessel until the
residue in the dish is almost dry.
9.2.9 Place the vessel into a vacuum oven at 100 6 10°C at
a pressure less than 13-13.5 kPa for a known suitable time
where constant weight is observed.
9.2.10 Cool the vessel to room temperature in a desiccator
for a minimum of 15 minutes and weigh the pan to the nearest
0.0001 g. Calculate the average blank-residual mass of the
three determinations.
9.3 Determine the Percent Soluble Fraction in the Polymer: FIG. 1 Equipment Setup
9.3.1 Dry polypropylene reactor powder before analysis. If
pellets or other large particles are used, drying is not necessary
unless it is known that they contain high levels of moisture. If 10.5 Place an insulation disk on top of the electromagnetic
necessary, dry the samples in a vacuum oven at 70 6 5°C, at a stirrer plate to prevent localized heating of the flask. Position
pressure range of 13-13.5 kPa for a minimum of 20 min. Cool the flask and condenser system on top of the insulation disk
the sample in a desiccator to prevent moisture pickup. (see Fig. 1, which shows a flat-bottom boiling and Erlenmeyer
NOTE 6—For large pellets or other large particles where there is concern flask). Position the nitrogen inlet tube in the top of the
that the polymer sample will not dissolve in a reasonable time frame, grind condenser. Turn on the cooling water to the condenser.
the pellets or particles to an appropriate size to afford a faster dissolution.
Avoid subjecting the sample to excessive mechanical shear, which can 10.6 Blanket the contents of the boiling flask with a slow
lead to an increase in residual solubles level. Ground material shall be flow of nitrogen directed across the top of the condenser, not
dried as specified in 9.3.1. directly into the condenser, to minimize possible xylene loss.
Nitrogen flow rate shall be approximately 2 L/h. Ensure that
10. Procedure nitrogen and water is flowing in the condenser with the aid of
10.1 Weigh out a sample in accordance with Table 1. When bubblers or indicator devices to ensure flow.
the expected solubles level is unknown or referee testing 10.7 Heat the polymer/xylene mixture to reflux temperature
between laboratories is being conducted, a 2.0 6 0.1 g sample while vigorously stirring. The stirring shall be vigorous enough
shall be used, unless there is agreement between the laborato- to obtain a deep vortex, which keeps the boiling under control
ries to use a different sample size. Determine the mass of the and prevents boiling up into the condenser. Ensure that the
sample to the nearest 0.0001 g. Pour the sample into a reflux is gentle so that localized burning, splashing, and
flat-bottom boiling flask. Place a magnetic stirring bar in the sticking of the polymer to the flask walls does not occur.
flask.
10.8 Once the reflux temperature is reached, stir the solution
10.2 Table 1 provides a choice of sample mass. Use the for an additional 30 min. The liquid will appear water-clear.
largest sample mass possible to minimize variability of the test
NOTE 7—For some polymers the total dissolution time can be longer
data, unless from prior experience it is known that the than 30 min for the liquid to appear water-clear.
polymer/xylene solution does not filter readily as in 10.15.
10.9 Remove the heating plate from beneath the flask.
10.3 Pipet 200 mL of unstabilized or stabilized xylene into Detach the flask from the condenser and lightly stopper the
the flask. flask. Cool the solution temperature from reflux temperature to
10.4 Attach the flask to the condenser. below 100°C by cooling the flask in air for 12 to 14 min. A

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D5492 − 17
timer, preferably with an alarm, must be used to ensure that the 10.20 A 100-mL aliquot shall be used in the case of referee
solution is cooled to within a narrow range of temperature from testing.
run to run.
10.21 Place the pan on a temperature-controlled hot plate
10.10 Transfer the flask to a thermostatically controlled maintained at 140 to 150°C. Allow the aliquot to obtain a
water bath at 25 6 0.5°C. Do not shake the flask to break up rolling boil to prevent splashing. Blanket the pan with a slow
any precipitate before immersing the flask in the bath. stream of nitrogen. Continue heating the pan until the residue
10.11 The water bath shall have sufficient cooling capacity in the dish is almost dry. Do not dry completely as this can
to maintain a constant temperature of 25 6 0.5°C during result in degradation of the residue.
cooling.
NOTE 15—Degradation or charring of the sample can lead to inaccurate
NOTE 8—Do not shake the flask while the xylene-polymer solution is results.
still hot as this may create a safety hazard. NOTE 16—Other methods of drying can be used if it has been shown
NOTE 9—Because the rate of cooling affects the crystal size and the rate that they provide equivalent results to the hot plate method (for example,
of crystallization, the time and temperature during the cooling steps are steam bath drying or vacuum oven).
very critical to the final test result.
10.22 Place the pan in a vacuum oven at 100 6 10°C at a
10.12 Precipitation Time: pressure less than 13.3 kPa for a known suitable time where a
10.13 Without stirring, cool the solution for 30 min in the constant weight is achieved.
temperature-controlled bath at 25 6 0.5°C. Using a timer, 10.23 Cool the pan to room temperature in a desiccator and
preferably with an alarm, to ensure that the solution-
weigh the pan to the nearest 0.0001 g.
precipitation time ranges from 30 to 32 min. Remove the flask
from the temperature-controlled bath. Stir or gently shake the 10.24 Obtain the mass of the soluble fraction by subtracting
flask to break up any precipitated-polymer gel. the mass of the pan from the residue-and-pan mass. Adjust the
final percent-soluble-fraction data to account for the percent
NOTE 10—Shorter precipitation times (for example, comparing 30
minutes versus 60 minutes or longer) lead to higher values of soluble residual contamination from xylene.
content for propylene plastics. Users of this method should be warned that
product specification ranges may need to be adjusted in order to 11. Calculation
compensate for these differences.
NOTE 11—With the shorter 30 minute precipitation time, a true 11.1 Calculate the mass percent of the soluble fraction by
equilibrium will not be reached. Consequently, it is very critical that both use of the following equation:
the precipitation time and cooling temperature be controlled very precisely
to minimize variance.
S s 5 ~~ V bo/V b1 3 ~ W 2 2 W 1 ! 2 V bo/V b2 3 B ! /W o ! 3 100
10.14 Place a 125-mm diameter or larger No. 4 filter paper
or equivalent in a 125-mm diameter or larger funnel in a funnel where:
rack over a 250-mL glass-stoppered flask. SS = soluble fraction of sample, %,
10.15 For each sample, pour the contents from the flask into Vbo = original volume of solvent, mL,
a funnel and allow the filtrate to drip into the second flask. Vb1 = volume of aliquot used for solubles determination,
mL,
NOTE 12—With some materials that may have been compounded with Vb2 = volume of aliquot used for blank residuals, mL,
filler or rubber, it may be extremely difficult to do the filtration because of W2 = mass of pan and solubles, g,
clogging of the filter paper. In this case, a filter cloth may be used to W1 = mass of pan, g,
remove the large particles of the filler or the precipitate.
W0 = mass of original sample, g, and
10.16 Continue the filtration until all the filtrate has been B = average blank residual, g.
collected. If the filtered solution is not completely clear it will
11.2 Materials, such as additives, with solubilities similar to
be necessary to repeat the filtration.
the soluble-polymer fraction interfere in the measurement of
10.17 Dry the aluminum pans (or other suitable container percent solubility. Corrections are made to the percent soluble
(refer to 7.14)) for 30 min in an oven at 200°C. Cool the pans fraction only if the material is present in concentrations that are
in a desiccator until ready for use. For each sample weigh a judged to impart a significant error on the soluble-fraction data.
clean, dry pan on the analytical balance to the nearest 0.0001 The material(s) must be 100 % soluble and the mass percent of
g. the material present in the polymer must be known for the
NOTE 13—It has been shown that other types of containers, including following correction to be made:
those made with stainless steel can be used by a laboratory.
10.18 Aluminum pans shall be used in the case of referee Sc 5 Ss 2 Sm
testing.
10.19 With the clean Class A pipet, pipet a 100-mL aliquot
of the soluble filtrate into the weighed pan. where:
Sc = corrected soluble fraction of sample, %,
NOTE 14—Smaller aliquots can be used within the laboratory with the
understanding that the repeatability may be different.
Ss = soluble fraction of sample, %, and

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D5492 − 17

Sm = contamination from materials added to polymer, %, TABLE 2 Xylene Solubles by the 60-Minute Precipitation Method
for Seven Laboratories and Five Materials
where Sm is the sum of the percent for each of the
Values Expressed in %
additives in the material formulation known to be Material
Average SrA SRB rC RD
100 % soluble.
PP 3.58 0.202 0.408 0.565 1.14
PP 5.62 0.490 0.729 1.37 2.04
12. Report PP 6.87 0.230 0.715 0.644 2.00
PP 15.0 0.354 0.799 0.993 2.24
12.1 Report the following information: PP 22.3 1.22 1.63 3.42 4.56
12.1.1 Sample identification and other pertinent A
Sr is the within-laboratory standard deviation for the indicated material. It is
information, obtained by pooling the within-laboratory standard deviations of the test results
12.1.2 Type and grade of xylene, from all of the participating laboratories.
B
12.1.3 Initial sample mass added to flask, Sr = [[s1)2 + (s2)2 +. . . . . . . . . + (sn) 2]/n]1/2
SR is the between-laboratories reproducibility, expressed as standard
12.1.4 Volume of aliquot used, and deviation.
12.1.5 Percent-soluble fraction. (If the data is adjusted for C
SR = [Sr2 + SL2]1/2, whereSL is the standard deviation of laboratory means.
r is the within-laboratory critical interval between two test results = 2.8 × Sr .
soluble additives, report corrected-percent-solubles fraction, D
R is the between-laboratories critical interval between two test results = 2.8 × SR
percent-solubles fraction, and percent contamination. Report .
values to three significant figures.)

13. Precision and Bias between specific laboratories. The principles of 13.2 through
5 13.2.3 then would be valid for such data.)
13.1 Tables are based on a round robin tests conducted in
1996 in accordance with Practice E691, involving five mate- 13.2 Concept of “r” and “R” in Table 2—If Sr and SR have
rials tested by seven laboratories. One laboratory distributed been calculated from a large enough body of data, and for test
the five commercial polypropylene formulations chosen for the results from testing one specimen for each test result, then
evaluation. The individual specimens were prepared at the perform the test as follows:
laboratories that tested them. All pellet samples were extracted 13.2.1 Repeatability—“r” the value below which the abso-
using a 60-minute precipitation time. Each test result was an lute difference between two individual test results obtained
individual determination. Each laboratory obtained two test under repeatability conditions are expected to occur with a
results for each material. Results for the 60-minute precipita- probability of approximately 0.95 (95 %).
tion time are listed in Table 2. These results shall only be used 13.2.2 Reproducibility—“R” the value below which the
as a guideline until a new round robin study can be completed absolute difference between two individual test results obtained
using the 30-minute precipitation time. (Warning—The fol- under reproducibility conditions are to be expected to occur
lowing explanation for r and R (13.2 through 13.2.3) only are with a probability of approximately 0.95 (95 %).
intended to present a meaningful way of considering the 13.2.3 Inferences about equivalence from applying esti-
approximate precision of this test method. Do not apply the mates based only on variability are likely conservative and can
data in Table 2 to acceptance or rejection of material, as these lead to incorrect decisions being made. Equivalence testing in
data apply only to materials tested in the round robin and are ASTM standards is covered by ASTM E2935. These terms and
unlikely to be rigorously representative of the other lots, definitions come from E456 on statistical terminology.
formulations, conditions, material, or laboratories. Users of this Alternatively, it’s permissible to use an appropriate test for two
test method shall apply the principles outlined in Practice E691 means.
to generate data specific to their materials and laboratory, or 13.3 There are no recognized standards by which to esti-
mate bias of this test method.

5
14. Keywords
Supporting data are available from ASTM Headquarters. Request RR:D20-
1199. 14.1 plastics; polypropylene; xylene solubles

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D5492 − 17
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue, D5492 - 10,
that may impact the use of this standard. (August 1, 2017)

(1) Technical additions incorporated and modifications made to (4) Subsections 13.2.1 and 13.2.2 revised definitions of repeat-
Sections 7 (Apparatus), 9 (Reagent and sample preparation- ability and reproducibility.
modified), 10 (Procedure-modified). (5) Notes 8 and 16 added.
(2) Editorial and permissive language changes. (6) Added reference of ASTM E456 and E2935 into the
(3) Subsections 7.1 and 7.2 revised to expand and explain referenced document section.
incorporation of the optional Teflon sleeves and the non-use of
silicon grease.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5507 − 99 (Reapproved 2012)

Standard Test Method for


Determination of Trace Organic Impurities in Monomer
Grade Vinyl Chloride by Capillary Column/Multidimensional
Gas Chromatography1
This standard is issued under the fixed designation D5507; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope valve or alternately as an expanded gas. An appropriate volume


1.1 This is a general-purpose capillary-based test method of the liquid or gas sample is injected to enable the required
for the determination of trace level impurities in high-purity detection limits to be achieved. A preliminary GC separation is
vinyl chloride. This test method uses serially coupled capillary achieved on a 6-m pre-column, the purpose of which is to
PLOT columns in conjunction with the multidimensional remove the bulk of the vinyl chloride peak from the trace peaks
techniques of column switching and cryogenic trapping to of interest. Two heart-cut transfers are made from this pre-
permit the complete separation of the 11 key vinyl chloride column separation, which sends selected portions to a second
impurities in a single 25-min run. column for additional separation. These two cuts incorporate
10 of the 11 trace impurities of interest, but they exclude 1,2
NOTE 1—There is no known ISO equivalent to this standard. ethylene dichloride and the bulk of the vinyl chloride peak. The
1.2 This standard does not purport to address all of the 1,2 EDC peak is eluted from the 6-m pre-column and detected
safety concerns, if any, associated with its use. It is the at the first FID after the two cuts are made.
responsibility of the user of this standard to establish appro- 4.2 The components eluting to the two FID detectors are
priate safety and health practices and determine the applica- identified and quantitated by comparing their retention times
bility of regulatory limitations prior to use. Specific hazards and area counts to those obtained previously from a calibration
statements are given in Section 8. standard run under identical conditions.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:2
5.1 The multidimensional approach permits all of the trace
D883 Terminology Relating to Plastics
impurities to be well separated from the main vinyl chloride
D1600 Terminology for Abbreviated Terms Relating to Plas-
peak, thereby improving quantitative accuracy over established
tics
packed column methods.
F307 Practice for Sampling Pressurized Gas for Gas Analy-
sis 5.2 The minimum detection limit (MDL) for all components
of interest has been shown to be well below 500 ppb for this
3. Terminology test method.
3.1 Definitions—Terminology is in accordance with Termi-
nologies D883 and D1600 unless otherwise indicated. 6. Apparatus
6.1 Instrumentation:
4. Summary of Test Method 6.1.1 HP 5890A3,4(or equivalent), equipped as follows:
4.1 The liquid vinyl chloride sample or calibration standard 6.1.1.1 Split/Splitless Injector System—Must be demon-
is injected either directly using a high-pressure liquid sampling strated to be free of discrimination effects induced by vapor
viscosity differences if helium- or nitrogen-based gas standards
are to be used for instrument calibration.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics 6.1.1.2 Dual Flame-Ionization Detectors.
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Oct. 10, 2012. Published November 2012. Originally
approved in 1994. Last previous edition approved in 2008 as D5507 - 99 (2008)ε1.
3
DOI: 10.1520/D5507-99R12. The sole source of supply of the apparatus known to the committee at this time
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or is Hewlett-Packard Co., 3495 Deer Creek Road, Palo Alto, California 94304.
4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM If you are aware of alternative suppliers, please provide this information to
Standards volume information, refer to the standard’s Document Summary page on ASTM International Headquarters. Your comments will receive careful consider-
the ASTM website. ation at a meeting of the responsible technical committee,1 which you may attend.

*A Summary of Changes section appears at the end of this standard


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7. Reagents and Materials
7.1 Helium—Carrier gas, zero grade, high quality. Traps
should be placed in the supply lines leading to the gas
chromatograph. These traps should reduce oxygen, moisture,
and hydrocarbons to the lowest possible levels.
7.2 Hydrogen—Flame gas, high-purity (hydrocarbon free).
7.3 Air—Flame gas, high-purity (hydrocarbon free).
7.4 Liquid CO2—Coolant, bone-dry grade, liquid-delivery,
1200-psi helium pad recommended.
7.5 Standards:
7.5.1 Primary Standard—The primary standard is a certified
reference standard, which is blended into a stable nitrogen or
helium matrix. The component concentrations should be pre-
pared and reported on an as-in-vinyl chloride basis. The
concentrations of the various components in this standard
should also represent typical values expected for the particular
process or sample. The following is a typical calibration
standard composition:
FIG. 1 Procedure B: On-Line Vaporization Using the LPG Vapor- Component Mole, ppm Weight, ppm
izing Injector
Ethylene 29.4 13.2
Propylene 20.0 13.5
Acetylene 6.8 2.8
6.1.1.3 Column Switching Device A pneumatics control Butane-1 6.8 6.1
system, available from Scientific Glass Engineering, Inc.,4,5 or Trans-butene-2 7.1 6.4
Cis-butene-2 7.5 6.7
equivalent. 1,3 butadiene 6.5 5.6
6.1.1.4 Sub-Ambient Oven Temperature Control (optional). Methyl chloride 36.8 29.7
6.1.1.5 LPG Vaporizing Injector, available from Microana- Vinyl acetylene 12.2 10.2
Ethyl chloride 15.9 16.4
lytics Instrumentation,4,6 or equivalent (Fig. 1). 1,2 ethylene dichloride 11.8 18.7
6.2 Data System—Dual HP 3396A Integrators3,4 (or equiva- Nitrogen balance

lent) permit the acquisition, storage, and reduction of the 7.5.2 Secondary Standard—The secondary standard is a
output signals from the two FIDs simultaneously. After the vinyl chloride-based blend, which is used for method setup and
initial method development, however, it is possible to consoli- day-to-day method calibration. This standard is prepared from
date the output to a single integrator using the instruments actual vinyl chloride product, which is spiked where appropri-
signal switching capability. ate to yield the approximate levels represented in the nitrogen-
6.3 Columns: based primary standard. The final concentrations should be
6.3.1 Pre-Column—100 cm of 0.20-mm inside diameter determined by averaging the results from multiple runs, which
fused silica fixed restrictor coupled to the front of a 6 m by are referenced to the primary standard. This calibration/
0.53-mm inside diameter GSQTM available from J & W recalibration process may be conducted using an alternate GC
Scientific4,7 (or equivalent). procedure.
6.3.2 Analytical Column—9 m by 0.53-mm inside diameter
GSQTM available from J & W Scientific4,7 (or equivalent) plus 8. Hazards
25 m by 0.53 mm inside diameter PORAPLOT UTM 8.1 Appropriate caution must be exercised in handling the
Chrompack4,8 (or equivalent). sample due to the suspected carcinogenicity of vinyl chloride.
6.4 Syringes—A range of high-quality gas-tight syringes Any excess of sample beyond that actually injected into the
representing volumes from 0.5 to 25 mL should be available. column should be routed to a purge waste line to be passed to
These syringes should be equipped with PTFE-tipped plunger a vent hood or other suitable disposal location. This excess
seals and on and off syringe valves to prevent the loss of gas sample includes the inlet splitter vent flow and the sample-loop
sample. purge flow in the case in which a gas-valve injection is being
made.

5
The sole source of supply of the apparatus known to the committee at this time 9. Sampling
is Scientific Glass Engineering 2007 Kramer Lane, Austin, Texas 78758.
6
9.1 This section is to be followed for all samples, including
The sole source of supply of the apparatus known to the committee at this time
is Microanalytics Instrumentation, 2713 Sam Bass Rd., Round Rock, TX 78681. unknown samples and the synthetic standards.
7
The sole source of supply of the apparatus known to the committee at this time
9.2 Samples should be supplied to the laboratory in high-
is J & W Scientific, 91 Blue Ravine Road, Folsom, California 95630-4714.
8
The sole source of supply of the apparatus known to the committee at this time pressure sample cylinders, obtained using the procedure de-
is Chrompack Inc., 1130 Route 202, Raritan, NJ 08869. scribed in Practice F307 or similar standards.

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E. Open Valve A and then Valve B. The liquid will expand,
filling the larger cylinder. Close Valve A and disconnect at E.
NOTE 2—To prevent possible rupture of the liquid-filled pipe cylinder,
the sample cylinder and its contents should be at room temperature prior
to sampling, and the liquid should be allowed to remain in the pipe
cylinder for only a minimum of time.
(2) Connect the cylinder containing the vaporized sample to
the chromatograph gas valve. Evacuate the sample loop and the
lines up to the sample cylinder. Close the valve to the vacuum
source and allow the sample loop to fill with sample up to
atmospheric pressure. Repeat the evacuation and filling of the
sample loop with vaporized sample. Turn the valve so that the
vaporized sample is displaced with carrier gas into the chro-
matograph.
9.5.2.2 Procedure B—On-line vaporization using the LPG
Vaporizing Injector (or equivalent). An alternate approach that
has been used successfully for the automated on-line LPG to
vapor conversion and sample introduction is shown in Fig. 1.
The vapor injection occurs in the upper half of this assembly
FIG. 2 Procedure A: Off-Line Vaporization
labeled “hot zone.” The automated injection process proceeds
as follows:
9.3 Place the cylinder in a horizontal position in a safe place (1) The lower valve of the sample cylinder is opened to
such as a hood. Check to see that the container is at least permit the flow of liquid to the fixed restricter (35 to 45-µm
one-half full by opening the valve slightly. The container is at pinpoint restriction or equivalent).
least one-half full if liquid is emitted (a white cloud of vapors). (2) The constant-pressure force above the liquid drives
Do not analyze any samples or use any synthetic standard if the liquid across the fixed restrictor at a constant rate.
liquid in the container is below this amount. (3) The vapor formed in the heated vaporizer tube is mixed
9.4 Place the cylinder in a vertical position and repressure to prior to passing through the block out valve and on through the
1.208 MPa (175 psig) with the chromatographic carrier or sample loop to vent.
equivalent inert gas through the valve at the top of the cylinder, (4) The sample loop purge is permitted to proceed for a
ensuring that no air enters during the operation. fixed period of time that is sufficient to ensure a complete purge
of the loop volume.
9.5 Use either of the following two procedures for obtaining (5) The block out valve automatically shuts off the flow of
a sample from the container: vapor to the sample loop after the sample-loop purge period.
9.5.1 Liquid Sample—Connect the cylinder to the liquid (6) A short delay period is permitted after sample block out
valve on the chromatograph using a minimum length of and before sample injection. This delay ensures that the sample
connecting tubing, so that sample is withdrawn from the loop is permitted to decay back to atmospheric pressure.
bottom of the cylinder and a liquid sample is obtained. The (7) The gas sampling valve is then actuated to inject the
liquid valve on the chromatograph must be designed in such a sample loop contents into the flowing carrier gas stream and
manner that full sample pressure can be maintained through the simultaneously begin the GC run.
valve without leaking and that means are provided for trapping
a liquid sample in the chromatograph valve under static flow 10. Preparation of Apparatus
conditions. With the exit of the chromatograph valve closed,
open the valve on the cylinder. Open the exit from the 10.1 The column/transfer tube combination is installed as
chromatograph valve slowly so that liquid flows through the outlined in the schematic shown in Fig. 3 (by-pass operation)
connecting line and valve. Close the exits so that the liquid and Fig. 4 (heart-cut operation).
sample is trapped in the valve. Perform the necessary opera- 10.2 Initial Instrument Parameters:
tions to introduce the liquid sample into the chromatograph 10.2.1 Columns:
column. 10.2.1.1 Pre-Column—100 cm of 0.20-mm inside diameter
9.5.2 Vaporized Sample: fused silica fixed restrictor coupled to the front of a 6 m by
9.5.2.1 Procedure A—Off-Line Vaporization: 0.53-mm inside diameter GCQTM available from J & W
(1) Assemble the apparatus in a manner similar to that Scientific4,7 (or equivalent).
illustrated in Fig. 2. Disconnect the 1700-cm3 cylinder at E and 10.2.1.2 Analytical Column—9 m by 0.53-mm inside diam-
evacuate. Close Valve B and open Valves C and D, allowing eter GSQTM plus 25 m by 0.53 mm inside diameter PORA-
the liquid sample to flow into the small cylinder. Open Valve B PLOT UTM (Chrompack).
slowly and allow the sample to flow through until a steady slow 10.2.2 Injection Mode—Split.
stream of liquid emerges from B. Close Valves B, C, and D in 10.2.3 Split Ratio—At 1:1.
that order, trapping a portion of the liquid sample in the pipe 10.2.4 Split Volume—At 15 mL/min.
cylinder. Attach the evacuated cylinder (1700-cm3 volume) at 10.2.5 Injection Volume—At 1.00 mL.

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10.3.1 Equilibrate the GC oven for isothermal operation at
150°C.
10.3.2 With the system operated in the monitor mode (that
is, heart-cut valve open and plunger up), a series of 1.0-mL gas
injections are made with a sample of high-purity vinyl chlo-
ride. The outputs from both detectors should be observed while
these test probes are being made.
10.3.3 When the mid-point pressure is set below the balance
point, splitting of the test peak will occur at the mid-point
restrictor, and responses will be recorded from both detectors.
10.3.4 The mid-point pressure is increased slightly after
each such injection until the pressure differential is reached, at
which the test peak is absent (or acceptably small) from the
second detector. This is the correct pressure differential for
normal heart-cut and back flush operations.
FIG. 3 By-Pass Operation
10.3.5 This pressure tuning process should be required only
once for any combination of columns and restrictors.
10.4 Establishing Column Switching Parameters—The
heart-cut and cold-trap times in the instrument parameters (see
10.2) can be used as a general guideline or can be developed
from the following procedure:
10.4.1 The process of establishing the heart-cut times for
this procedure is begun by determining retention times for the
pre-column separation only. This is accomplished by holding
the system in the monitor mode while the first complete run is
made with the secondary standard. A sample volume of 1.0 to
1.25 mL should be used for this and all subsequent injections.
10.4.2 The retention times from this first run are then used
to determine the approximate start and stop times required for
heart-cut No. 1. This cut should include all of the trace
impurities, which elute prior to the vinyl chloride peak (that is,
FIG. 4 Heart-Cut Operation ethane, ethylene, acetylene, propylene, and methyl chloride).
The best results are achieved in practice if the first cut is
10.2.6 Injection Temperature—180°C. terminated just into the front edge of the large vinyl chloride
10.2.7 Detector Temperature—240°C. peak.
10.2.8 Column Temperature (Typical): 10.4.3 After the times are finalized for the first cut, the last
of those tuning runs is used to determine the appropriate times
Ramp 1 40°C initial, 3 min, 7°C/min, 100°C final, 2–min hold
Ramp 2 5°C/min, 135°C final, 0–min hold for heart-cut No. 2. This cut includes ethyl chloride and the C4
Ramp 3 15°C/min, 155°C final, 5-min hold unsaturates group (that is, cis-butene-2, trans-butene-2,
10.2.9 Carrier Gas: butene-1, 1,3-butadiene, and vinyl acetylene).
Pre-column pressure 82.8 kPa (12.0 psi) 10.4.4 The final step in establishing the MDGC parameters
Midpoint pressure 55.2 kPa (8.0 psi) is to select the on and off times for the LCO2 cold trap
10.2.10 Detectors: operation. These times will be selected on the basis of the start
Monitor FID B—Signal 2
and stop cut times, which were determined for heart-cut No. 2.
Analytical FID A—Signal 1 The cold trap is turned on at 1.5 min prior to the start of cut No.
10.2.11 Instrument Gas Pressures: 2 and is turned off at 1.0 min after cut No. 2 is completed.
10.4.5 The system is ready for calibration and sample
helium 372.5 kPa (54 psi)
hydrogen 110.4 kPa (16 psi) analysis after the multidimensional parameters have been
air 220.7 kPa (32 psi) determined.
10.2.12 MDGC Event Times (Approximate):
Heart-cut No. 1 0 min 5 s to 4 min 0 s
11. Calibration and Standardization
Cold trap 7 min 0 s to 12 min 15 s 11.1 Initial Calibration—After the initial setup, it is recom-
Heart-cut No. 2 8 min 10 s to 11 min 0 s
mended that 5 to 7 replicate calibration runs be made in
10.2.13 Fixed Resistor—200-µm inside diameter deacti- succession with the secondary calibration standard. The results
vated fused silica 86 cm in length. from the first run should be discarded, and those from the
10.3 Pressure Balancing—The switching system is then remaining runs should be used for the determination of
adjusted to a pressure balanced condition using the following response factors, mean area counts, standard deviations, and
procedure: percent relative standard deviations for each of the trace

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D5507 − 99 (2012)
components. If the variability is found to be within acceptable Aes = integrated-area count for the component from the
limits (less than 3 % RSD for all components), the subsequent standard run.
sample analysis can be conducted. The average response factor
13.2 Alternately, an average response factor can be deter-
for each of the trace components is used for subsequent
mined for each of the components from a series of calibration
calculation.
runs. This factor can in turn be used as a multiplier for
11.2 Continuing Calibration Check—Although the calibra- calculating the concentrations from the subsequent sample
tion results for this test method have proven to be very stable runs.
over long periods of time (days to weeks), it is highly
Qx 5 ~ Ax!~ Rf! (2)
recommended that an instrument-calibration check be made at
least once per day, and preferably once per shift. If the response where:
factor for any component is found to vary from the previous ~ Qes!
calibration by a value greater than 5 %, it will be necessary to Rf 5 (3)
~ Aes!
re-run the calibration standard or locate the cause of the
13.3 Any units can be used for area count concentration, but
variation, or both. If no mechanical problems are found (leaks,
the units selected must be consistent throughout.
etc.) to explain the variation and the system is found to be
functioning correctly otherwise, it will be necessary to adjust 14. Precision and Bias
the calibration to reflect the current level of detector response. 14.1 Precision—The following precision data were devel-
12. Procedure oped within a single laboratory. Table 1 is the precision data for
four impurities that were measured by Procedure B. Each result
12.1 Using the same conditions that were used in the is an average of five or more independent tests made by a
previous calibration runs, inject an identical volume of gas single operator in the same laboratory.
from the vinyl chloride sample to be analyzed. Measure,
record, and store the retention time and area count data for each 14.2 This data is provided to give an operator a range of
of the components of interest. In order to ensure the accuracy values that could be expected using this test method. An
and reproducibility of the analysis, it is essential that good interlaboratory study of precision is being organized.
laboratory procedures be followed when vaporizing the liquid 14.3 The concept of the r values (repeatability limits) in
vinyl chloride and sampling the gas stream. Table 1 is as follows: when comparing two test results for the
same material, obtained by the same operator using the same
13. Calculation
equipment on the same day, the two test results should be
13.1 Calculate the concentrations of each of the components judged not equivalent if they differ by more than the r value for
of interest using the following equation: that material.
~ Ax!~ Qes! 14.3.1 Any judgment in accordance with 14.3 would have
Qx 5 (1) an approximate 95 % (0.95) of being correct.
~ Aes!
where: 14.4 Bias—Bias is systematic error that contributes to the
difference between a test result and true (or reference) value.
Qx = concentration of the components in the vinyl chloride
There are no recognized standards on which to base an estimate
sample,
of bias for this test method.
Qes = concentration of the component in the calibration
standard, 15. Keywords
Ax = integrated-area count for the component from the
15.1 capillary-column chromatography; VCM impurities;
sample run, and
vinyl chloride monomer

TABLE 1 Single Laboratory and Single Operator Repeatability for Four Key Impurities Using Procedure B Vapor Injection
Retention Time (Short-Term) Quantitative (Short Term) Quantitative (Long Term)
(1 day—6 Sequential Runs) (1 day—6 Sequential Runs) (9 day—10 Sequential Runs)
Impurity
Mean, Mean, Mean,
Sr A rB Sr r Sr r
min ppm ppm
Methyl chloride 11.02 0.02 0.057 29.50 0.12 0.340 34.48 0.60 1.698
1,3 butadiene 17.48 0.01 0.028 2.75 0.02 0.057 3.27 0.06 0.170
Vinyl acetylene 17.86 0.01 0.028 5.23 0.03 0.085 10.09 0.14 0.396
Ethyl chloride 18.14 0.01 0.028 17.44 0.09 0.255 19.23 0.29 0.821
A
Sr = standard deviation.
B
r = 2.83 × Sr .

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of infringement of such rights, are entirely their own responsibility.

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Designation: D5508 − 16

Standard Test Method for


Determination of Residual Acrylonitrile Monomer in Styrene-
Acrylonitrile Copolymer Resins and Nitrile-Butadiene
Rubber by Headspace-Capillary Gas Chromatography (HS-
CGC)1
This standard is issued under the fixed designation D5508; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* the polymer, solvent, plus a known standard addition of


1.1 This test method covers the determination of the re- acrylonitrile (AN). Both vials are agitated for a specified time
sidual acrylonitrile (RAN) content in nitrile-butadiene rubbers under ambient conditions. After agitation, the vials are ther-
(NBR), styrene-acrylonitrile (SAN) copolymers, and rubber- mally equilibrated in a constant-temperature bath.
modified acrylonitrile-butadiene-styrene (ABS) resins. 3.2 After completion of the timed equilibration, an aliquot
1.2 Any components that can generate acrylonitrile in the of the heated headspace gas from each vial is injected into a
headspace procedure will constitute an interference. The pres- capillary gas-chromatographic column using an automated
ence of 3-hydroxypropionitrile in latices limits this procedure injection system. The capillary column will provide the chro-
to dry rubbers and resins. matographic resolution necessary to isolate the AN from other
volatiles potentially present. The AN response is measured
1.3 The values stated in SI units are to be regarded as using a nitrogen-specific detector (NPD). The raw data signal
standard. No other units of measurement are included in this is converted to a relative RAN concentration through a
standard. standard addition calculation.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Significance and Use
responsibility of the user of this standard to establish appro- 4.1 A measurement of the residual acrylonitrile in nitrile
priate safety and health practices and determine the applica- rubbers (NBR), styrene-acrylonitrile copolymers or ABS ter-
bility of regulatory limitations prior to use. Specific precau- polymers will determine the polymer’s suitability for various
tionary statements are given in 6.3 and 6.4. applications.
NOTE 1—There is no known ISO equivalent to this standard. 4.2 Under optimum conditions, the minimum level of de-
2. Referenced Documents tection of RAN in NBR, SAN, or ABS terpolymers is approxi-
mately 50 ppb.
2.1 ASTM Standards:2
E691 Practice for Conducting an Interlaboratory Study to 5. Apparatus
Determine the Precision of a Test Method
5.1 Gas Chromatograph, equipped with a nitrogen-
3. Summary of Test Method phosphorus specific detector, backflush valve (see Fig. 1), split
3.1 Two dispersions (in o-dichlorobenzene) are prepared injector, and capable of accepting megabore (0.53 mm inside
and sealed in headspace vials for each polymer; one vial diameter) fused silica capillary columns. Detector make-up gas
contains the polymer in solvent while the second vial contains is required.
NOTE 2—The use of a backflush configuration will provide for
1
operating advantages, but its use is optional. Chlorinated solvents quench
This test method is under the jurisdiction of ASTM Committee D20 on Plastics the alkali bead in a nitrogen-phosphorous detector, producing a loss of
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods and
signal. While the bead (signal) will recover as the solvent evacuates the
Section D20.70.02 on Chromatography.
detector, repeated quenching during a multi-run sequence may produce
Current edition approved Sept. 1, 2016. Published September 2016. Originally
approved in 1994. Last previous edition approved in 2009 as D5508 - 94a(2009)ε1.
instabilities in the signal (and precision) over the sequence period.
DOI: 10.1520/D5508-16.
2
5.2 Automated Headspace Sampler, shall have a thermost-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
atted sample tray capable of 90°C heating with constant
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on heating times. Automated sampling of the headspace gas in the
the ASTM website. sample vials via a heated, constant-volume sample loop or

*A Summary of Changes section appears at the end of this standard


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D5508 − 16
7. Sampling and Storage
7.1 The polymer test unit (sample) submitted for analysis
shall be supplied in the form of a 13⁄4 in. (45 mm) cube.
7.2 All test specimens shall be taken from the interior of the
polymer-test unit to minimize the contribution of surface
effects on the residual-acrylonitrile level.
7.3 Keep all polymer-test units in sealed containers. Ana-
lyze test-specimen solutions immediately after preparation.
Report any analysis delays along with the test results.

8. Calibration
FIG. 1 Configuration of Eight-Port Valve Backflush Assembly 8.1 Preparation of External Standard Solutions:
8.1.1 Tare (to the nearest 0.1 mg) a 25-mL volumetric flask
containing 10 mL of o-dichlorobenzene (DCB).
8.1.2 Weigh (to the nearest 0.1 mg) into the 25-mL volu-
pressure balancing sampling mechanism is required. Conduct metric flask 40 6 5 mg of AN. Dilute to the mark with DCB.
sampling to the gas chromatograph by means of a heated Label this solution as the “external-standard master solution”.
transfer line of minimum dead volume. 8.1.3 Add 1 mL of the “external-standard master solution”
to a clean 10-mL volumetric flask containing 2 mL of DCB.
5.3 Fused Silica Porous-Layer-Open-Tubular (PLOT) Cap-
Dilute to the mark with additional DCB. Label this solution as
illary Column, 30 m × 0.53 mm inside diameter.
the “external-standard working solution”.
NOTE 3—The column should be cut so as to have a 3 m section for the 8.1.4 Prepare fresh “master” and “working” solutions each
pre-column (Column 1) and a 27-m section for the analytical column week and keep refrigerated at 4°C using Parafilm “M” to seal
(Column 2).
volumetric stoppers.
5.4 Variable Restrictor.
8.2 Generation of the External-Standard Calibration
5.5 Data-Recording Device—A strip-chart recorder, record- Curve:
ing integrator, or computer-based data system is suitable.
NOTE 5—A new external-standard calibration curve should be gener-
5.6 Wrist-Action Shaker. ated each week to account for any changes in the AN response due to NPD
bead fluctuations.
5.7 Analytical Balance, 0.1-mg readability.
8.2.1 Transfer 5 mL of DCB into seven clean headspace
5.8 Headspace Vials, 20-mL capacity. vials, using a volumetric pipet.
5.9 Aluminum Crimp Caps, 20-mm diameter. 8.2.2 Add 0 (solvent blank), 1, 5, 10, 20, 60, or 100 µL of
the “external-standard working solution”, respectively, to the
5.10 Septa, TFE-fluorocarbon-faced silicone construction, vials.
20-mm diameter. 8.2.3 Seal each vial immediately after addition with a
5.11 Crimper, for 20-mm crimp caps. septum and crimp cap.
8.2.4 Establish the instrument parameters as listed in Annex
6. Reagents and Materials A1.
8.2.5 Obtain the peak-area values for AN in each of the
6.1 Purity of Reagents—Chemicals of the highest purity
standards.
shall be used in all tests. Solvents shall have a minimum of
volatile impurities. Other grades shall only be used after
9. Procedure
ascertaining that the reagent is free of interferences.
9.1 Determine the Target AN Weight for Polymer Test Units:
6.2 Observe all health and safety recommendations for each
9.1.1 Weigh (to the nearest 0.1 mg) into a clean headspace
chemical, as prescribed by the manufacturer.
vial 400 6 10 mg of polymer. Add 5 mL of DCB, using a
6.3 Acrylonitrile, 99 + %. (Warning—Acrylonitrile is an volumetric pipet. Seal vial with septum and crimp cap.
OSHA-regulated carcinogen and should not be released into 9.1.2 Place the vial on a wrist-action shaker, set at maxi-
the laboratory atmosphere. All work involving acrylonitrile mum agitation for 16 h under ambient conditions.
should be carried out in a hood or with proper personal 9.1.3 Analyze the sample under the same instrument param-
protection to minimize human exposure.) eters as was used to generate the external-standard calibration
6.4 o-Dichlorobenzene. (Warning—o-Dichlorobenzene is curve.
moderately toxic and should only be handled in a hood or with 9.1.4 Obtain the peak-area value for AN.
proper personal protection to limit human exposure.) 9.2 Preparation of AN Standard-Addition Solution:
NOTE 4—Each lot of o-dichlorobenzene should be analyzed under the NOTE 6—The following steps in preparing the AN standard addition
same instrumental conditions as the NBR samples to ensure that impuri- solution are given as an illustration only. Depending on the target weights
ties are not present that will interfere with the acrylonitrile peak. involved, the AN concentration of these solutions may need to be adjusted.

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9.2.1 Tare (to the nearest 0.1 mg) a 25-mL volumetric flask 10.1.1 Plot AN added (ng) versus AN peak area (seven data
containing 10 mL of DCB. points obtained from 8.2.5).
9.2.2 Weigh (to the nearest 0.1 mg) into the 25-mL volu- 10.1.2 Perform a linear regression on the data set. The
metric flask 165 6 10 mg of AN. Dilute to the mark with DCB. inverse of the slope, 1/slope, will be the AN-response factor
Label this solution as the “AN master solution”. with units of ng/unit area.
9.2.3 Add 50 µL of the “AN master solution” to a clean 10.2 Target AN weight:
10-mL volumetric flask containing 2 mL of DCB. Dilute to the 10.2.1 Calculate the target AN weight in ng for the polymer:
mark with DCB. Label this solution as the “AN working
solution”. This solution has an AN concentration of 33 ng/µL. TW, ~ ng! 5 A ~ sp! 3 RF (1)
9.2.4 Prepare fresh “master” and “working” solutions where:
weekly or as needed for varying target levels. Keep refrigerated A(sp) = peak area for AN in polymer test specimen (from
at 4°C using Parafilm “M” to seal volumetric stoppers. 9.1.4), and
9.3 Determination of the RAN Concentration: RF = external-response factor for AN from the external-
calibration curve in ng/unit area (from 10.1.2).
NOTE 7—At this point, it must be decided which type of determination
is required: (1) Linearity Test—Required for each different polymer type 10.3 RAN Concentration:
as it is encountered. Once the linearity of the standard addition has been 10.3.1 Linearity Test:
established it may be assumed valid for further analyses for that specific
10.3.1.1 Plot AN added (ng) versus AN peak area (eight
polymer type. (2) Precision Test—Required for each different polymer
type as it is encountered. Once the precision of the standard addition has data points obtained from 9.3.6) to obtain a curve as illustrated
been established it may be assumed valid for further analyses for that in Fig. 2.
specific polymer type. (3) Routine Test —Both linearity and precision 10.3.1.2 Perform a linear regression on the data set. The
have been established for the specific polymer type to be tested. Only a correlation coefficient will determine the degree of linearity for
routine RAN determination is required.
the specific polymer type. The absolute value of the x-intercept
9.3.1 Weigh (to the nearest 0.1 mg) into a clean headspace will give the weight of AN in the polymer.
vial 400 6 10 mg of polymer. Add 5 mL of DCB to the vial,
NOTE 9—The degree of linearity increases as the correlation coefficient
using a volumetric pipet. Loosely place the septum and crimp nears a value of 1.
cap on the vial. Do not seal at this time.
9.3.1.1 For a Linearity Test—Prepare eight vials with the 10.3.1.3 Calculate the RAN concentration for the polymer
identical weight (65 mg) of polymer in each vial. in parts per billion (ng/g):
9.3.1.2 For a Precision Test—Prepare a minimum of twelve
RAN, ~ ppb! 5
? x 2 intercept? (2)
vials with the identical weight (65 mg) of polymer in each W ~ sp!
vial.
where:
9.3.1.3 For a Routine Test—Prepare two vials per polymer
test specimen with the identical weight (65 mg) of polymer in |x − intercept| = absolute value of the x-intercept obtained
each vial. from the linear regression (nanograms), and
9.3.2 Add to each vial a volume of the “AN working W(sp) = weight (grams) of NBR (polymer).
solution,” resulting in a weight of AN based on the target
weight as specified below for each test.
9.3.2.1 For a Linearity Test—Add 0, 0.25, 0.5, 1, 2, 3, 4, and
five times the target AN weight to the vials, respectively.
9.3.2.2 For a Precision Test—Make no addition to six vials
and an addition of three times the target AN weight to the other
six vials.
NOTE 8—This group of vials is to be run as six sets each containing one
from the null addition and three times the target weight. The pairing is
carried through the calculations.
9.3.2.3 For a Routine Test—Make no addition to one vial
and an addition of three times the target AN weight to the
remaining vial.
9.3.3 Seal vials with crimper (immediately after an addi-
tion).
9.3.4 Place the vials on a wrist-action shaker, set at maxi-
mum agitation for 16 h under ambient conditions.
9.3.5 Establish the instrument parameters as listed in Annex
A1.
9.3.6 Obtain the peak-area values for AN from each vial.
10. Calculations
FIG. 2 Plot of Detector Response Versus Nanograms Acryloni-
10.1 External-Standard-Calibration Curve: trile Added

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10.3.2 Precision Test: 12.3 No valid statement of between-laboratories reproduc-
10.3.2.1 Plot AN added (ng) versus AN peak-area values for ibility is acceptable for data from less than six laboratories.
the six pairs of data points obtained from 9.3.6. Six lines will However, within-laboratory repeatability precision values are
be plotted. shown in Table 1.
10.3.2.2 Perform a linear regression on each of the six pairs NOTE 11—Laboratories interested in performing between labs repro-
of data points. Determine the x-intercept for each pair (six ducibility round-robin testing should contact ASTM headquarters.
values total). 12.3.1 The concept of the “r” and “(r)” values (repeatability
10.3.2.3 Calculate the RAN concentration using each limits) in Table 1 is as follows: when comparing two test
x-intercept value. Refer to 10.3.1.3. results for the same material obtained by the same operator
10.3.2.4 Calculate the mean for the six RAN values ob- using the same equipment on the same day, judge the two test
tained above. Determine the standard deviation (s) for the data results as not equivalent if they differ by more than the “r” or
set. The precision will be expressed as the percent relative “(r)” value for that material.
standard deviation (%RSD). 12.3.2 Any judgement in accordance with 12.3.1 would
have an approximate 95 % (0.95) probability of being correct.
s
%RSD 5 3 100 (3) 12.4 Bias—By definition, bias is a measure of the system-
mean RAN value
atic error that contributes to the difference between the mean
10.3.3 Routine Test: value of the test-result population and an accepted reference or
10.3.3.1 Plot AN added (ng) versus AN peak area values true value. It is possible that one or more bias elements
(two points obtained from 9.3.6). contribute to the systematic error.
10.3.3.2 Perform a linear regression on the data set. The 12.5 No statement of bias is made for this test method due
absolute value of the x-intercept will be the weight (ng) of AN to the lack of an absolute method for comparison.
in the polymer.
13. Keywords
10.3.3.3 Calculate the RAN concentration for the polymer
in parts per billion (ng/g). Refer to 10.3.1.3. 13.1 headspace-gas chromatography; nitrile rubber; residual
acrylonitrile; styrene-acrylonitrile copolymers
11. Report TABLE 1 Type I—Precision (Residual Acrylonitrile in Nitrile-
11.1 Report parts per billion (ng/g) residual acrylonitrile Butadiene Rubber)
monomer. Within Laboratories
Material Mean, ppm
srA rB (r)C

12. Precision and Bias A 0.66 0.07 0.20 30.5


B 1.25 0.13 0.35 28.4
NOTE 10—Data were generated only for nitrile rubbers, although C 1.12 0.23 0.64 57.7
comparable repeatability can be expected for SAN and ABS resins. D 0.17 0.04 0.11 67.7
E 0.16 0.05 0.13 82.5
12.1 Precision statements were prepared in accordance with “A” 1.84 0.07 0.19 10.3
Practice E691. “B” 0.66 0.04 0.12 17.9
“C” 38.5 2.06 5.77 15.0
12.2 Ten materials (NBRs) of varying levels of the test “D” 10.8 0.73 2.04 18.9
“E” 1.25 0.12 0.34 27.3
component were used in the interlaboratory program. Materials
A
“A” through “E” were 30 to 37 % AN NBRs, and materials sr = Within-laboratory standard deviation.
B
r = Repeatability (in measurement units).
“A” through “E” were 40 to 48 % AN NBRs. Testing was C
(r) = Repeatability (in percent).
conducted in four laboratories.

ANNEX

(Mandatory Information)

A1. PARAMETERS FOR GAS CHROMATOGRAPH AND HEADSPACE SAMPLER

A1.1.4 Linear Flow Velocity—38 cm/s (at approximately


130°C).
A1.1 Gas Chromatograph Parameters:
A1.1.5 Oven Temperature Profile—Isothermal, 155°C.
A1.1.1 Injection Mode—Capillary, split.
A1.1.2 Injection Temperature—250°C. A1.1.6 Detector Type—Nitrogen-phosphorus detector.
A1.1.3 Carrier Gas—Helium. A1.1.7 Detector Temperature—300°C.

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TABLE A1.1 Parameters for Gas Chromatograph and Headspace A1.2 Headspace Sampler Parameters:
Sampler
Time min:s Action Description A1.2.1 Bath Temperature—90°C.
:01 Probe Needle enters vial A1.2.2 Equilibration Time—3 hour.
:03 Pressure Vial pressurization begins
:18 Pressure Vial pressurization stops
:19 Vent/fill loop Initialize sample loop filling
A1.2.3 Sample Loop Size—3 mL.
:28 Vent/fill loop Close sample loop-loop filled
:33 Inject Flush sample onto analytical column
A1.2.4 Sample Loop Temperature—110°C.
1:03 Vent/fill loop Open loop to vent
1:04 Pressure Initialize sample loop cleaning A1.2.5 Injection Cycle Parameters—(For volume-
2:34 Pressure Stop carrier flow through sample loop controlled headspace sampler).
2:35 Vent/fill loop Close vent
2:36 Inject Stop injection cycle
2:37 Probe Needle exits vial

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D5508 - 94a(2009)ε1) that may impact the use of this standard. (September 1, 2016)

(1) Updated ISO equivalency statement.


(2) Removed product-specific references throughout docu-
ment.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5511 − 18

Standard Test Method for


Determining Anaerobic Biodegradation of Plastic Materials
Under High-Solids Anaerobic-Digestion Conditions1
This standard is issued under the fixed designation D5511; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 1.6 This standard does not purport to address all of the
1.1 This test method covers the determination of the degree safety concerns, if any, associated with its use. It is the
and rate of anaerobic biodegradation of plastic materials in responsibility of the user of this standard to establish appro-
high-solids anaerobic conditions. The test materials are ex- priate safety, health, and environmental practices and deter-
posed to a methanogenic inoculum derived from anaerobic mine the applicability of regulatory limitations prior to use.
digesters operating only on pretreated household waste. The Specific hazards are given in Section 8.
anaerobic decomposition takes place under high-solids (more NOTE 1—This test method is equivalent to ISO 15985.
than 30 % total solids) and static non-mixed conditions. 1.7 This international standard was developed in accor-
1.2 This test method is designed to yield a percentage of dance with internationally recognized principles on standard-
conversion of carbon in the sample to carbon in the gaseous ization established in the Decision on Principles for the
form under conditions found in high-solids anaerobic digesters, Development of International Standards, Guides and Recom-
treating municipal solid waste (1, 2, 3, 4).2 This test method mendations issued by the World Trade Organization Technical
may also resemble some conditions in biologically active Barriers to Trade (TBT) Committee.
landfills where the gas generated is recovered and biogas
production is actively promoted by inoculation (for example, 2. Referenced Documents
codeposition of anaerobic sewage sludge, anaerobic leachate 2.1 ASTM Standards:3
recirculation), moisture control (for example, leachate D618 Practice for Conditioning Plastics for Testing
recirculation), and temperature control (for example, short- D883 Terminology Relating to Plastics
term injection of oxygen, heating of recirculated leachate) (5, D1293 Test Methods for pH of Water
6, 7). D1888 Methods Of Test for Particulate and Dissolved Matter
in Water (Withdrawn 1989)4
1.3 This test method is designed to be applicable to all
D2908 Practice for Measuring Volatile Organic Matter in
plastic materials that are not inhibitory to the microorganisms
Water by Aqueous-Injection Gas Chromatography
present in anaerobic digesters operating on household waste.
D3590 Test Methods for Total Kjeldahl Nitrogen in Water
1.4 Claims of performance shall be limited to the numerical D4129 Test Method for Total and Organic Carbon in Water
result obtained in the test and not be used for unqualified by High Temperature Oxidation and by Coulometric
“biodegradable” claims. Reports shall clearly state the percent- Detection
age of net gaseous carbon generation for both the test and E260 Practice for Packed Column Gas Chromatography
reference samples at the completion of the test. Furthermore, E355 Practice for Gas Chromatography Terms and Relation-
results shall not be extrapolated past the actual duration of the ships
test. 2.2 APHA-AWWA-WPCF Standards:
1.5 The values given in SI units are to be regarded as the 2540 D Total Suspended Solids Dried at 103°–105°C5
standard. 2540 E Fixed and Volatile Solids Ignited at 550°C5
212 Nitrogen Ammonia5

1 3
This test method is under the jurisdiction of ASTM Committee of D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and is the direct responsibility of Subcommittee D20.96 on Environmen- contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
tally Degradable Plastics and Biobased Products. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Jan. 15, 2018. Published February 2018. Originally the ASTM website.
4
approved in 1994. Last previous edition approved in 2012 as D5511 – 12. DOI: The last approved version of this historical standard is referenced on
10.1520/D5511-18. www.astm.org.
2 5
The boldface numbers is parentheses refer to a list of references at the end of Standard Methods for the Examination of Water and Wastewater, 17th Edition,
the text. 1989, American Public Health Association, 1740 Broadway, New York, NY 10018.

*A Summary of Changes section appears at the end of this standard


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D5511 − 18
2.3 ISO Standard:6
ISO 13641-1 Water quality—Determination of inhibition of
gas production of anaerobic bacteria—Part 1: General test
ISO 15985 Plastics—Determination of the ultimate anaero-
bic biodegradability and disintegration under high-solids
anaerobic-digestion conditions—Method by analysis of
released biogas

3. Terminology
3.1 Definitions—Definitions of terms applying to this test
method appear in Terminology D883.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 methanogenic inoculum—anaerobically digested or-
ganic waste containing a high concentration of anaerobic
methane-producing microorganisms.

4. Summary of Test Method FIG. 1 Test Setup


4.1 This test method consists of selection and analysis of
material for testing, obtaining a concentrated anaerobic inocu- 6. Apparatus
lum from an anaerobic laboratory-scale digester, exposing the
material to an anaerobic-static-batch fermentation at more than 6.1 Inverted Graduated Cylinder or Plastic Column, in
20 % solids, measuring total carbon in the gas (CO2 and CH4) water or other suitable device for measuring gas volume. The
evolved as a function of time, and assessing the degree of water in contact with the gas must be at a pH of less than two
biodegradability. during the whole period of the test to avoid CO2 loss through
dissolution in the water. The gas-volume-measuring device, as
4.2 The percentage of biodegradability is obtained by de- well as the gas tubing, shall be of sufficient quality to prevent
termining the percent of conversion of carbon from the test gas migration and diffusion between the system and the
material to carbon in the gaseous phase (CH4 and CO2). This surrounding air (see Fig. 1).
percentage of biodegradability will not include the amount of
carbon from the test substance that is converted to cell biomass 6.2 Gas Chromatograph, (optional) or other apparatus,
and that is not, in turn, metabolized to CO2 and CH4. equipped with a suitable detector and column(s) for measuring
methane and carbon dioxide concentration in the evolved
5. Significance and Use gases.
5.1 Biodegradation of a plastic within a high-solids anaero- 6.3 Incubator, or hot-water bath capable of maintaining the
bic digestion unit is an important phenomenon because it will test bottles at 37°C (62°C) or 52°C (62°C) for the duration of
affect the decomposition of other waste materials enclosed by the test.
the plastic and the resulting quality and appearance of the 6.4 Erlenmeyer Flasks, with sufficient capacity for the
digestate after an anaerobic digestion process. Biodegradation experiment and openings of at least 7-cm diameter, set up so
of plastics could allow for the safe disposal of these plastics that no loss of gas occurs.
through aerobic and anaerobic solid-waste-treatment plants.
This procedure has been developed to permit the determination 6.5 pH Meter, precision balance (60.1 g), analytical balance
of the rate and degree of anaerobic biodegradability of plastic (60.1 mg), thermometer, and barometer.
products when placed in a high-solids anaerobic digester for 6.6 Devices, suitable for determining volatile fatty acids by
the production of digestate from municipal solid waste. aqueous-injection chromatography, total Kjeldahl nitrogen,
5.2 Limitations—Because there is a wide variation in the ammonia nitrogen, dry solids (105°C) and volatile-solids
construction and operation of anaerobic-digestion systems and (550°C) concentrations.
because regulatory requirements for composting systems vary, 7. Reagents and Materials
this procedure is not intended to simulate the environment of
any particular high-solids anaerobic-digestion system. 7.1 Anaerboic Inoculum, derived from a properly operating
However, it is expected to resemble the environment of a anaerobic digester with pretreated household waste as a sole
high-solids anaerobic-digestion process operated under opti- substrate.
mum conditions. More specifically, the procedure is intended 7.2 Analytical-Grade Cellulose, for thin-layer chromatogra-
to create a standard laboratory environment that will permit a phy as a positive control.
rapid and reproducible determination of the anaerobic biode- 7.3 Polyethylene, as a negative control (optional). It is
gradability under high-solids digestion conditions. optimal if it is in the same form as the form in which the
sample is tested (for example, film polyethylene for film
6
Available from American National Standards Institute (ANSI), 25 W. 43rd St., samples, pellets of polyethylene if the sample is in the form of
4th Floor, New York, NY 10036, http://www.ansi.org. pellets, etc.).

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D5511 − 18
8. Hazards 9.3 Analyses are performed after dilution of the inoculum
8.1 The procedure given in this test method involves the use with distilled water on a ratio of distilled water to inoculum of
of an inoculum composed of biologically and possibly chemi- 5 to 1 on a weight over weight basis.
cally active materials known to produce a variety of diseases.
Avoid contact with these materials by wearing gloves and other 10. Test Specimen
appropriate protective garments. Use good personal hygiene to 10.1 The test specimen shall be of sufficient carbon content,
minimize exposure. analyzed in accordance with Test Method D4129, to yield
8.2 It is possible that the solid-waste mixture contains sharp carbon dioxide and methane volumes that can be accurately
objects. Take extreme care when handling this mixture to avoid measured by the trapping devices described. Add more test
injury. specimen when low biodegradability is expected, up to 100 g
on a dry weight basis of the test specimen.
8.3 The biological reactor is not designed to withstand high
pressures; operate it at close to ambient pressure. 10.2 It is acceptable if the test specimen is in the form of
films, powder, pellets, formed articles, or in the form of a dog
8.4 This test method includes the use of hazardous chemi- bone and conforming to Practice D618. The test set-up shall be
cals. Avoid contact with the chemicals and follow the manu- able to handle articles that are 100 mm by 50 mm by 4 mm
facturer’s instructions and Material Safety Data Sheets. thick.
8.5 The methane produced during this procedure is explo-
sive and flammable. Upon release of the biogas from the 11. Procedure
gas-collection system, take care in venting the biogas to the
11.1 Inoculum Medium:
outside or to a hood.
11.1.1 Remove enough inoculum (approximately 15 kg)
9. Inoculum from the post-fermentation vessel and mix carefully and
consistently by hand in order to obtain a homogeneous
9.1 The inoculum must be derived from a properly operat- medium.
ing anaerobic digester functioning with a pretreated household 11.1.2 Test three replicates each of a blank (inoculum only),
waste as a sole substrate. The pretreated household waste shall positive control (thin-layer chromatography cellulose), nega-
come from an existing waste treatment facility treating munici- tive control (polyethylene), and the test substance being
pal solid waste, where through sorting, shredding, sieving, or evaluated.
other means, a fairly homogeneous organic fraction is pro- 11.1.2.1 Manually mix 1000 g wet weight (at least 20 % dry
duced of less than 60 mm. The digester shall be operating for solids) of inoculum in a small container for a period of 2 to 3
a period of at least four months on the organic fraction, with a min with 15 to 100 g of volatile solids of the test substance or
retention time of a maximum of 30 days under thermophilic the controls for each replicate. (Determine dry solids and
conditions (52 6 2°C). Gas-production yields shall be at least volatile solids in accordance with APHA Standards , 2540, and
15 mL at standard temperature and pressure of biogas per gram Test Method D1888).
of dry solids in the digester and per day on the average for at
11.1.2.2 For the three blanks containing inoculum only,
least 30 days.
manually mix 1000 g of the same inoculum in a small container
9.1.1 It is preferable to derive the inoculum from a digester
for a period of 2 to 3 min with the same intensity as was done
operating under dry (>20 % total solids) conditions, but it is
for the other vessels containing test substance or controls.
acceptable to derive it from a wet fermentation whereby the
anaerobically digested sludge is dewatered through 11.1.2.3 Determine the weight of the inoculum and test
centrifugation, with a press or through drying at a maximum substance added to each individual Erlenmeyer flask accu-
temperature of 55°C to a dry-solids content of at least 20 %. rately.
11.1.3 Add the mixtures to a 2-L wide-mouth Erlenmeyer
9.2 The prepared inoculum shall undergo a short post- flask and gently spread and compact the material evenly in the
fermentation of approximately seven days at the same operat- flask to a uniform density.
ing temperature from which it was derived. This means that the 11.1.4 After placing the Erlenmeyer flask in a water bath or
inoculum is not fed but allowed to post-ferment anaerobically incubator, connect it with the gas-measurement or gas-
by itself. This is to ensure that large easily biodegradable collection device.
particles are degraded during this period and also to reduce the
11.1.5 Record room temperature and atmospheric pressure
background level of degradation of the inoculum itself.
prior to turning on the heating system of the incubator or water
9.2.1 The most important biochemical characteristics of the
bath.
inoculum shall be as follows:
9.2.1.1 pH—Between 7.5 and 8.5 (in accordance with Test 11.2 Incubation:
Methods D1293), 11.2.1 Incubate the Erlenmeyer flasks in the dark or in
9.2.1.2 Volatile Fatty Acids (VFA)—Below 1 g/kg wet diffused light at 52°C (62°C) for thermophilic conditions, or
weight (in accordance with Practice D2908), and 37°C (62°C) for mesophilic conditions for a period of nor-
9.2.1.3 NH4+-N—Between 0.5 and 2 g/kg wet weight (in mally 15-30 days.
accordance with APHA Test Method 212 and Test Method 11.2.1.1 For the test to be considered valid, the positive
D3590). control must achieve 70 % biodegradation within 30 days.

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D5511 − 18
11.2.1.2 The incubation time shall be run until no net gas mean C g ~ test! 2 mean C g ~ blank!
% biodegradation: 3 100 (2)
production is noted for at least five days from both the positive Ci
control and test substance reactors.
where:
11.2.1.3 The test substance and the positive control shall be
Cg = amount of gaseous carbon produced, g, and
run for the same duration.
Ci = amount of carbon in test compound added, g.
11.2.2 Control the pH of the water used to measure biogas
production to less than two by adding HCl. 12.4 Calculate the standard error, se, of the percentage of
biodegradation as follows:
11.3 Analytical Measurements:
S e 5 SQRT~~ s 2 test /n1 ! 1 ~ s 2 blank /n2 !! 3 100/C i (3)
11.3.1 Make at least five measurements of gas volume per
week in order to establish the gas production as a function of where:
time. n1 andn2 = number of replicate test and blank digesters
11.3.2 Determine methane and carbon dioxide concentra- respectively, and
tion by using analytical devices suitable for the detection and s = standard deviation of the total gaseous carbon
quantification of these gases, such as a gas chromatograph with produced.
an appropriate detector, in accordance with Practices E260 and 12.5 Calculate the 95 % confidence limits (CL) as follows:
E355.
95 % CL 5 % biodegradation6 ~ t 3 s e ! (4)
11.3.3 Verify the quality of the inoculum by analyses for
pH, volatile fatty acids, and total Kjeldahl nitrogen (in accor- where:
dance with Test Methods D1293 and D3590 and Practice t = t-distribution value for 95 % probability with
D2908). (n1 + n2 − 2) degrees of freedom, thus n = 3 + 3 − 2 = 4.
11.4 At the end of the digestion period, allow the setup to
cool to room temperature for 8 h and determine the following
parameters: 13. Interpretation of Results
11.4.1 Total gas-volume production produced during the 13.1 Information on the toxicity of the plastic material
test, provides useful information in interpreting whether the plastic
11.4.2 Gas composition at the end of the test, material falls within the scope of this test method. ISO 13641-1
11.4.3 Weight loss of each vessel, and is an appropriate standard suitable to assess the toxicity of
11.4.4 Room temperature and atmospheric pressure at the plastic materials to anaerobic sludge.
end of the test. 13.2 This test method includes the use of thin-layer chro-
matography cellulose as a positive control. If sufficient biodeg-
12. Calculation radation (a minimum of 70 % for cellulose after 30 days, and
the deviation among the cellulose replicates is less than 20 %
12.1 By using the total carbon content in the test specimen,
of the mean) is not observed within the duration of the test
calculate the maximum theoretical gas production (carbon
method, then the test method must be regarded as invalid and
dioxide plus methane) originating from the anaerobic biodeg-
shall be repeated with fresh inoculum.
radation of the test specimen added, based on the following
biochemical transformations: 13.3 Results shall not be extrapolated past the actual dura-
C12 H 2 →CH4 (1)
tion of the test.
13.4 If the confidence interval on percentage biodegradation
C1O 2 →CO2 calculated in 12.5 includes zero, then the percentage biodeg-
Each mmole (12 mg) of organic carbon from the test sample radation is not statistically significantly different from zero.
can be converted into 1 mmole of gaseous CH4 or CO2, or both.
14. Report
One mmole of gas produced occupies 22.4 mL at standard
temperature and pressure (STP). 14.1 Report the following data and information:
14.1.1 Information on the inoculum, including: source;
12.2 Temperature and Pressure—Measure the percentages
mesophilic or thermophilic; pH; volatile fatty acids (in milli-
of CH4 and CO2 and transform the gas volumes to STP. Correct
grams per kilogram); NH4+-N in grams per kilogram); percent
also for water vapor-pressure and atmospheric-pressure varia-
of dry solids; percent volatile solids; date of collection and use;
tion during the test. Calculate the amount of gaseous carbon.
storage time and conditions; and handling and potential accli-
Determine the mean (of the three replicates) net gaseous
mation to the test material,
carbon production by anaerobic biodegradation of the test
14.1.2 Carbon content of the plastic material, the positive
substances by subtracting the mean gaseous carbon production
control and the negative control (if used), and maximum
of the control (three replicates) containing only the inoculum.
theoretical gas production (carbon dioxide and methane),
12.3 Calculate the percent of biodegradation by dividing the 14.1.3 Numerical extent and graphical display of the cumu-
average net gaseous carbon production of the test material by lative gas productions of each replicate over time for the
the original average amount of total carbon of the test inoculum, positive control, negative control (if used) and test
compound and multiplying by 100: substance; numerical extent and graphical display of the

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D5511 − 18
percentage biodegradation over time for the positive control, TABLE 1 Results from Within-Laboratory Testing for the
negative control (if used) and test substance, Anaerobic Biodegradability of Cellulose Under the High-Solids
Anaerobic Conditions at 52°C
14.1.4 Result of the calculation of the 95 % confidence
95 %
limits, and Biodegradability Standard
Confidence
14.1.5 Analysis of gas as percent methane and percent After Ten Days Deviation
Limit
carbon dioxide for each reading at the end of the test, or each Run 1 86.7 % 0.3 % 2.4 %
Run 2 85.6 % 2.2 % 4.5 %
time the gas is released to the atmosphere during the course of Run 3 86.2 % 1.1 % 5.4 %
the test. Run 4 84.2 % 4.5 % 9.0 %
Mean of Four Runs 85.7 % .. ...
15. Precision and Bias Mean Variance With ... 5.1 % 10.2 %
95 %
15.1 The precision and bias of the procedure in this test Confidence Limit
method for measuring the anaerobic biodegradation of plastic
materials under high-solids anaerobic conditions is being
determined. containing cellulose as the positive control, with a standard
15.2 Preliminary results for within-laboratory repeatability deviation of 0.3 % and a 95 % confidence limit interval of
testing are presented in Table 1. These data represent four 2.4 %. Fig. 2 represents the gas production of three replicates
different determinations of the degradation of thin-layer chro- with inoculum only as the blanks, while Fig. 3 gives a view of
matography cellulose as the positive reference material under the total biogas production after cellulose as a positive refer-
thermophilic conditions (52°C). The average degradation of ence has been added. Fig. 4 represents the net biogas produc-
cellulose after ten days in the test method is 85.7 %, with a tion from the cellulose after the average biogas production
mean variance of 5.1 % and a 95 % confidence limit interval of coming from the inoculum has been subtracted.
610.2 % for the four runs. All four runs were carried out
within a twelve-month period by the same operators. Figs. 2-4 16. Keywords
represent the results of the first run in which a biodegradability 16.1 anaerobic biodegradation; anaerobic digestion; biodeg-
of 86.7 % was obtained as the mean for the three replicates radation; high-solids digestion; landfill; plastics test method

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D5511 − 18

FIG. 2 Representative Plot Showing Total Biogas Production


from Inoculum for Three Replicate Specimens Tested in a Single
Run

FIG. 3 Representative Plot Showing Total Biogas Production


from Inoculum Plus Cellulose for Three Replicate Specimens
Tested in a Single Run

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D5511 − 18

FIG. 4 Representative Plot Showing Net Biogas Production from


Cellulose for Three Replicate Specimens Tested in a Single Run

REFERENCES

(1) De Baere, L. A., et al., “High-Rate Dry Anaerobic Composting (5) Campbell, D. J. V., and Croft B., “Landfill Gas Enhancement:
Process for the Organic Fraction of Solid Wastes,” Biotechnology and Brogborough Cell Programme,” Landfill Gas: Energy and Environ-
Bioengineering Symposium No. 15, John Wiley & Sons, Inc., New ment 90, United Kingdom Department of Energy, 1990, p. 281.
York, N.Y., 1986, p. 321. (6) Westlake, K., “Landfill Microbiology,” Landfill Gas: Energy and
(2) De Wilde, B., et al., “Dry Anaerobic Conversion of Source Separated Environment 90, United Kingdom Department of Energy, 1990, p.
Household Waste to Biogas and Humotex,” Journal of Resource 271.
Management and Technology, Vol 18, No. 1, 1990, p. 40. (7) Suflita, J. M., et al., “The World’s Largest Landfill: A Multidisci-
(3) European Patent No. 84200801.3, 06.06. 1984. plinary Investigation,” Environmental Science and Technology, Vol
(4) U.S. Patent No. 4 684 468, 03.31.1986 . 26, No. 8, 1992, p. 1486.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5511–12)
that may impact the use of this standard. (January 15, 2018)

(1) Deleted 11.1.2.4.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5523 − 15

Standard Test Method for


Polyurethane Raw Materials: Acidity by Argentometric
Determination of Hydrolyzable Chlorine in Monomeric,
Aromatic Isocyanates1
This standard is issued under the fixed designation D5523; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 3.2.1 acidity—the acid strength of a sample expressed as


1.1 This test method measures the hydrolyzable chlorine parts per million hydrochloric acid (HCl) present.
content of monomeric, aromatic isocyanates used as polyure- 3.2.2 hydrolyzable chlorine—the amount of chlorine re-
thane raw materials and expresses it as HCl acidity. The test leased as chloride ion under the conditions of the test,
method is applicable to toluene diisocyanate (TDI) and mono- expressed as parts per million chlorine.
meric methylene di(phenylisocyanate), known as MDI. The
main sources of hydrolyzable chlorine and, therefore, acidity in 4. Summary of Test Method
monomeric aromatic isocyanates are carbamyl chlorides, acid 4.1 The sample reacts with 2-propanol to form urethanes
chlorides, and dissolved phosgene. All of these compounds and hydrochloric acid, which is liberated from the labile
react with alcohols and water to form hydrochloric acid. carbamyl chlorides, acid chlorides, and dissolved phosgene.
1.2 This test method applies only to monomeric isocyanates The chlorides of the liberated acid are then determined
in which all of the acidity is derived from species that generate potentiometrically using standard methanolic silver nitrate
HCl on solvolysis. solution and calculated as parts per million HCl.

1.3 The values stated in SI units are to be regarded as the 5. Significance and Use
standard. 5.1 This test method is suitable for research or for quality
1.4 This standard does not purport to address all of the control to characterize TDI and MDI.
safety concerns, if any, associated with its use. It is the 5.2 This test method was developed to overcome problems
responsibility of the user of this standard to establish appro- with low-level acidity determinations that use glass electrodes
priate safety and health practices and determine the applica- in the presence of reagent alcohol solvents. Reagent alcohols
bility of regulatory limitations prior to use. contain acidic and basic species, which complicate the glass
NOTE 1—There is no known ISO equivalent to this standard. electrode methods at low levels of acidity.
2. Referenced Documents 6. Interferences
2
2.1 ASTM Standards: 6.1 Acidic species that do not generate chloride ions under
D883 Terminology Relating to Plastics the conditions of this test method will not be determined
because acidity is determined indirectly from the chloride ion
3. Terminology concentration.
3.1 Definitions—For definitions of terms used in this test 6.2 Acidic species that do not produce chloride ions are
method, see Terminology D883. expected to be negligible at low levels of acidity and for the
3.2 Definitions of Terms Specific to This Standard: monomeric isocyanates in this test method.
6.3 Care must be taken to avoid chloride contamination of
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics glassware and sample containers.
and is the direct responsibility of Subcommittee D20.22 on Cellular Materials -
Plastics and Elastomers. 7. Apparatus
Current edition approved April 1, 2015. Published May 2015. Originally
approved in 1994. Last previous edition approved in 2010 as D5523 - 10. DOI: 7.1 Potentiometric Titrator.
10.1520/D5523-15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
7.2 Combination Silver Billet Electrode (Note 2).
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 7.3 Oven, 70°C (Note 3).
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 7.4 Magnetic Stirrer.

*A Summary of Changes section appears at the end of this standard


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D5523 − 15
NOTE 2—The combination silver billet electrode is to be stored in 0.01 11. Procedure
N methanolic silver nitrate solution in order to keep the electrode
conditioned properly. The use of chloride containing solutions must be 11.1 Weigh 10.0 g of the sample into a beaker and record the
avoided during storage and maintenance of the apparatus. weight to the nearest 0.0001 g (Note 4).
NOTE 3—Monomeric MDI samples can be solid when received in the
laboratory. An oven is to be used to melt the sample prior to beginning the 11.2 Add 100 mL of 2-propanol to the beaker, cover, and stir
test procedure. the sample for 10 min.
8. Reagents and Materials 11.3 Add 100 mL of methanol, cover, and continue stirring
the sample solution for an additional 20 min (Note 5).
8.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that 11.4 Add ten drops of concentrated nitric acid solution to
all reagents conform to the specifications of the Committee on the sample solution.
Analytical Reagents of the American Chemical Society where 11.5 Cool the sample solution to room temperature in an ice
such specifications are available.3 Other grades can be used, bath if necessary.
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of 11.6 Titrate the sample solution potentiometrically with the
the determination. appropriate methanolic silver nitrate solution (Note 6).
8.2 Methanol. 11.7 Record the volume of titrant used to reach the end point
to at least the nearest 0.001 mL.
8.3 2-Propanol.
11.8 If the chloride content of the reagents is in question,
8.4 Nitric Acid, concentrated, 70 %.
run a blank (steps 11.1 to 11.7 with no isocyanate sample
8.5 Silver Nitrate. added) to ensure that the reagents are free of chloride interfer-
8.6 Methanolic Silver Nitrate Solution (0.01 N)—Prepare ences. If chloride is detected, subtract the volume (mL) of
by dissolving 1.70 g AgNO3/L of solution. Potentiometrically AgNO3 required to titrate the blank from the volume (mL) of
standardize with titration-grade sodium chloride frequently AgNO3 required to titrate the sample.
enough to detect changes of 0.00005 N. NOTE 4—The beaker must be of such size to accommodate approxi-
mately 300 mL of solution, and it must be of a shape to allow the proper
8.7 Methanolic Silver Nitrate Solution (0.001 N)—Prepare coverage for the electrode. For monomeric MDI, it is acceptable to gently
by dissolving 0.170 g AgNO3/L of solution. Potentiometrically warm the beaker on a hot plate to keep the sample molten prior to the
standardize with titration-grade sodium chloride frequently addition of 2-propanol. This will assist in dissolution of the sample. Once
2-propanol has been added, remove the beaker from the hot plate.
enough to detect changes of 0.000005 N.
NOTE 5—The stirring times were chosen to ensure an adequate reaction
9. Sampling time for material that has been adjusted with an acid chloride. In
monomeric, unadjusted material, it is acceptable to reduce the stirring
9.1 Since organic isocyanates react with atmospheric times to those required to obtain uniform solutions and stable electrode
moisture, take special precautions in sampling. Usual sampling responses (approximately 2 min).
methods, even when conducted rapidly, can cause contamina- NOTE 6—For expected acidities or hydrolyzable chlorines below 20
ppm, use the 0.001 N methanolic silver nitrate solution as the titrant. For
tion of the sample with insoluble urea. Therefore, blanket the expected acidities or hydrolyzable chlorines above 20 ppm, use the 0.01
sample with dry air or nitrogen at all times. (Warning— N methanolic silver nitrate solution as the titrant.
Diisocyanates are eye, skin, and respiratory irritants at concen-
trations above the occupational exposure limit (TLV or PEL). 12. Calculation
Diisocyanates can cause skin and respiratory sensitization
(asthma) in some people. Once sensitized, it is essential to limit 12.1 Calculate the acidity, as ppm HCl, as follows:
further exposure to diisocyanates. Use a combination of S 3 N 3 36.465 3 106
acidity 5 (1)
engineering controls and personal protective equipment, in- W 3 1000
cluding respiratory, skin and eye protection, to prevent over- where:
exposure to diisocyanates. Consult the product suppliers’
Safety Data Sheet (SDS) for more detailed information about S = AgNO3 required for titration of the sample, mL (If
potential health effects and other specific safety and handling a blank is run, subtract the volume in mL of
instructions for the product.) AgNO3 required to titrate the blank from the
volume (mL) of AgNO3 required to titrate the
10. Test Conditions sample),
N = normality of AgNO3 solution, meq/mL,
10.1 Since isocyanates react with moisture, keep laboratory
W = sample weight, g,
humidity low, preferably around 50 % relative humidity. See 36.465 = equivalent weight of HCl, mg/meq,
warning statement in 9.1. 1000 = factor for converting milligrams to grams, and
106 = factor for converting to parts per million.
3
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not 12.2 Because hydrolyzable chlorine is measured, the ppm
listed by the American Chemical Society, see Analar Standards for Laboratory hydrolyzable chlorine can be calculated as follows:
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, S 3 N 3 35.465 3 106
hydrolyzable chlorine 5 (2)
MD. W 3 1000

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D5523 − 15
where: Conshohocken, PA 19428–2959, if you are interested in
S = AgNO3 required for titration of the sample, mL (If participating in the development of precision and bias data for
a blank is run, subtract the volume in mL of this test method.
AgNO3 required to titrate the blank from the 13.2 A limited round robin was conducted with nine labo-
volume (mL) of AgNO3 required to titrate the ratories.
sample), 13.2.1 It has been estimated that duplicate results for either
N = normality of AgNO3 solution, meq/mL,
acidity or hydrolyzable chlorine by the same analyst are to be
W = sample weight, g,
35.465 = equivalent weight of Cl, mg/meq, considered suspect if they differ by 63.9 ppm for results
1000 = factor for converting milligrams to grams, and greater than 10 ppm and 60.6 ppm for results less than 10
106 = factor for converting to parts per million. ppm.
13.2.2 It has been estimated that results reported by different
13. Precision and Bias4 laboratories for either acidity or hydrolyzable chlorine are to be
13.1 Attempts to develop a precision and bias statement for considered suspect if they differ by 615.5 ppm for results
this test method have not been successful due to the limited greater than 10 ppm and 63.5 ppm for results less than 10
number of laboratories participating in round-robin tests. Data ppm.
on precision and bias cannot be given for this reason. Contact
the Chairman, Subcommittee D20.22 (Section D20.22.01), 14. Keywords
ASTM, 100 Barr Harbor Drive, PO Box C700, West 14.1 acidity; HC; hydrolyzable chlorine; isocyanates; iso-
cyanates aromatic; MDI; methylene-4,4’-di(phenylisocyanate);
4
Supporting data have been filed at ASTM International Headquarters and may methylene di(phenylisocyanate); polyurethane; raw materials;
be obtained by requesting Research Report RR:D20-1181. TDI; test method; titration; toluene diisocyanate

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D5523 –
10) that may impact the use of this standard. (April 1, 2015)

(1) Subsection 9.1: Sampling—The previous warning state- (3) Section 12: Calculations—Added calculations to perform if
ment was edited to remove non-mandatory language and a blank is used.
updated with input from the Center for the Polyurethanes (4) Section 14: Keywords—Changed keyword for MDI to be
Industry’s (CPI) Product Stewardship Committee. consistent with that used in the other polyurethane raw material
(2) Section 10: Test Conditions—Removed redundant informa- analysis methods.
tion.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

Copyright by ASTM Int'l (all rights reserved); Sat Jun 20 15:33:06 EDT 2020
3
Downloaded/printed by
Indian Inst of Tech Kharagpur (Indian Inst of Tech Kharagpur) pursuant to License Agreement. No further reproductions authorized.
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5526 − 18

Standard Test Method for


Determining Anaerobic Biodegradation of Plastic Materials
Under Accelerated Landfill Conditions1
This standard is issued under the fixed designation D5526; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope “biodegradable” claims. Reports shall clearly state the percent-


1.1 This test method covers determination of the degree and age of net gaseous carbon generation for both the test and
rate of anaerobic biodegradation of plastic materials in an reference samples at the completion of the test. Furthermore,
accelerated-landfill test environment. This test method is also results shall not be extrapolated past the actual duration of the
designed to produce mixtures of household waste and plastic test.
materials after different degrees of decomposition under con- 1.5 The values stated in SI units are to be regarded as the
ditions that resemble landfill conditions. The test materials are standard.
mixed with pretreated household waste and exposed to a 1.6 This standard does not purport to address all of the
methanogenic inoculum derived from anaerobic digesters op- safety concerns, if any, associated with its use. It is the
erating only on pretreated household waste. The anaerobic responsibility of the user of this standard to establish appro-
decomposition occurs under dry (more than 30 % total solids) priate safety, health, and environmental practices and deter-
and static nonmixed conditions. The mixtures obtained after mine the applicability of regulatory limitations prior to use.
this test method can be used to assess the environmental and Specific hazards statements are given in Section 8.
health risks of plastic materials that are degraded in a landfill.
NOTE 1—There is no known ISO equivalent to this standard.
1.2 This test method is designed to yield a percentage of
1.7 This international standard was developed in accor-
conversion of carbon in the sample to carbon in the gaseous
dance with internationally recognized principles on standard-
form under conditions that resemble landfill conditions. It is
ization established in the Decision on Principles for the
possible that this test method will not simulate all conditions
Development of International Standards, Guides and Recom-
found in landfills, especially biologically inactive landfills.
mendations issued by the World Trade Organization Technical
This test method more closely resembles those types of
Barriers to Trade (TBT) Committee.
landfills in which the gas generated is recovered or even
actively promoted, or both, for example, by inoculation (code- 2. Referenced Documents
position of anaerobic sewage sludge and anaerobic leachate
recirculation), moisture control in the landfill (leachate 2.1 ASTM Standards:3
recirculation), and temperature control (short-term injection of D618 Practice for Conditioning Plastics for Testing
oxygen and heating of recirculated leachate) (1-7).2 D883 Terminology Relating to Plastics
D1293 Test Methods for pH of Water
1.3 This test method is designed to produce partially de- D1888 Methods Of Test for Particulate and Dissolved Matter
graded mixtures of municipal solid waste and plastics that can in Water (Withdrawn 1989)4
be used to assess the ecotoxicological risks associated with the D2908 Practice for Measuring Volatile Organic Matter in
anaerobic degradation of plastics after various stages of an- Water by Aqueous-Injection Gas Chromatography
aerobic biodegradation in a landfill. D3590 Test Methods for Total Kjeldahl Nitrogen in Water
1.4 Claims of performance shall be limited to the numerical D4129 Test Method for Total and Organic Carbon in Water
result obtained in the test and not be used for unqualified by High Temperature Oxidation and by Coulometric
Detection
E260 Practice for Packed Column Gas Chromatography
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.96 on Environmentally
3
Degradable Plastics and Biobased Products. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 15, 2018. Published October 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1994. Last previous edition approved in 2012 as D5526 – 12. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5526-18. the ASTM website.
2 4
The boldface numbers in parentheses refer to the list of references at the end of The last approved version of this historical standard is referenced on
this standard. www.astm.org.

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D5526 − 18
E355 Practice for Gas Chromatography Terms and Relation- the environmental hazards posed by the breakdown of plastics
ships to varying degrees in landfills. This test method has been
2.2 APHA-AWWA-WPCF Standards:5 designed to assess biodegradation under optimum and less-
2540D Total Suspended Solids Dried at 103°–105°C than-optimum conditions.
2540E Fixed and Volatile Solids Ignited at 550°C
5.3 Limitations—Because a wide variation exists in the
212 Nitrogen Ammonia
construction and operation of landfills, and because regulatory
3. Terminology requirements for landfills vary greatly, this procedure is not
intended to simulate the environment of all landfills. However,
3.1 Definitions—For definitions of terms used in this test it is expected to closely resemble the environment of a
method see Terminology D883. biologically active landfill. More specifically, the procedure is
3.2 Definitions of Terms Specific to This Standard: intended to create a standard laboratory environment that
3.2.1 methanogenic inoculum—anaerobically digested or- permits rapid and reproducible determination of the anaerobic
ganic waste containing a high concentration of anaerobic biodegradability under accelerated landfill conditions, while at
methane-producing microorganisms. the same time producing reproducible mixtures of fully and
partially decomposed household waste with plastic materials
4. Summary of Test Method for ecotoxicological assessment.
4.1 This test method described consists of the following: (1)
selecting and analyzing material for testing; (2) obtaining a 6. Apparatus
pretreated municipal-solid-waste fraction and a concentrated 6.1 Pressure-Resistant Glass Vessels—Twenty-seven, each
anaerobic inoculum from an anaerobic digester; (3) exposing with a volume of 4 to 6 L, which can be closed airtight and
the material to an anaerobic static batch fermentation at more capable of withstanding an overpressure of two atmospheres.
than 30 % solids; (4) measuring total carbon in the gas (CO2 The lids of the reactors are equipped with an overpressure
and CH4) evolved as a function of time; (5) removing the valve (to prevent the overpressure from becoming higher than
specimens for cleaning (optional), conditioning, testing, and 2 bars), a manometer that provides a rough indication of the
reporting; (6) assessing the degree of biodegradability; and (7) overpressure, a septum that allows one to take gas samples and
assessing the degree of biodegradability under less than opti- measure the exact overpressure, and, finally, a valve to release
mum conditions. the overpressure (Fig. 1).
4.2 The percentage of biodegradability is obtained by de-
termining the percent of conversion of carbon from the test 6.2 Incubators, sufficient to store the vessels in the dark at
material to carbon in the gaseous phase (CH4 and CO2). This 35 6 2°C for the duration of the test.
percentage of biodegradability will not include the amount of 6.3 Pressure Transducer, connected to a syringe needle to
carbon from the test substance that is converted to cell biomass measure the headspace pressure in the test vessel.
and that is not, in turn, metabolized to CO2 and CH4.
6.4 Gas Chromatograph, or other apparatus, equipped with
5. Significance and Use a suitable detector and column(s) for measuring methane and
carbon dioxide concentrations in the evolved gases.
5.1 Decomposition of a plastic within a landfill involves
biological processes that will affect the decomposition of other 6.5 pH Meter, precision balance (60.1 g), analytical balance
materials enclosed by, or in close proximity to, the plastic. (60.1 mg), thermometer, and barometer.
Rapid degradation of the plastic has the ability to increase the
6.6 Suitable Devices, for determining volatile fatty acids by
economic feasibility of landfill-gas recovery, minimize the
aqueous-injection chromatography, total Kjeldahl nitrogen,
duration of after-care of the landfill, and make possible the
ammonia nitrogen, dry solids (105°C), and volatile solids
recovery of the volume reduction of the waste due to biodeg-
(550°C) concentrations.
radation during the active life of the landfill. This procedure
has been developed to permit determination of the anaerobic
7. Reagents and Materials
biodegradability of plastic products when placed in biologi-
cally active environments simulating landfill conditions. 7.1 Pretreated-Household Waste, derived from mixed mu-
5.2 As degradation occurs inevitably in a landfill, it is of nicipal solid waste or the organic fraction thereof, after
immediate concern that the plastic materials do not produce homogenizing, screening over a screen with holes of a diam-
toxic metabolites or end products under the various conditions eter of 40 to 80 mm, and aerobically stabilized over a period of
that have the potential to occur in a landfill. The mixtures 2 to 4 weeks by blowing air into the material and maintaining
remaining after completion of the test method, containing fully a dry-matter content of 50 6 5 % and a temperature of 55 6
or partially degraded plastic materials or extracts, can be 10°C. (Optional: the pretreated household waste can be re-
submitted subsequently to ecotoxicity testing in order to assess placed by a similarly pretreated simulated solid waste.)
7.2 Anaerobic Inoculum, derived from a properly operating
5
Standard Methods for the Examination of Water and Wastewater, 20 ed., th anaerobic digester with pretreated household waste as a sole
1999, available from American Public Health Association, 800 I Street, NW, substrate or a digester that treats predominantly household
Washington, D.C. 20001-3710, or http://www.standardmethods.org. waste.

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8.4 The methane produced during the procedure is explo-
sive and flammable. Upon release of the biogas from the
gas-collection system, take care in venting the biogas to the
outside or to a hood.
9. Inoculum
9.1 The inoculum can be derived either from a laboratory-
scale or full-scale continuous digester or batch digester, oper-
ating at 35°C and functioning with an organic fraction of
household waste as the predominant substrate. In case the
inoculum is derived from a continuous laboratory-scale or
full-scale digester, the digester must be operating for a period
of at least one month on the organic fraction of household
waste, with a maximum retention time of 30 days under
mesophilic conditions (35 6 2°C). Gas production yields must
be at least 15 mL at standard temperature and pressure of
biogas/gram of dry solids in the digester and per day for at least
7 days. In case the inoculum is derived from a batch digester,
the gas production rate must have exceeded 1 L/kg waste/day,
and the methane concentration of the biogas being produced
must be above 60 %.
9.2 The prepared inoculum needs to undergo a short meso-
philic post-fermentation of approximately 7 days at the same
dry-matter content as the digester from which it was derived.
This means that the inoculum is not fed but is allowed to
1 = Digester.
post-ferment anaerobically by itself. This is to ensure that
2 = Incubation chamber. large, easily biodegradable particles are degraded during this
3 = Overpressure valve. period and also to reduce the background level of degradation
4 = Manometer.
5 = Septum.
of the inoculum itself.
6 = Valve. 9.3 The biochemical characteristics of the inoculum shall be
FIG. 1 Setup of Accelerated Landfill as follows:
9.3.1 pH—Between 7.5 and 8.5 (in accordance with Test
Methods D1293);
9.3.2 Volatile Fatty Acids (VFA)—Below 1 g/kg wet weight
7.3 Cellulose, Analytical-Grade, for thin-layer chromatog-
(in accordance with Practice D2908); and
raphy as a positive control.6
9.3.3 NH+ 4- N—Between 0.5 and 2 g/kg (in accordance
7.4 Polyethylene (optional), as a negative control. It needs with APHA Test 212 and Test Method D3590).
to be in the same form as that in which the sample is tested:
9.4 Analyses are performed after dilution of the inoculum
film polyethylene for film samples, pellets of polyethylene in
with distilled water on a ratio of distilled water to inoculum of
case the sample is in the form of pellets, etc.
5 to 1 on a weight-over-weight basis.
8. Hazards 10. Test Specimen
8.1 This procedure involves the use of inoculum and mu- 10.1 The test specimen needs to be of sufficient carbon
nicipal solid waste containing biologically and possibly chemi- content, analyzed in accordance with Test Method D4129, to
cally active materials known to produce a variety of diseases. yield carbon dioxide and methane volumes that can be mea-
Avoid contact with these materials by wearing gloves and other sured accurately by the trapping devices described. Add more
appropriate protective equipment. Use good personal hygiene test specimen when low biodegradability is expected, up to 100
to minimize exposure. g of dry matter of the test specimen.
8.2 It is possible that the solid waste mixture will contain 10.2 It is acceptable for the test specimen to be in the form
sharp objects. Take extreme care when handling this mixture to of films, powder, pellets, or formed articles, or in the form of
avoid injury. a dog bone and in accordance with Practice D618.
8.3 This test method includes the use of hazardous chemi- 11. Procedure
cals. Avoid contact with the chemicals and follow the manu-
facturer’s instructions and material safety data sheets. 11.1 Preparation of the Mixtures:
11.1.1 Determine the volatile solids, dry solids, and nitrogen
content of the pretreated household waste and the inoculum in
6
Avicel®, available from EM Chemicals, Inc., Hawthorne, NY, was used for accordance with Test Methods D1888, D3590, and APHA
development of this test method. 2540D and 2540E.

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D5526 − 18
11.1.2 Determine the volatile solids, dry solids, and carbon 11.4.3 Remove sufficient residual material from the vessel
content of all test substances in accordance with APHA 2540D and submit to ecotoxicity testing, in accordance with appropri-
and 2540E and Test Method D4129. ate standard test methods and practices (optional).
11.1.3 Weigh and combine the components and adjust the
dry matter content of the final mixtures with water to reach the 12. Calculation
desired dry-matter content for each vessel. Roughly weigh out
12.1 By using the total carbon in the test specimen, calculate
600 g on a dry-weight basis of pretreated household waste, and
the maximum theoretical gas production (carbon dioxide plus
mix it with 100 g on a dry-weight basis of mesophilic
methane) originating from the anaerobic biodegradation of the
anaerobic inoculum from a continuously operating digester or
test specimen, based on the following biochemical transforma-
150 g on a dry-weight basis of anaerobic inoculum from a
tions:
batch digester. Add 60 to 100 g of dry matter of the test
substance. Add water until the appropriate final dry matter C12H 2 →CH4 (1)
content is reached. (In order to reach 60 % dry matter content
C1O 2 →CO2
in the mixture, it is necessary, in some cases, to have water
removed prior to combining the different components of the Each millimole (12 mg) of organic carbon from the test
mixture. This can be accomplished by drying the pretreated sample can be converted into 1 mmole of gaseous CH4 or CO2,
household waste or centrifuging the anaerobic inoculum.) Mix or both. One millimole of gas produced occupies 22.4 mL at
the required amounts of pretreated household waste, inoculum, standard temperature and pressure (STP).
and test substance in a small container for 2 to 3 min. Introduce
12.2 Temperature and Pressure—Measure the percentages
the mixture in the vessel, weigh the vessel with all of the
of CH4 and CO2, and transform the gas volumes to STP. Also
contents, and close it airtight. Prepare the pressure vessels in
correct for vapor pressure and atmospheric pressure variation
the triplicate at each of the following dry matter contents: 35,
during the test. Calculate the amount of gaseous carbon.
45, and 60 %, so nine vessels are necessary for each sample.
Determine the mean (of the three replicates) net gaseous
11.1.4 The blanks consist of 600 g dry matter of pretreated
carbon production by anaerobic biodegradation of the test
household waste and anaerobic inoculum at the respective total
substances by subtracting the mean gaseous carbon production
dry-matter contents. As references, thin-layer chromatography
of the control (three replicates) containing only the inoculum.
cellulose must be used as a positive control. The blank and
reference are performed in triplicate at the three different 12.3 Calculate the percent of biodegradation for each dry-
dry-matter contents. matter concentration by dividing the average net gaseous-
11.2 Start-Up Procedure—After all reactors are filled and carbon production of the test material by the original average
closed, place them in incubators at 35 6 2°C. Acclimate the amount of total carbon of the test compound and multiplying
reactors for approximately 1 h and release the pressure, which by 100.
originates from the temperature increase, to the atmosphere. mean C g ~ test! 2 mean C g ~ blank!
% biodegradation 5 3 100 (2)
Incubate the reactors in the dark for a period of four months. Ci
11.3 Operating Procedure: where:
11.3.1 Check the gas production (measured as a pressure Cg = amount of gaseous carbon produced, g, and
increase) at least weekly. When the overpressure reaches more Ci = amount of carbon in test compound added, g.
than 700 mbar, measure the pressure exactly with the pressure
Calculate the standard error, se, of the percentage of biodeg-
transducer and release to atmospheric pressure. Take care that
radation as follows:
the temperature decrease, due to the opening of the incubator
2
or incubation room, is not more than 1°C during measurement s e 5 SQRT ~~ s test /n1 ! 1 ~ s 2blank /n2 !! 3 100/C i (3)
of the overpressure. where:
11.3.2 Analyze the gas composition biweekly. Determine
n1 andn2 = number of replicate test and blank digesters,
the methane and carbon dioxide concentration by using ana-
respectively, and
lytical devices suitable for the detection and quantification of
s = standard deviation of the total gaseous carbon
these gases, such as a gas chromatograph with an appropriate
produced.
detector, conforming to Practices E260 and E355. Pay special
attention to the occurrence of leaks through the septum. Calculate the 95 % confidence limits as follows:
11.4 End of the Test: 95 % CL 5 % biodegradation6 ~ t 3 s e ! (4)
11.4.1 It is acceptable for the incubation time to be where:
extended, depending on the activity of the inoculum, until no
t = t-distribution value for 95 % probability with
significant gas production in excess of the blank has been
(n1 + n2 − 2) degrees of freedom; thus n = 3 + 3 − 2 = 4.
recorded during one week or until the positive reference has
degraded for more than 70 %.
11.4.2 At the end of the test, analyze the dry matter, volatile 13. Interpretation of Results
fatty acids, and pH for each of the reactor mixtures, in 13.1 Information on the toxicity of the plastic material is
accordance with APHA 2540E, Practice D2908, and Test potentially useful for interpreting inhibitory effects on the
Methods D1293. inoculum.

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D5526 − 18
13.2 This test method includes the use of thin-layer chro- 14.1.10 Temperature range of the test.
matography cellulose as a positive control. If sufficient biodeg- 14.1.11 Wet-weight loss (optional).
radation (a minimum of 70 % for cellulose) is not observed
within the duration of the test, the test must be regarded as 15. Precision and Bias
invalid and needs to be repeated with fresh inoculum. 15.1 The precision and bias of the procedure presented in
this test method for measuring the anaerobic biodegradation of
14. Report plastic materials under accelerated landfill conditions is being
14.1 Report the following data and information: determined.
14.1.1 Information on the inoculum, including source, pH, 15.2 Preliminary results at 40 % dry-matter content and
volatile fatty acids (in milligram per kilogram wet weight), 35°C are presented in Fig. 2. The curves in Fig. 2 represent the
NH4+ -N (in gram per kilogram wet weight), percent dry solids,
percent volatile solids, date of collection and use, storage time
and conditions, handling, and potential acclimation to the test
material.
14.1.2 Information on the pretreated household waste used
to produce the inoculum and used as a substance. In case a
simulated solid waste is used, report the composition of the
mix. For both pretreated household waste and simulated solid
waste, report the source, pH, type of pretreatment, NH4+ -N (in
gram per kilogram), percent dry solids, percent volatile solids,
date of collection, storage time and conditions, handling, and
transportation.
14.1.3 Carbon content of the plastic material and the posi-
tive control and maximum theoretical gas production (carbon
dioxide and methane) for each.
14.1.4 Record and display graphically the cumulative gas
evolution over time.
14.1.5 Analysis of gas as percent methane and percent
carbon dioxide for each reading at the end of the test, or each
time the gas is released to the atmosphere during the course of
the test. Concomitantly, report the barometric pressure and FIG. 2 Cumulative Biogas Production Over a Period of 300 Days
temperature in the incubator and in the gas-collection device. for 1 kg of Pretreated Household Waste Plus 100 g of Mesophilic
Anaerobic Inoculum Without Sample (Blank) and With 60 g of
14.1.6 Record the percent of carbon conversion, along with Cellulose (Plus Positive Control)
the form of plastic material, that is, sheet, powder, pellets, etc.
Record specific information on the size, shape, volume, and
thickness of the plastic materials and control substances tested. biogas production in litres from 1 kg of pretreated household
14.1.7 Percent of biodegradation relative to cellulose. waste plus 10 % mesophilic inoculum without sample (blank)
14.1.8 Standard deviation and 95 % confidence interval for and with 60 g of cellulose (plus positive control).
the percentage of biodegradation for each triplicate set.
14.1.9 In case biogas production has not reached a plateau 16. Keywords
for the vessels at 45 and 60 % dry matter, report total biogas 16.1 accelerated landfill; anaerobic biodegradation; biodeg-
production as percentage of total biogas production at 35 % dry radation; dry digestion; ecotoxicity; landfill; metabolites; plas-
matter. tics; test method

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D5526 − 18
REFERENCES

(1) Campbell, D. J. V., and Croft, B.,“Landfill Gas Enhancement: Management and Technology, Vol 18, No. 1, 1990, p. 40.
Brogborough Test Cell Programme,” Landfill Gas: Energy and (4) European Patent No. 84200801.3, 06.06.1984.
Environment 90, United Kingdom Department of Energy, 1990, p. (5) U.S. Patent No. 4 684 468, 03.31.1986.
281. (6) Westlake, K., “Landfill Microbiology,” Landfill Gas: Energy and
(2) De Baere, L. A., et al., “High-Rate Dry Anaerobic Composting Environment 90, United Kingdom Department of Energy, 1990, p.
Process for the Organic Fraction of Solid Wastes,” Biotechnology and 271.
Bioengineering Symposium No. 15, John Wiley & Sons, Inc., New (7) Suflita, J. M., et al., “The World’s Largest Landfill: A Multidisci-
York, NY, 1986, p. 321. plinary Investigation,” Environmental Science and Technology, Vol
(3) De Wilde, B., et al., “Dry Anaerobic Conversion of Source Separated 26, No. 8, 1992, p. 1486.
Household Waste to Biogas and Humotex,” Journal of Resource

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5575 − 18

Standard Classification System for


Copolymers of Vinylidene Fluoride (VDF) with Other
Fluorinated Monomers1
This standard is issued under the fixed designation D5575; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 1.5 The minimum specification properties are established by


this classification system. Additional specification properties,
1.1 This classification system covers both developing prop-
based on the designation properties cited, can be established by
erty designations and specifications for thermoplastic compo-
the resin supplier and customer.
sitions consisting of vinylidene fluoride (VDF) polymers
modified with other fluoromonomers and property-enhancing 1.6 The values stated in SI units are to be regarded as
additives. The other fluoromonomers include one or more of standard.
the following: hexafluoropropylene (HFP), tetrafluoroethylene 1.7 The property tests are intended to provide information
(TFE), and chlorotrifluoroethylene (CTFE). The additives are for specifications of modified VDF-copolymer compositions. It
those that improve its flame resistance, processing, or physical is not the purpose of this classification system to provide
properties. However, these additives are not normally consid- engineering data for design purposes.
ered to be reinforcing. This classification system covers ther-
NOTE 1—Although the values listed in Table 1, Table 2, Table 3, Table
moplastic compositions supplied in pellet or powder forms. 4, and Table 5 are necessary to include the range of properties available in
1.2 A designation or specification applies only to the virgin existing materials, they are not to be interpreted as implying that every
possible combination of the properties exists or can be obtained. It is
polymers prepared from vinylidene fluoride (>50 weight %) possible for a user or designer, using Tables 1-5, to call out property
with one or more of the following comonomers: relationships that are physically impossible to occur in a copolymer made
hexafluoropropylene, tetrafluoroethylene, and chlorotrifluoro- using current technology.
ethylene. Some polymers contain additives to enhance certain NOTE 2—Many of these polymers exhibit polymorphism.3 The type and
properties. extent of crystalline structure will vary with the thermomechanical history
of the sample. Properties vary based on the technique used to prepare the
1.3 This system constitutes a line callout as a means of specimens.
designating and specifying properties of VDF-based copoly- 1.8 Test methods used in this classification system can result
mers. At least four of the designated properties are used to in the incidental production of hazardous materials. Modified
define a polymer’s specification. Specification criteria from VDF polymer fluoroplastics melt between 90 and 182°C (194
international documents can be used if their criteria match and 359°F) and are thermally stable up to about 350°C (662°F),
designation properties currently used by this classification or somewhat higher, depending on the composition.
system.2 This classification system is not intended for the (Warning—Evolution of corrosive, colorless, and toxic hydro-
selection of materials. gen fluoride can occur under certain conditions.)
1.4 The manufacturer of the virgin resin shall establish the 1.9 This standard does not purport to address all of the
designation of a resin based on the property value criteria in safety concerns, if any, associated with its use. It is the
this classification system. responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1
See Warning in 1.8 and Section 10 for specific hazards
This classification system is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic statements.
Materials. NOTE 3—Many, but not all of the codes and specifications found in this
Current edition approved Aug. 1, 2018. Published August 2018. Originally
classification system are also in ISO 12086-1 and ISO 12086-2.
approved in 1994. Last previous edition approved in 2013 as D5575 - 07(2013).
DOI: 10.1520/D5575-18. 1.10 This international standard was developed in accor-
This standard is needed to cover commercial products outside the scope of dance with internationally recognized principles on standard-
Specification D3222.
2
Fluoropolymer property specification data from international standards can
ization established in the Decision on Principles for the
include properties intentionally excluded from this classification system (for
3
example, composition). The only property criteria from other documents that can be Lovinger, A. J., “Poly(vinylidene fluoride),” Developments in Crystalline
used are those having similar properties allowed under the designation system. Polymers, Vol 1, Chapter 5, D.C. Bassett, Ed., Applied Science, London, 1982.

*A Summary of Changes section appears at the end of this standard


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D5575 − 18
TABLE 1 Codes for the Information on Fluoropolymers Used in rable method is listed after each citation in parentheses.
Data Block 1 D150 Test Methods for AC Loss Characteristics and Permit-
Code Meaning tivity (Dielectric Constant) of Solid Electrical Insulation
A modified D257 Test Methods for DC Resistance or Conductance of
B block copolymer
H homopolymer Insulating Materials
K copolymer D618 Practice for Conditioning Plastics for Testing
L graft polymer D638 Test Method for Tensile Properties of Plastics
R random copolymer
Z other D792 Test Methods for Density and Specific Gravity (Rela-
tive Density) of Plastics by Displacement
D883 Terminology Relating to Plastics
TABLE 2 Code-Letters Used in Data Block 2 (Intended D1238 Test Method for Melt Flow Rates of Thermoplastics
Application or Method of Processing, Essential Properties, by Extrusion Plastometer
Additives, or Other Information D1600 Terminology for Abbreviated Terms Relating to Plas-
Code Position 1 Code Positions 2 to 8 tics
A adhesives C colored
B blow molding D powder D2863 Test Method for Measuring the Minimum Oxygen
B1 extrusion blow molding D2 free-flowing Concentration to Support Candle-Like Combustion of
B2 injection blow molding D3 not free-flowing Plastics (Oxygen Index)
C calendaring E expandable
E extrusion F special burning characteristics D3222 Specification for Unmodified Poly(Vinylidene Fluo-
G general use F1 nonflammable ride) (PVDF) Molding Extrusion and Coating Materials
H coating F2 flame retarded D3418 Test Method for Transition Temperatures and En-
H1 powder coating F4 reduced smoke emission
H2 dip coating G granules thalpies of Fusion and Crystallization of Polymers by
K cable and wire coating G1 pellets Differential Scanning Calorimetry
L monofilament extrusion L light and weather stabilized D3835 Test Method for Determination of Properties of
M molding (injection/transfer) M nucleated
Q compression molding N natural (no color added) Polymeric Materials by Means of a Capillary Rheometer
R rotational molding N1 suitable for food contact D3892 Practice for Packaging/Packing of Plastics
V thermoforming N2 high purity D4591 Test Method for Determining Temperatures and
X no indication P impact modified
Y textile yarns, spinning R mold release agent Heats of Transitions of Fluoropolymers by Differential
Z other S lubricated Scanning Calorimetry
T transparent D4703 Practice for Compression Molding Thermoplastic
T1 translucent
T2 opaque Materials into Test Specimens, Plaques, or Sheets
W1 improved chemical resistance D5740 Guide for Writing Material Standards in the Classi-
Y increased electrical conductivity
fication Format
Z antistatic
IEEE/ASTM S1–10 Standard for Use of the International
System of Units (SI)
TABLE 3 Designatory and Specification Properties for Data Block 2.2 IEC and ISO Standards:5
3
IEC 60093 Recommended Methods of Test for Volume and
Position NumberA Property Surface Resistivities of Electrical Insulating Materials
B
1 melt temperature
2 B
melt flow rate/melt viscosity IEC 60250 Recommended Methods for the Determination of
3 B
tensile strength and modulus the Permittivity and Dielectric Dissipation Factor of
4 tensile elongation
5 B
density
Electrical Insulating Materials at Power, Audio and Radio
6 electrical Frequencies Including Metre Wavelengths
7 flammability by oxygen index (OI) ISO 291 Plastics—Standard Atmospheres for Conditioning
8 specimen preparation method and type
and Testing (Practice D618)
A
Property test information for Positions 1 to 7 are given in Section 8. ISO 293 Plastics—Compression Molding Test Specimens of
B
Positions 1, 2, 3, and 5 are mandated as the minimum specification properties.
Thermoplastic Materials (Practice 4703)
ISO 472 Plastics—Vocabulary (Terminology D883)
Development of International Standards, Guides and Recom- ISO 527/1,2,3 Plastics—Determination of Tensile Properties
mendations issued by the World Trade Organization Technical (Test Method D638)
Barriers to Trade (TBT) Committee. ISO 1043/1 Plastics—Symbols—Part 1: Symbols for Basic
Polymers and Their Special Characteristics (Terminology
2. Referenced Documents D883)
2.1 ASTM Standards:4 ISO 1043/2 Plastics—Symbols—Part 2: Fillers and Rein-
forcing Materials (Terminology D883)
NOTE 4—For ASTM and ISO documents, the equivalent or a compa- ISO 1133 Plastics—Determination of the Melt Mass-Flow
Rate (MFR) and the Melt Volume-Flow Rate (MVR) of
4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.

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TABLE 4 Date Block 3
Position 1 Position 2 Position 3 Position 4
Melt Viscosity/Melt-Flow Rate Tensile Strength Tensile Elongation
Melt Temp-
Code Tm,° C Melt-Flow Yield
Load, Vis- era- Modulus,
Code Rate, Code Strength, Code Yield, % Break, %
kg cosity, ture, MPa
g/10 min MPa
Pa/sA °C
a <20 a <0.1 <250 a <15 <500 a <5 <50
b 20 to <30 b 0.1 to< 0.2 0.325 >250 b 15 to <20 500 to< 800 b 5 to <10 50 to <100
c 30 to <40 c 0.2 to <0.5 1.20 >500 c 20 to <25 800 to< 1200 c 10 to <15 100 to <150
d 40 to< 50 d 0.5 to <1.0 2.16 >100 d 25 to< 30 1200 to <1600 d 15 to <20 150 to <200
e 50 to <60 e 1.0 to <2.0 3.80 >1500 e 30 to< 35 1600 to <2000 e 20 to <25 200 to <250
f 60 to <70 f 2.0 to <5.0 5.00 >2000 230 f 35 to< 40 2000 to< 3000 f 25 to <30 250 to <300
g 70 to <80 g 5.0 to <10 10.00 >2500 125 g 40 to< 45 3000 to< 4000 g >30 300 to <350
h 80 to< 90 h 10 to < 20 12.50 >3000 h 45 to< 50 4000 to <6000 h 350 to <400
i 90 to < 100 i 20 to <50 21.60 >3500 i 50 to< 55 >6000 i 400 to <500
j 100 to< 110 j $50 31.60 j 55 to< 60 j 500 to <600
k 110 to< 120 k k 60 to <65 k 600 to< 800
l 120 to< 130 l l $65 l >800
m 130 to <140 m m m
n 140 to <150 n n n
o 150 to <160 o o o
p 160 to <170 p p p
q 170 to <180 q q q
r 180 to <190 r r r
s 190 to <200 s s s
t 200 to <210 t t t
u u u u
v v v v
w w w w
x x x x
y y y y
z not specified z not specified z not specified z not specified
A
1 Pa/s = 10 P.

Position 5 Position 6 Position 7 Position 8


Specific Gravity, Electrical a-c d-c Electric Vol- Limiting Oxygen
Code Code Loss Code Code Specimen Type
g/cm3 Dielectric Constant ume Index
a <1.6 a >10E3 a <40 a D638 Type I
b 1.6 to <1.7 b 10E3 to 10E12 b 40 to <50 b D638 Type II
c 1.7 to< 1.8 c >10E12 c 50 to <60 c D638 Type III
d 1.8 to <1.9 d d 60 to< 70 d D638 Type IV
e 1.9 to< 2.0 e e 70 to <80 e ISO 527 Type 1A
f 2.0 to <2.1 f f 80 to <90 f ISO 527 Type 1B
g 2.1 to< 2.2 g <0.0012 g >90 g ISO 527 Type 6A
h 2.2 to< 2.3 h <3.0 <0.0014 h h ISO 527 Type 7A
i 2.3 to <2.4 i 3.0 to< 3.1 <0.0016 i i ISO 12086/1 Fig. 1
j 2.4 to <2.5 j 3.1 to <3.2 <0.0018 j j D638 Type MI
k k 3.2 to< 3.5 <0.0020 k k D638 Type MII
l l 3.5 to <4.0 <0.0022 l l D638 Type MIII
m m 4.0 to< 4.5 <0.0024 m m
n n 4.5 to <5.0 <0.0026 n n
o o 5.0 to< 5.5 <0.0028 o o
p p 5.5 to <6.0 <0.0030 p p D1708
q q 6.0 to <6.5 <0.0035 q q
r r 6.5 to <7.0 <0.0040 r r
s s 7.0 to <8.0 <0.0060 s s
t t 8.0 to <9.0 <0.0080 t t
u u 9.0 to <10 <0.0100 u u
v v 10 to <11 <0.0300 v v
w w 11 to <12 <0.1000 w w
x x 12 to <14 >0.1000 x x
y y >14 y y
z not specified z not specified not specified z not specified z

Thermoplastics (Test Method D1238) ISO 12086-1 Fluoropolymer Dispersion and Molding and
ISO 1183 Plastics—Methods for Determining Density and Extrusion Materials—Part 1: Designation and Specifica-
Relative Density of Non-Cellular Plastics (Test Methods tion
D792) ISO 12086-2 Fluoropolymer Dispersion and Molding and
ISO 4589 Plastics—Determination of Flammability By Oxy- Extrusion Materials—Part 2: Preparation of Test Speci-
gen Index mens and Determination of Properties

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TABLE 5 Codes for Filler and Physical Form of Materials for Use 3.3.4 HFP—hexafluoropropylene (1,1,2,3,3,3-hexaflu-
in Data Block 4 oropropylene).
Code Material Code Form/Structure
B boron B beads, spheres, balls
3.3.5 MFR—melt-flow rate.
C carbon C chips, cuttings 3.3.6 MV—melt viscosity.
CG graphite D powder
E clay F fiber 3.3.7 PVDF—poly(vinylidene fluoride).
G glass G ground
K calcium carbonate H whisker 3.3.8 TFE—tetrafluoroethylene (1,1,2,2-tetrafluoro-
M mineral, metal K knitted fabric ethylene). D1600
Ma aluminum oxide L layer
Mb bronze M mat (thick) 3.3.9 VDF—vinylidene fluoride (1,1,-difluoroethylene).
MC calcium fluoride N nonwoven (fabric) 3.3.10 VDF/CTFE—vinylidene fluoride/
Md molybdenum disulfide P paper
Me stainless steel S roving chlorotrifluoroethylene copolymer.
P mica T scale, flake 3.3.11 VDF/HFP—vinylidene fluoride/hexafluoropro-
Q silica V cord
R aramid W veneer penecopolymer.
S synthetic, organic X not specified
T talcum Y yarn
3.3.12 VDF/TFE—vinylidene fluoride/tetrafluoroethylene
X not specified Z others copolymer.
Z none
3.3.13 VDF/TFE/HFP—vinylidene fluoride/
tetrafluoroethylene/hexafluoropropene copolymer.

3. Terminology 4. Classification and Designation


3.1 Definitions: 4.1 The classification and designation system of the poly-
3.1.1 copolymer—a polymer derived from more than one mers is based on the following standardized pattern taken from
species of monomer. ISO 12086-1:
3.1.2 fluoroplastic—a plastic based on polymers made with Designation and Classification System
monomers containing one or more atoms of fluorine, or Description Block
copolymers of such monomers with other monomers, the | Identity Block |
| Individual Item Block |
fluoro-monomer(s) being in the greatest amount by mass. Data Data Data Data Data
ISO 12086-1 Block 1 Block 2 Block 3 Block 4 Block 5
3.1.3 monomer—a low-molecular-weight substance consist- 4.1.1 The designation system consists of the following:
ing of molecules capable of reacting with like or unlike 4.1.1.1 An optional description block, reading
molecules to form a polymer. “Thermoplastics,”
3.1.4 thermoplastic—a plastic that repeatedly can be soft- 4.1.1.2 An identity block comprising the ASTM standard
ened by heating and hardened by cooling through a tempera- number, and
ture range characteristic of the plastic, and that in the softened 4.1.1.3 An individual item block.
state can be shaped by flow into articles by molding or (1) The individual item block is subdivided into five data
extrusion. blocks that include the information in 4.2 – 4.6. Data Block 5
is used when a designation is converted to a specification. See
3.2 Definitions of Terms Specific to This Standard:
Section 7 for more details.
3.2.1 amorphous—noncrystalline or devoid of regular struc-
(2) The blocks shall be separated from each other by
ture.
commas. If a data block is not used, this shall be indicated by
3.2.2 contamination—the presence of nonpolymer particu- doubling the separation sign, that is, by two commas (,,).
late and debris in the polymer, excluding any property-
enhancing additives. 4.2 Data Block 1—This data block identifies the fluoropo-
lymer by its abbreviation from the list in 3.3 (additional terms
3.2.3 fluoropolymer—synonymous with fluoroplastic. are listed in ISO 12086-1, 2, or Terminology D1600). The
3.2.4 melt-processible—capable of being processed by, for abbreviation is followed by a hyphen and a one-letter code
example, injection molding, screw extrusion, and other opera- giving more information about the polymer, using the codes
tions typically used with thermoplastics. from Table 1.
3.2.5 polymorphism—the ability of a material to form two 4.3 Data Block 2:
or more different but stable crystalline forms. 4.3.1 This block can indicate up to eight items of informa-
3.2.6 thermomechanical history—the mechanical and ther- tion coded by letters as specified in Table 2. Position 1 gives
mal exposure that a material experiences before testing. information about intended application or method of process-
ing. Positions 2 through 8 provide up to seven items that can
3.3 Abbreviations:
use codes from Table 2 to indicate the polymer’s form as well
3.3.1 CTFE—chlorotrifluoroethylene (1-chloro-1,2,2-
as specific special characteristics.
trifluoroethylene).
4.3.2 If only one letter is given (for example, E), it must
3.3.2 DMAC—dimethylacetamide. apply to Position 1. Whenever there is an indication of
3.3.3 DSC—differential scanning calorimetry. properties, etc., in Positions 2 to 8, a code in Position 1 is

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required. The code “X” indicates that no other letter code is and percentage elongation at yield and break. Order for
appropriate. An alphabetical order is recommended if more Positions 3 and 4 are as follows:
than one code letter is used in Positions 2 to 8. Position 3 Order Position 4 Order

NOTE 5—Selecting the application or processing method for Position 1 1st = tensile yield 1st = tensile-yield elongation
of Data Block 2 must be done carefully. Many polymers are capable of 2nd = tensile break 2nd = tensile-break elongation
more than one application or method of processing (for example, 3rd = tensile modulus
extrusion (E) and molding (M) resins must be coded “general use” (G)).
Coding for special methods of processing must be reserved for polymers 4.4.5 Density (Relative Density, Specific Gravity) (Position
only designed for the application. 5)—Density shall be determined in accordance with the prin-
ciples of Test Methods D150 or ISO 12086-2. The cell codes
4.4 Data Block 3:
are listed in Table 4.
4.4.1 Data Block 3 is used as the designation or general
description of the fluoropolymer’s properties. The property 4.4.6 Electrical Properties (Position 6)—Electrical proper-
values are presented by code letters in seven of eight positions ties for d-c and a-c currents shall be determined by Test
within Data Block 3. Each position represents a specific Methods D150, D257, or their ISO equivalents. The cell codes
property listed in Table 3. Table 4 lists the code letters are listed in Table 4. Order for Position 6 is as follows:
corresponding to the various property values. The values are Position 6 Order
determined by the methods cited in Section 8. At least four of Position 1 = resistivity
the seven properties are specification properties. Position 8 Position 2 = frequency (listed as the exponent of the power of ten)
cites specimen preparation methods when the designation is Position 3 = dielectric constant
Position 4 = dissipation factor
converted to a specification. Positions 5 to 7, 8 to 10, 11 to 13, ... (repeat of 2 to 4 for each frequency cited)
4.4.1.1 Each position shall contain one or more code letters,
depending on the property cited. The positions are separated by 4.4.7 Flammability Properties (Position 7)—Flammability
a hyphen (-). Use of an asterisk (*) or question mark (?) before properties shall be determined by oxygen index (OI) values
the code letters denotes that property as a specification prop- using Test Method D2863 or ISO 4583. The cell codes are
erty. listed in Table 4.
4.4.1.2 The resin manufacturer shall assign the codes in 4.4.8 Specimen Preparation and Type (Position 8)—This
Data Block 3, based on test results from Table 4. If test values position is used only when a designation is converted to a
lie on, or on either side of, a cell limit because of manufactur- specification to describe the molded specimen type and its
ing tolerances, the resin manufacturer shall state which cell preparation. Section 9 provides information on preparing
will designate. compression-molded specimens. Cell codes are listed in Table
2 and Table 4. Order for Position 8 is as follows:
NOTE 6—Properties other than those in this classification system or do
Position 8 Order
not have standard test methods are outside of the property focus of the
document scope (for example, comonomer ratios). 1st = molding method (from Table 2, Position 1)
2nd = tensile bar type and method (Table 4)
4.4.2 Melting Endotherm Peak Temperature (Position 1)—
Melting endotherm peak temperature shall be determined in NOTE 7—Using specimen preparation method and type cited in Position
accordance with the principles of Test Methods D3418 and 8 allows the supplier and customer to monitor polymer properties while
D4591. Semicrystalline polymers shall use melting endotherm minimizing the effects of specimen preparation.
peak temperature as a designatory property. Cell codes and 4.5 Data Block 4—Data Block 4 is used to site the type
ranges are given in Table 4. (Position 1) and form (Position 2) of fillers or other materials
4.4.3 Melt-Flow Rate or Melt Viscosity (Position 2)—Melt added to the fluoropolymer. Letter codes listed in Table 5 are
viscosity (MV) shall be determined using Test Method D3835. used to indicate the type and form used (supplemental codes
Melt-flow rate (MFR) shall be determined in accordance with can be found in ISO 1043/2). The nominal content, by weight
Test Method D1238 or ISO 1133, using test conditions selected percent, is noted by arabic numerals after Position 2 to the
from Table 4. The melt viscosity or the melt-flow rate is nearest 1 %. Additive contents below 2 % need not be speci-
indicated in Data Block 3 by the cell code and ranges in fied. For designation clarity, a hyphen (-) is used to separate
accordance with Table 4, followed by the codes for tempera- material type codes. When a material is present in more than
ture and load for MFR and shear rate for MV also included in one form, a plus sign ( + ) is used to separate the form codes.
Table 4. Order for Position 2 is as follows:
4.6 Data Block 5:
Position 2 Order
4.6.1 Data Block 5 is used to denote changes in the values
1st = MFR of a property when the designation is converted to specifica-
2nd = MFR load
3rd = MV
tion. The type of changes would be the following:
4th = Temperature 4.6.1.1 To cite the alternate property value range when a (?)
4.4.4 Tensile Strength Properties (Positions 3 and 4)— is used in Data Block 3. Where more than one (?) is cited, the
Tensile-strength properties shall be determined in accordance value ranges shall be listed in order of their occurrence.
with the principles of Test Method D638 or ISO 527 modified NOTE 8—It is recommended that any ranges smaller than designated by
by details given in 8.9 or ISO 12086-2. Table 4 provides the Table 4 codes be greater than the precision and bias for the test method
codes to use for each range of tensile strength and modulus, that measures the property.

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4.6.1.2 To cite a current ASTM or other standard specifica- Data Block 3 Position Property
tion for the polymer (see 4.7 for restrictions).
1 melt temperature
4.6.1.3 A combination of 4.6.1.1 and 4.6.1.2. 2 melt-flow rate or melt viscosity, or both
3 tensile strength and modulus
4.7 Designation and Specification Restrictions: 5 density
4.7.1 Data Block 5 of the specification call-out cannot cite 7.1.2 Specification Using Designation Ranges:
properties beyond the scope of this classification system. In 7.1.2.1 Example (see Appendix X2):
other words, specification criteria or properties from other A VDF/CTFE copolymer, a general-use grade, sold as granules, and
specifications that conflict with this classification system’s having the following (specification properties are in boldface type):
(1) A melting point of 165°C,
scope are not allowed. (2) An MV of 1500 Pa/s when tested at 230°C at 100 s−1,
(3) A tensile strength yield of 28 MPa; break strength not cited;
NOTE 9—Some specifications cite properties that are either not detect- modulus of 800 MPa,
able or use test methods not available to most customers. Therefore, (4) Elongation yield of 9 %; break of 450 %,
specification property values or results shall be able to be determined by (5) Density between 1.78,
a user without a priori knowledge of the polymer’s manufacturer, (6) Electricals of:
polymerization process, or any other unique finishing process. Volume resistivity greater than 2.3 E14Ω,
Dielectric constant at 1 kHz at 10.1; at 10 kHz at 9.3; 1 MHz at 7.3,
4.7.2 A commercial grade of polymer shall not have mul- Dissipation factor at 1 kHz at 0.021; at 10 kHz at 0.031; at 1 MHz at
tiple designations for Data Block 2. The application choice 0.15,
(7) OI at 53, and
shall be broad enough for a variety of the applications to which (8) Tested using compression-molded specimens using ISO 527 Type-6A
it can be applied. tensile bars.
Designation and specification where each designatory property is desired
4.7.3 An alternate specification property range in Data as part of the specification with the specification limits equal to the cell limits
Block 5 shall not be greater than the original designation-code is as follows:
range from Table 4 and either the preceding or following code. ASTM D5XXX, VDF/CTFE-K, GG,*P-*ZZE-*DZC-BI-*C-
C3VU4UVSXY-C-*QG,Z,, ASTM D5XXX, VDF/CTFE-K,
In other words, if a property code is normally “D,” the new GG,*P-*ZZE-*DZC-BI-*C-C3VU4UVSXY-C-*QG, Z,,
range could encompass values or ranges from Code “C and D”
7.1.3 Specification Using Alternate Property Ranges:
or “D and E.” The new values cannot encompass a range cited
7.1.3.1 When the values given in the cell tables are not
by Codes “C to E” or greater.
satisfactory for specification purposes, indicate this situation
4.7.4 At no time shall a designation for a commercial grade by inserting a question mark in Data Block 3 at the beginning
have more than one designation for Data Blocks 1, 2, 3, and 4. of the destination cell code and the specification range given in
If the code values need to be modified from those cited in Table Data Block 5.
4, the changes shall be done by use of a (?) and listed in Data 7.1.3.2 Example (see Appendix X3):
Block 5.
A modified VDF/HFP copolymer that is processed by extrusion, with
reduced-burning characteristics and smoke emissions. The resin is marketed
5. General Requirements as pellets, contains a lubricant, and is opaque. The additive level is less than
2 %. Its properties are as follows (specification properties are in boldface
5.1 The material shall be ordered by the manufacturer’s type):
(1) A melting point of 143°C,
trade name and corresponding copolymer line callout and the
(2) An MV between 1300 and 1700 Pa/s when tested at 230°C at 100
necessary suffix properties to define the material. −1
s ,
(3) A tensile strength yield of 24 MPa; break not cited; modulus of
5.2 The material shall be of uniform composition and free of 1000 MPa,
foreign matter to a contamination level agreed upon between (4) Elongation yield of 12 %; break of 350 %,
(5) Density of 1.79,
the purchaser and the seller. (6) Electricals not cited.
(7) OI greater than 80,
5.3 Adequate statistical sampling shall be considered an (8) Tensile specimens are compression-molded and Test Method
acceptable alternative. D638, Type I, and
(9) The melt-viscosity range encompasses two ranges.
Designation and specification is as follows:
6. Example of a Designation
ASTM D5XXX, VDF/HFP-A, EFF4G1ST2, *N-*ZZ?E-*CZC-CH-
6.1 The following example is for VDF/HFP fluoropolymer *C-ZZ-*C-QA, Z, ?1300–1700,
material for general-purpose molding with a designation of:
8. Property Determination Methods
7. Specifications for Fluoropolymers 8.1 The following subsections of Section 8 cite test methods
used to determine polymer-property values of code levels from
7.1 Designation Conversion to Specification: Table 4 for Data Block 3 of a designation or specification line
7.1.1 A designation is converted into a specification by call-out. When a test value normally varies between two code
preceding 4 or more property codes in Data Block 3 with an levels, the manufacturer shall designate the code levels. Sev-
asterisk and adding the specimen preparation codes in Data eral properties are tested using molded specimens. Section 9
Block 3, Position 8, from Table 2 and Table 4. presents a procedure to prepare compression-molded speci-
7.1.1.1 Four property codes, cited by Data Block 3 mens. Injection molded specimens are allowed, but due to
positions, that must be included in a specification are as stress effects on many properties, compression molding of
follows: specimens is preferred.

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8.2 Melt Temperature—The copolymers peak melting points Tensile modulus shall use a strain rate of 2 % of the previous
are determined using Test Methods D4591 or D3418 using strain rate (0.5 mm/mm/min or 0.013 in./in./min). The property
DSC. The sample size is 10 6 1 mg. The sample is heated, values of the resin shall be determined as the average of results
cooled, and reheated over a temperature range from − 20 to from at least five specimens.
220°C at a rate of 10°C/min. The sample is held at the upper
temperature for 5 min before cooling. The second heating NOTE 10—When test equipment cannot test at a 2 % strain rate for the
smaller test bars, a higher strain rate (less than 5 %) is allowed.
endotherm peak value shall be used. Occasionally multiple
peaks are observed. The temperature of the tallest peak shall be 8.4.2 Elongation is determined as the percent change in
reported as the melting point. specimen length during the test, based on the original gauge
8.3 Melt-Flow Rate and Melt Viscosity: length. This value can be determined by either cross-head
8.3.1 Melt-Flow Rate—The melt-flow rate (MFR) shall be separation or by use of an extensometer.
determined using Test Method D1238 or ISO 1133 at 230°C for 8.4.3 Compression molded specimens are preferred (see
all resins whose melt point is above 100°C. Lower melt-point Section 9), but injection-molded specimens or specimens cut
resins shall use a test temperature of 125°C. from extruded sheet are allowed. Dies or mold cavity-
8.3.2 Melt Viscosity—The melt-viscosity value at 100 s−1 at dimensions to cut or mold specimens shall match the required
230°C shall be determined from a shear-rate viscosity curve of specimen dimensions and tolerances.
four or more points ranging from less than 50 s−1 to greater
NOTE 11—The different test bar shapes have three basic types with
than 500 s−1 shear rate. For polymers with melt points less than minor variations. Unfortunately, these differences can affect the test
110°C, a test temperature of 125°C shall be used. The values. For this reason Position 8 in Data Block 3 is used when a
rheometer die shall have an entrance angle of 60° (cone angle designation is changed to a specification. Examples of the three basic
of 120°) and a capillary L/D ratio of 15. The sample shall be shapes are as follows:
pellets or pieces cut from molded or extruded forms. Strips Large: D638 Type I or ISO 527 Type 1A (50-mm gauge)
about 6 mm wide by 76 mm long are easily handled. Medium: ISO 527 Type 6A or Test Method D638 Type IV (25-mm gauge)
Small: ISO 12086-2 Figure 1 (22-mm gauge)
8.4 Tensile Properties:
8.4.1 Tensile properties, except modulus, shall be tested in NOTE 12—Due to the molded-in stress and orientation, injection-
molded or samples cut from extruded sheet are subject to breaking outside
accordance with Test Method D638 or ISO 527 at a strain rate of the gauge region and show low (and possibly variable) elongation
of 25 mm/mm/min (1 in./in./min). The strain rate is the ratio of compared to compression-molded specimens. Some samples exhibit strain
the cross-head speed divided by the specimen-gauge length. hardening. This effect can result in variable break properties.

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8.5 Specific Gravity—The specific gravity shall be deter- tests. Die-cutting is the preferred method of preparing specimens. The
mined by Test Methods D792 using two test specimens cut cutting edges shall be sharp and free from any nicks or other defects that
could cause a dimensional defect in the specimen.
from a compression-molded sample. With this test, care must
be exercised to eliminate all air bubbles attached to the 10. Handling
specimens upon immersion. Dipping the specimens in a very
dilute solution (less than 0.1 weight %) of a surfactant will 10.1 As with any synthetic resin, it is advisable to wear a
minimize the problem. dust mask when handling large quantities of powder grades to
prevent ingestion.
8.6 Electrical Properties:
8.6.1 Specimen Type: 10.2 The Material Safety Data Sheets of the fluoropolymer
8.6.1.1 The electrical tests are determined on three grade must be reviewed to determine if there is any special-
specimens, each 100 mm in diameter and 0.12 to 0.25 mm handling information.
(0.005 to 0.010 in.) in accordance with IEC 250, Test Methods
11. Inspection and Certification
D150, and Test Method D257.
8.6.2 Volume Resistivity—The d-c volume resistivity shall 11.1 Inspection and certification of the material supplied
be measured using Test Method D257 or IEC 93. Cell codes under this classification system or specification shall be for
and ranges are listed in Table 4. conformance to the requirements specified herein.
8.6.3 Dielectric Constant and Dissipation Factor—The a-c 11.2 Lot-acceptance inspection shall be the basis on which
dielectric constant and dissipation factor shall be determined acceptance or rejection of the lot is made. The lot-acceptance
by Test Methods D150. The testing shall be done at the inspection shall consist of melt-flow rate, melt viscosity, tensile
following frequencies: 1 kHz, 10 kHz, 0.1 MHz, and 1 MHz. and elongation at break.
Codes for dielectric constant and dissipation factor are listed in 11.2.1 Those tests that ensure process control during manu-
Table 4. The code used for each frequency shall be the first facture as well as those necessary to ensure certifiability in
integer of the base 10 log of the frequency (for example, 1 accordance with 11.5.
kHz = 3; 1 MHz = 6). 11.2.2 The four minimum lot-acceptance tests are melt
8.7 Limiting Oxygen Index (LOI)—Limiting oxygen index is temperature, melt flow rate/melt viscosity, tensile strength and
determined by Test Method D2863. For formulations that modulus, and density as listed in Table 3.
extinguish before the 3-min burn time that defines the LOI 11.3 A lot is defined as one production run or a uniform
value at oxygen levels above 95 %. In this case, the LOI value blend of two or more production runs.
is the highest oxygen level used.
11.4 Periodic check inspection shall consist of the tests
NOTE 13—If a column with a restricted opening is used, the top of the specified for all requirements of the material under this
specimen shall be positioned at least 40 mm below the opening. classification system. Inspection frequency shall be adequate to
9. Preparation of Compression-Molded Specimens ensure that the material is certifiable in accordance with 11.5.
9.1 Molding Conditions: 11.5 Certification shall be that the material was manufac-
9.1.1 Compression-molded sheets can be prepared by Prac- tured by a process in statistical control, tested, and inspected in
tice D4703 using a “picture frame” mold. The resin form can accordance with this classification system and that average
be pellets, molded preforms, or powder. Due to the variety of values meet the requirements at a confidence level of 95 %.
grade types possible, follow manufacturer’s recommendations 11.6 A report of the test results shall be furnished when
for processing the material. Where possible, cooling shall be requested. The report shall consist of the results of the
done under pressure either by slow cooling (Method A or B) or lot-acceptance inspection for the shipment and the results of
quench cooling (Method C). It is recommended that an inert the most recent periodic-check inspection.
mold-release sheet (less than 0.007 in.) of aluminum,
polyimide, or PTFE be used. 12. Packaging, Packing, and Marking
9.1.2 The ram forces are used based on the size of the 12.1 Unless otherwise agreed upon between the purchaser
specimen area. The force adjustment exerts an approximate and the seller, the packing, packaging, and marking provisions
pressure of 0.25 kN/cm2 (360 lb/in.2) of specimen area. of Practice D3892 shall apply to this classification system.
NOTE 14—Powder samples tend to entrap air and cause bubbles in the
specimen when compression molded. Such specimens are not suitable for 13. Precision and Bias
any test in this classification system. Use molded preforms or densified 13.1 The precision and bias statements of the ASTM test
powder to eliminate bubble formation.
methods referenced herein apply to the specific tests required
9.2 Specimen Preparation—Test specimens can be molded in this classification system.
directly by a shaped mold or cut from a molded sheet. The
dimensions of shaped molds can vary due to mold-shrinkage 14. Keywords
effects. Cutting specimens from a molded sheet is preferred. 14.1 fluoropolymers; line callout; plastics; poly(vinylidene
NOTE 15—The specimen edge will affect performance in mechanical fluoride) copolymers

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D5575 − 18
APPENDIXES

(Nonmandatory Information)

X1. FORM TO DEVELOP DESIGNATION AND SPECIFICATION CODE

Specification
Test/Parameter Actual Lot Data Data Block Data Table Code Used Other Comments
YN
Polymer abbreviation Y-mandated No. 1–2 Section 3.3
Polymer type Y-mandated No. 1-2 Table 1
Application/process and Y-mandated No. 2-1 Table 2-1
special characteristics
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Properties
Melt temperature °C Y-mandated No. 3-1 Table 4-1 * Test Method D4591
MFR g/10 min Y-mandated DB 3-2a Table 4.1 * Test Method D1238
Load kg [or use] DB 3-2b Table 4.2 * Test Method D1238
Melt viscosity Pa/s Y-mandated DB 3-2c Table 4.3 * Test Method D3835
Temperature °C Y-mandated DB 3-2d Table 4.4 *
Tensile strength:
Yield MPa Y-mandated DB 3-3a Table 4.3a * Test Method D638/ISO 527
Break MPa Y N (optional) DB 3-3a Table 4.3b Test Method D638/ISO 527
Modulus MPa Y-mandated DB 3-3b Table 4.3c * Test Method D638/ISO 527
Tensile elongation:
Yield MPa Y N (optional) DB 3-4a Table 4.4a Test Method D638/ISO 527
Break MPa Y N (optional) DB 3-4b Table 4.4 Test Method D638/ISO 527
Density g/cm3 Y-mandated DB 3-5 Table 4.5 * Test Method D1505
Electricals:
d-c volume resistivity Ω Y N (optional) DB 3-6 Table 4.6c Test Methods D257
Frequency No. 1 Hz Y N (optional) DB 3-6 exponent
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6 Test Methods D150/IEC 250
Frequency No. 2 Hz Y N (optional) DB 3-6 exponent
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6b Test Methods D150/IEC 250
Frequency No. 3 Hz Y N (optional) DB 3-6 exponent
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6b Test Methods D150/IEC 250
Frequency No. 4 Hz Y N (optional) DB 3-6 exponent
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6b Test Methods D150/IEC 250
Flammability (OI) Y N (optional) DB 3-7 Table 4.7 Test Method D2863/ISO 4583
Molding method Y as specified DB 3-8 Table 2-1
Specimen type (above 2 %) Y as specified DB 3-8 Table 4.8
Additives type Y N (optional) DB 4-1 Table 5.1
Form Y N (optional) DB 4-2 Table 5.2
Form Y N (optional) DB 4-2 Table 5.2
Alternate:
Property range No. 1 Y if used
Property range No. 2 Y if used
Method specification Y If used
Designation code: ASTM
D5 XXX

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D5575 − 18

X2. DEVELOPMENT OF DESIGNATION FOR 7.1.2.1

Specification
Test/Parameter Actual Lot Data Data Block Data Table Code Used Other Comments
YN
Polymer abbreviation VDF/CTFE Y-mandated No. 1-2 Section 3.3 VDF/CTFE
Polymer type copolymer Y-mandated No. 1-2 Table 1 K
Application/process and general Y-mandated No. 2-1 Table 2-1 Gn
special characteristics granules Y N (optional) No. 2-2 Table 2-2 G
natural Y N (optional) No. 2-2 Table 2-2 N
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Properties
Melt temperature 168 °C Y-mandated No. 3-1 Table 4-1 *P Test Method D4591
MFR ... g/10 min Y-mandated DB 3-2a Table 4.1 Z Test Method D1238
Load ... kg [or use] DB 3-2b Table 4.2 Z Test Method D1238
Melt Viscosity 1500 Pa/s Y-mandated DB 3-2c Table 4.3 *E Test Method D3835
Temperature 230 °C Y-mandated DB 3-2d Table 4.4 *F
Tensile strength:
Yield 28 MPa Y-mandated DB 3-3a Table 4.3a *D Test Method D638/ISO 527
Break ... MPa Y N (optional) DB 3-3a Table 4.3b Z Test Method D638/ISO 527
Modulus 800 MPa Y-mandated DB 3-3b Table 4.3c *C Test Method D638/ISO 527
Tensile elongation:
Yield 9 MPa Y N (optional) DB 3-4a Table 4.4a B Test Method D638/ISO 527
Break 450 MPa Y N (optional) DB 3-4b Table 4.4 I Test Method D638/ISO 527
Density 1.78 g/cm3 Y-mandated DB 3-5 Table 4.5 C Test Method D1505
Electricals:
d-c volume resistivity >2.4E14 Ω Y N (optional) DB 3-6 Table 4.6c C Test Methods D257
Frequency No. 1 1K Hz Y N (optional) DB 3-6 exponent 3
Dielectric constant 10.1 Y N (optional) DB 3-6 Table 4.6a V Test Methods D150/IEC 250
Loss 0.021 Y N (optional) DB 3-6 Table 4.6b U Test Methods D150/IEC 250
Frequency No. 2 10K Hz Y N (optional) DB 3-6 exponent 4
Dielectric constant 9.3 Y N (optional) DB 3-6 Table 4.6a U Test Methods D150/IEC 250
Loss 0.031 Y N (optional) DB 3-6 Table 4.6b V Test Methods D150/IEC 250
Frequency No. 3 1M Hz Y N (optional) DB 3-6 exponent 6
Dielectric constant 7.3 Y N (optional) DB 3-6 Table 4.6a S Test Methods D150/IEC 250
Loss 0.15 Y N (optional) DB 3-6 Table 4.6b U Test Methods D150/IEC 250
Frequency No. 4 Hz Y N (optional) DB 3-6 exponent
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6b Test Methods D150/IEC 250
Flammability (OI) 53 Y N (optional) DB 3-7 Table 4.7 C Test Method D2863/ISO 4583
Molding method compression Y as specified DB 3-8 name Q
Specimen type (above 2 %) 527—Type 6a Y as specified DB 3-8 Table 4. G
Additives type none Y N (optional) DB 4-1 Table 5.1 Z
Form Y N (optional) DB 4-2 Table 5.2
Form Y N (optional) DB 4-2 Table 5.2
Alternate:
Property range No. 1 Y if used
Property range No. 2 Y if used
Method specification Y if used
Designation code: ASTM D5XXX VDF/CTFE-K, GGN, *P-*ZZEF-*DZC-BI-*C-C3VU4VU6SU-C-QG, Z, ,

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D5575 − 18

X3. DEVELOPMENT OF DESIGNATION AND SPECIFICATION FOR 7.1.3.2

Specification
Test/Parameter Actual Lot Data Data Block Data Table Code Used Other Comments
YN
Polymer abbreviation VDF/HFP Y-mandated No. 1-2 Section 3.3 VDF/HFP
Polymer type modified Y-mandated No. 1-2 Table 1 A
Application/process and extrusion Y-mandated No. 2-1 Table 2-1 E
special characteristics specification Y N (optional) No. 2-2 Table 2-2 F
burn
low smoke Y N (optional) No. 2-2 Table 2-2 F4
pellets Y N (optional) No. 2-2 Table 2-2 G1
lubricated Y N (optional) No. 2-2 Table 2-2 S
opaque Y N (optional) No. 2-2 Table 2-2 T1
Y N (optional) No. 2-2 Table 2-2
Y N (optional) No. 2-2 Table 2-2
Properties
Melt temperature 143 °C Y-mandated No. 3-1 Table 4-1 *N Test Method D4591
MFR ... g/10 min Y-mandated DB 3-2a Table 4.1 Z Test Method D1238
Load ... kg [or use] DB 3-2b Table 4.2 Z Test Method D1238
Melt Viscosity 1300–1400 Pa/s Y-mandated DB 3-2c Table 4.3 *? Test Method D3835
Temperature 230 °C Y-mandated DB 3-2d Table 4.4 F
Tensile strength:
Yield 24 MPa Y-mandated DB 3-3a Table 4.3a *C Test Method D638/ISO 527
Break ... MPa Y N (optional) DB 3-3a Table 4.3b Z Test Method D638/ISO 527
Modulus 1000 MPa Y-mandated DB 3-3b Table 4.3c *C Test Method D638/ISO 527
Tensile elongation:
Yield 12 MPa Y N (optional) DB 3-4a Table 4.4a C Test Method D638/ISO 527
Break 350 MPa Y N (optional) DB 3-4b Table 4.4 H Test Method D638/ISO 527
Density 1.79 g/cm3 Y-mandated DB 3-5 Table 4.5 *C Test Method D1505
Electricals:
d-c volume resistivity none Ω Y N (optional) DB 3-6 Table 4.6c Z Test Methods D257
Frequency No. 1 none Hz Y N (optional) DB 3-6 exponent Z
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6b Test Methods D150/IEC 250
Frequency No. 2 Hz Y N (optional) DB 3-6 exponent
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6b Test Methods D150/IEC 250
Frequency No. 3 Hz Y N (optional) DB 3-6 exponent
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6b Test Methods D150/IEC 250
Frequency No. 4 Hz Y N (optional) DB 3-6 exponent
Dielectric constant Y N (optional) DB 3-6 Table 4.6a Test Methods D150/IEC 250
Loss Y N (optional) DB 3-6 Table 4.6b Test Methods D150/IEC 250
Flammability (OI) >80 Y N (optional) DB 3-7 Table 4.7 *F Test Method D2863/ISO 4583
Molding method compression Y as specified DB 3-8 Table 2-1 *Q
Specimen type (above 2 %) D638 TYPE I Y as specified DB 3-8 Table 4.8 A
Additives type ... Y N (optional) DB 4-1 Table 5.1 Z
Form Y N (optional) DB 4-2 Table 5.2
Form Y N (optional) DB 4-2 Table 5.2
Alternate:
Property range No. 1 1300–1700 Y if used ?1300–1700
Property range No. 2 Y if used
Method specification Y if used
Designation code: ASTM D5XXX VDF/HFP-A, EFF4G1ST2, *N-*ZZ?F-*CZC-CH-*C-ZZ-*F-*QA, Z, ?1300–1700

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D5575 − 18
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D5575 - 07(2013)) that may impact the use of this standard. (August 1, 2018)

(1) Revised 8.3.2 and 9.1.1.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5576 − 00 (Reapproved 2013)

Standard Practice for


Determination of Structural Features in Polyolefins and
Polyolefin Copolymers by Infrared Spectrophotometry (FT-
IR)1
This standard is issued under the fixed designation D5576; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* Content of Ethylene-Vinyl Acetate (EVA) Copolymers by


1.1 This practice covers infrared procedures for determining Fourier Transform Infrared Spectroscopy (FT-IR)
the molecular structural features in polyolefins and polyolefin D6248 Test Method for Vinyl and Trans Unsaturation in
copolymers. The structural features of primary concern are the Polyethylene by Infrared Spectrophotometry
types and numbers of branches. Although this practice centers E131 Terminology Relating to Molecular Spectroscopy
its attention on polyolefins and polyolefin copolymers, the E168 Practices for General Techniques of Infrared Quanti-
techniques, with proper modification, can be used for some tative Analysis
other polymers as well. E932 Practice for Describing and Measuring Performance of
NOTE 1—Quantitative determinations require either an internal or an Dispersive Infrared Spectrometers
external evaluation of sample thickness. ASTM test methods available for E1421 Practice for Describing and Measuring Performance
specific features are listed in Tables 1 and 2. of Fourier Transform Mid-Infrared (FT-MIR) Spectrom-
1.2 This standard does not purport to address all of the eters: Level Zero and Level One Tests
safety concerns, if any, associated with its use. It is the IEEE/ASTM SI-10 Standard for Use of the International
responsibility of the user of this standard to establish appro- System of Units (SI): The Modern System
priate safety and health practices and to determine the
3. Terminology
applicability of the regulatory limitations prior to use.
3.1 Definitions—For definitions of plastics terms used in
NOTE 2—There is no known ISO equivalent to this standard.
this practice see Terminology D883 and D1600.
2. Referenced Documents 3.2 Units, symbols and abbreviations used in this practice
2.1 ASTM Standards: 2 appear in Terminology E131 or IEEE/ASTM SI-10.
D883 Terminology Relating to Plastics 4. Summary of Practice
D1505 Test Method for Density of Plastics by the Density-
Gradient Technique 4.1 Infrared absorption bands suitable for quantitative
D1600 Terminology for Abbreviated Terms Relating to Plas- analysis by FT-IR are listed in Tables 1 and 2. These are only
tics typical bands and are not to be construed as exhaustive.
D2238 Test Methods for Absorbance of Polyethylene Due to 4.2 For quantitative determinations, sample specimen thick-
Methyl Groups at 1378 cm−1 ness is measured internally at some band representing the basic
D3124 Test Method for Vinylidene Unsaturation in Polyeth- chain structure, such as 2019 cm–1 for polyethylene, or
ylene by Infrared Spectrophotometry externally using a micrometer (see Tables 1 and 2 for ASTM
D3594 Test Method for Copolymerized Ethyl Acrylate In test methods).
Ethylene-Ethyl Acrylate Copolymers NOTE 3—Warning: Molding can cause carbonyl formation due to
D5594 Test Method for Determination of the Vinyl Acetate oxidation. This should be checked in the 1700 to 1750 cm–1 range.

5. Significance and Use


1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
5.1 The structural features expressed by these determina-
Current edition approved April 1, 2013. Published April 2013. Originally tions affect the ultimate polymeric properties and are useful in
approved in 1994. Last previous edition approved in 2006 as D5576 - 00(2006). showing correlations with many performance properties.
DOI: 10.1520/D5576-00R13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Apparatus
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 6.1 Infrared Spectrophotometer, either double beam or a
the ASTM website. Fourier transform (FT-IR).

*A Summary of Changes section appears at the end of this standard


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D5576 − 00 (2013)
TABLE 1 Polyolefin Structural Features Determined by FT-IR 9.1.1.1 Control the hot plate temperature at 100 6 10°C
Structure
Absorption Band,
ASTM Test Method
above the melting temperature of the polymer.
cm–1 9.1.1.2 Place a portion of the sample on a microscope slide
Methyl group 1378 D2238 on the hot plate.
(polyethylene)
Methyl group (eth-prop 1380 9.1.1.3 Cover the sample with another slide and press with
copol) a wooden pestle. Use firm circular motions to press a uniform
Pendant methyl 935 film.
Terminal vinyl 908 D6248
Trans-vinylene 965 D6248 9.1.1.4 To quench the pressed polymer film, dip the two
Vinylidene 888 D3124 slides carefully into a beaker of cold water. Remove the film
and blot dry.
9.1.2 Procedure B:
TABLE 2 Structural Features in Polyolefin Copolymer Determined 9.1.2.1 Preheat the press to about 50°C above the melting
by FT-IR
point of the polymer.
Structure Absorption Band, cm–1 ASTM Test Method
9.1.2.2 Place a brass shim on the sheet material chosen (see
Vinyl acetate 609 D5594 7.1) that, in turn, covers a metal plate.
1020 D5594
3270 D5594 9.1.2.3 Add polymer in sufficient quantity to completely fill
Styrene 770–700 the shim aperture during pressing.
1600–1500
Ethyl acrylate 1640–1730
9.1.2.4 Cover with another piece of sheet (see 7.1) and
862 D3594 another metal plate.
Ethylene acrylate 1280–1200 9.1.2.5 Insert the mold assembly between the press platens
1640–1625
and apply a slight pressure.
9.1.2.6 Allow the sample to preheat for about 30 s. Apply
6.1.1 Double-beam infrared spectrophotometer capable of a the full press pressure at a temperature approximately 50°C
4 cm-1 spectral resolution as defined in Practice E932. The above the melting point of the polymer for 1 min or until all
instrument should be capable of scale expansion along the exudation ceases.
wavelength axis. 9.1.2.7 Turn off the heat, turn on the cooling water, and
6.1.2 Fourier Transform Infrared Spectrometer, capable of 4 allow the sample to press quench at full pressure until the
cm–1 resolution. The instrument should be capable of scale temperature drops below 50°C (or cool enough to remove the
expansion along the wavelength axis. Also, see Practice E1421 mold assembly by hand).
for testing procedures. 9.1.2.8 Release the pressure and remove the sample.
9.1.2.9 Select plaques that are clear and of uniform thick-
6.2 Hot Plate. ness for the FT-IR analysis. To avoid interference fringes in the
6.3 Microscope Slides. spectrum, the plaque/film surfaces must be slightly dimpled.
6.4 Compression-Molding Press, capable of 200°C. 9.2 Spectral Measurements:
6.5 Metal Plates, two, 150 by 150 mm or larger, of 0.5–mm 9.2.1 Place the sample in the infrared spectrophotometer.
thickness with smooth surfaces. 9.2.2 Set the controls of the infrared spectrophotometer for
quantitative conditions with a good signal to noise ratio and
6.6 Brass Shims, approximately 75 by 75 mm, of 0.5-mm satisfactory repeatability. For a FT-IR, a spectral resolution of
thickness with an aperture in the center at least 25 by 38 mm. 4 cm–1 and an apodization function (Beer-Norton medium and
6.7 Micrometer (optional), with thimble graduations of Happ-Genzel have been found to be appropriate) that gives
0.001 mm. good quantitation should be used.
6.8 Film Mounts, with apertures at least 6 by 27 mm, to hold 9.2.3 Record the infrared spectrum from 4000 to 500 cm–1.
the specimens in the infrared spectrophotometer. 9.2.4 Determine which structural feature(s) are present and
select the appropriate ASTM method for quantitative determi-
7. Materials nation.
7.1 Polyethylene Terephthalate, Aluminum or Matte Fin-
ished Teflon-Fiberglass Sheets. 10. Calculation

8. Hazards 10.1 If no standard method is available and an estimate of


the concentration of the feature of interest is sought, the
8.1 Wear gloves when plaques are prepared using a heated approach in 10.1.1-10.1.3 is suggested.
press. 10.1.1 Determine the thickness of the plaque or, preferably,
8.2 The optical bench of the FT-IR spectrometer contains a its spectral cross-section, b, in cm2/g, by measuring the
laser. To avoid eye injury, do not look directly into the laser thickness and density or alternatively the mass and surface area
beam. of a uniformly thick portion of the plaque
10.1.2 Measure the absorbance of the peak of interest.
9. Procedure Choose a baseline between valleys on either side of the peak in
9.1 Sample Preparation: a manner to produce the most accurate and repeatable repre-
9.1.1 Procedure A: sentation of the actual background absorbance

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D5576 − 00 (2013)
10.1.3 Calculate the concentration, c, of the feature using 11.1.2 Date of test, and
either the Beer-Lambert Law (A = a · b · c) with the appropri- 11.1.3 Any sample or spectral anomalies observed during
ate molar absorptivity, a, or an appropriate calibration curve. If the measurement.
a calibration curve is used, it should have a minimum of 5 data
points, and the unknown should be within the high and low 12. Keywords
limits of the standards.
12.1 copolymers; FT-IR; infrared spectrophotometry; poly-
11. Report ethylene; structural features
11.1 Report the following information:
11.1.1 Complete identification of material tested including
name, manufacturer, lot number and physical form when
sampled,

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D5576 - 00(2006)) that may impact the use of this standard. (April 1, 2013)

(1) Reapproved without change.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/
COPYRIGHT/).

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5577 − 19

Standard Guide for


Techniques to Separate and Identify Contaminants in
Recycled Plastics1
This standard is issued under the fixed designation D5577; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 2. Referenced Documents


1.1 This guide is intended to provide information on avail- 2.1 ASTM Standards:2
able methods for the separation and classification of contami- D789 Test Method for Determination of Relative Viscosity
nants such as moisture, incompatible polymers, metals, of Concentrated Polyamide (PA) Solutions
adhesives, glass, paper, wood, chemicals, and original-product D792 Test Methods for Density and Specific Gravity (Rela-
residues in recycled plastic flakes or pellets. Although no tive Density) of Plastics by Displacement
specific methods for identification or characterization of foam D883 Terminology Relating to Plastics
products are included, foam products are not excluded from D1003 Test Method for Haze and Luminous Transmittance
this guide. The methods presented apply to post-consumer of Transparent Plastics
plastics. D1193 Specification for Reagent Water
1.2 For specific procedures existing as ASTM test methods, D1238 Test Method for Melt Flow Rates of Thermoplastics
this guide only lists the appropriate reference. Where no by Extrusion Plastometer
current ASTM standard exists, however, this guide gives D1457 Specification for Polytetrafluoroethylene (PTFE)
procedures for the separation or identification, or both, of Molding and Extrusion Materials (Withdrawn 1996)3
specific contaminants. Appendix X1 lists the tests and the D1505 Test Method for Density of Plastics by the Density-
specific contaminant addressed by each procedure. Gradient Technique
D1898 Practice for Sampling of Plastics (Withdrawn 1998)3
1.3 This guide does not include procedures to quantify the D1925 Test Method for Yellowness Index of Plastics (With-
contaminants unless this information is available in referenced drawn 1995)3
ASTM standards. D3418 Test Method for Transition Temperatures and En-
1.4 This standard does not purport to address all of the thalpies of Fusion and Crystallization of Polymers by
safety concerns, if any, associated with its use. It is the Differential Scanning Calorimetry
responsibility of the user of this standard to establish appro- D4019 Test Method for Moisture in Plastics by Coulometric
priate safety, health, and environmental practices and deter- Regeneration of Phosphorus Pentoxide (Withdrawn
mine the applicability of regulatory limitations prior to use. 2002)3
D5033 Guide for Development of ASTM Standards Relating
NOTE 1—There is no known ISO equivalent to this standard.
to Recycling and Use of Recycled Plastics (Withdrawn
1.5 This international standard was developed in accor- 2007)3
dance with internationally recognized principles on standard- D5227 Test Method for Measurement of Hexane Extractable
ization established in the Decision on Principles for the Content of Polyolefins
Development of International Standards, Guides and Recom- E169 Practices for General Techniques of Ultraviolet-Visible
mendations issued by the World Trade Organization Technical Quantitative Analysis
Barriers to Trade (TBT) Committee. E355 Practice for Gas Chromatography Terms and Relation-
ships

1 2
This guide is under the jurisdiction of ASTM Committee D20 on Plastics and For referenced ASTM standards, visit the ASTM website, www.astm.org, or
is the direct responsibility of Subcommittee D20.95 on Recycled Plastics. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved April 1, 2019. Published May 2019. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1994. Last previous edition approved in 2010 as D5577 - 94(2010)ɛ1, the ASTM website.
3
which was withdrawn January 2019 and reinstated in April 2019. DOI: 10.1520/ The last approved version of this historical standard is referenced on
D5577-19. www.astm.org.

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E682 Practice for Liquid Chromatography Terms and Rela- Techniques to separate and identify incompatible plastics,
tionships moisture, chemicals, or original product residues, and solid
E794 Test Method for Melting And Crystallization Tempera- contaminants such as metals, paper, glass, and wood are
tures By Thermal Analysis essential to the processing of recycled plastic materials.
E1252 Practice for General Techniques for Obtaining Infra- 5.2 This guide lists existing ASTM and ISO methods plus
red Spectra for Qualitative Analysis currently practiced industrial techniques for identification and
2.2 ISO Standards:4 classification of contaminants in recycled plastics flake or
ISO 3451/1-1981 Plastics—Determination of Ash; Part 1: pellets.
General Methods
ISO 1183-1987 Methods for Determining the Density and 6. Sampling
Relative Density of Noncellular Plastics
6.1 Unless otherwise stated, materials should be sampled in
3. Terminology accordance with the procedures described in Practice D1898.
3.1 This terminology used in this guide is in accordance Adequate statistical sampling should be considered as an
with Terminology D883 and Guide D5033. acceptable alternative.
3.2 Definitions of Terms Specific to This Standard: 7. Existing ASTM or ISO Procedures
3.2.1 chemicals—nonhazardous or hazardous materials (for
example, insecticides or herbicides) potentially used in contact 7.1 Moisture:
with plastic materials. 7.1.1 A coulometric method (Test Method D4019), the
standard test method for haze (Test Method D1003), Karl
3.2.2 glue—adhesives used for labels or joining bottle parts
Fisher titration (Test Method D789), or a gravimetric proce-
(for example, ethylene-vinyl acetate).
dure (13.6.1 of Specification D1457) can be used to estimate
3.2.3 heavy metals—metals heavier than sodium on the the moisture content of recycled plastic materials.
periodic table (for example, lead, arsenic, cadmium,
chromium, or copper). 7.2 Visual Inspection and Product Uniformity:
7.2.1 Color:
3.2.4 heavy plastic—unfilled polymers such as polystyrene, 7.2.1.1 Test Method D1925 measures the yellowness index
poly(ethylene terephthalate), and poly(vinyl chloride) and of clear acrylic plastics and the haze and the luminous
filled materials with densities greater than 1.00 g ⁄cm3. transmittance procedure (Test Method D1003) characterizes
3.2.5 light plastic—polymers such as polyethylene and the color of transparent unpigmented recycled plastic materi-
polypropylene with densities less than 1.00 g/cm3. als. These tests are not readily applied to pigmented plastic
3.2.6 original-product residues—residues from any samples.
original-product contents of a plastic package (for example, NOTE 2—Test Method D1925 is currently being revised by ASTM
milk, juice, or detergent). Subcommittee D20.40 to address reproducibility and bias problems.
3.2.7 particles—piece of metal, glass, wood, paper, or other 7.2.2 Melt Flow for Product Uniformity—Uniformity of
discreetly shaped material equal to or larger than 0.1 mm2. some recycled plastic flakes or pellets can be estimated by
3.2.8 specks—any material equal to or less than 0.1 mm2. measuring the flow rate of the material using an extrusion
plastometer (Test Method D1238).
4. Summary of Guide
7.3 Density or Specific Gravity—The displacement method
4.1 This guide provides details of several procedures used to for specific gravity or relative density (Test Method D792) or
separate and classify contaminants including, but not limited the density-gradient procedure for density (Test Method
to, moisture, original product residues, incompatible plastic, D1505) are useful techniques to determine contamination of
metal, paper, glass, adhesives, and wood in recycled plastic recycled plastic flakes or pellet samples with one or more other
flakes or pellets. This guide lists existing ASTM and ISO polymers.
methods that can be used to characterize solid and some liquid
contaminants. In addition, this guide presents details of some NOTE 3—Test Method D1505 uses relatively small test specimens, so it
may not be applicable for analysis of nonhomogeneous recycled plastic
industry procedures for identification of contaminants. Appen- materials.
dix X1 provides information on quantitative aspects of some of
these industry standards that can also be used to estimate the 7.4 Inorganic Contaminants:
concentration of various contaminants. 7.4.1 An ash test, such as ISO 3451/1, or the muffle-furnace
techniques currently being evaluated within ASTM Subcom-
5. Significance and Use mittee D20.70 (project designation X70-8702) can be used to
estimate the inorganic filler content of recycled plastic flake or
5.1 Recycled plastic materials may contain incompatible
pellets.
plastic or other undesirable contaminants that could affect the
processing or quality, or both, of the plastic prepared for reuse. NOTE 4—Some volatile metals may be lost using the test indicated in
7.4.1. ASTM Subcommittee D20.70 is currently developing a test method
(project X70-9201) for metals, including heavy metals, that will include
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., sample-preparation techniques to minimize the loss of volatile metals
4th Floor, New York, NY 10036, http://www.ansi.org. prior to analysis by X-ray fluorescence or spectroscopic techniques.

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7.4.2 Ferrous (iron) contaminants can be removed with a 8.2.2.2 Press a plaque from the recycled plastic sample.
magnet and aluminum contaminants are separated from plastic Remove the plaque from the press and cool.
materials using density procedures in accordance with 8.3. 8.2.2.3 Visually examine the test plaque within a 10-cm2
7.5 Thermal Analysis: area using a fluorescent-light table. For comparison, repeat
7.5.1 Since most polymers exhibit unique temperatures for 8.3.1 and 8.3.2 with a portion of virgin resin representing the
melting or other phase transitions, measurement of these bulk of the test material (for example, poly(ethylene terephtha-
transition temperatures (Test Method D3418) or the melting late) (PET) if you are interested in contaminants in recycled
and crystallization temperatures (Test Method E794) of a PET).
sample may provide useful information regarding the identity NOTE 6—The presence of glue contamination is indicated by bonding of
of polymeric components present in a recycled plastic material. the plastic to the polyester sheet used as a release material during molding
7.5.2 Both Test Methods D3418 and E794 involve thermal of the plaque.
NOTE 7—An alternative procedure for poly(ethylene terephthalate)
gravimetric analysis (TGA) or differential scanning calorim- involves melting pellets for 10 min at 275°C in an aluminum pan. This
etry (DSC). These techniques utilize small samples (5 to 15 melt is rapidly quenched in ice water to prevent crystallization and the
mg), so they may not be practical for use in characterization of resulting disk or plaque is visually inspected for contaminants and black
potentially nonhomogeneous recycled plastic materials. specks by comparison with a control disk or plaque prepared from virgin
PET. In this case, black specks are attributed to degraded paper, adhesives,
7.6 Infrared Analysis—Qualitative infrared analysis using poly(vinyl chloride), or other contaminants in the poly(ethylene terephtha-
the techniques of Practice E1252 can be used to identify late).
polymeric, chemical, and, in some cases, inorganic compo- 8.3 Separations Based on Density:
nents of recycled plastic materials. Sample size considerations 8.3.1 Water-Density Separation:
indicated in 7.5.2 may also apply to preparation of samples for 8.3.1.1 Fill a clean plastic container with 2 L of clean water.
infrared analysis. Add sufficient nonionic surfactant to make a 2 % (weight ⁄vol-
7.7 Chromatographic Analysis—The principles of gas ume) solution and mix thoroughly.
chromatography, described in Practice E355, and liquid NOTE 8—Acknowledging that water quality varies from one part of the
chromatography, described in Practice E682, are useful for country to another, minimum water quality for this test includes properties
separation and classification of chemical contaminants or of Type III grade reagent water as defined in Specification D1193.
residues from original-use contents of plastic packages. NOTE 9—Air pockets within flake material may cause the material to
fold back on itself. The surfactant (for example, Triton X-1005) helps
eliminate this problem with plastic flakes.
8. Additional Industrial Procedures
8.3.1.2 Obtain a representative sample of recycled plastic
8.1 Specimen Preparation:
flakes (see 6.1) and weigh 100 6 10 g into a clean, dry plastic
8.1.1 Using standard injection molding equipment, prepare
container.
homogenized sample plaques.
8.1.2 Plaques, or slices from plaques prepared in 8.1.1, can NOTE 10—The sample should be free of particles identified by a
be used for differential scanning calorimetry (DSC), infrared procedure such as that described in 8.1.
analysis, and other test procedures requiring small, homoge- 8.3.1.3 Add the surfactant solution from 8.3.1.1 to the
neous specimens. sample container and mix well with a spatula. Allow solids to
8.2 Visible Inspection Procedures: settle for at least 5 min.
8.2.1 Inspection Table for Large, Visible Contaminants: 8.3.1.4 Skim light plastic and any contaminants (for
8.2.1.1 Using a laboratory spatula, spread 450 6 20 g of example, paper) from the top of the water using a small kitchen
recycled plastic flakes or pellets on a clean, white inspection strainer. Transfer these materials to a larger strainer and rinse
table. with water to remove residual surfactant.
8.2.1.2 Without the benefit of magnification, describe the 8.3.1.5 Pour the remaining contents from the sample con-
types of individual contaminant “particles” as defined in 3.2.7, tainer (see 8.3.1.4) through another large strainer and wash
then using 10× magnification, describe the “specks” as defined these heavier materials with water to remove residual surfac-
in 3.2.8. tant.
8.2.1.3 Thermal techniques (see 7.5) and infrared analysis 8.3.1.6 If desired, these collected heavy materials are dried
(see 7.6) can be used to identify some of the isolated contami- and characterized by thermal (see 7.5) or infrared (see 7.6)
nants. techniques.
8.3.2 Propanol/Water Density Separation:
NOTE 5—To obtain a quantitative estimate of the contaminants, these 8.3.2.1 Add 1840 mL of 2-propanol and 1660 mL of water
contaminants can be removed and weighed, but there is not existing
(drinking, distilled, or deionized) to a 4-L plastic bottle. Mix
precision and bias data related to this estimated contaminant concentra-
tions in recycled plastics. well to provide a solution containing 52 % (volume:volume)
2-propanol in water.
8.2.2 Inspection of Molded Specimens or Plaques:
8.3.2.2 Pour 200 mL of the solution from 8.3.2.1 into a
8.2.2.1 Weigh 4 to 5 g of dry plastic flake on to a polyester
500-mL graduated cylinder and measure the specific gravity of
sheet or aluminum foil in a 15.2 by 15.2 by 0.013-cm mold.
Cover with another sheet of polyester film or aluminum foil,
then adjust the press temperature to at least 10°C above the 5
Available from Rohm & Haas Co., Independence Mall West, Philadelphia, PA
melting temperature of the bulk of the test material. 19105.

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this solution with a hydrometer. The specific gravity should be 8.5.2.3 Place the test solution in a 400-mL beaker on a hot
between 0.914 and 0.917. If not, add small amounts of plate and add approximately 100 g of the recycled plastic.
2-propanol or water to the solution from 8.3.2.1 to bring the 8.5.2.4 Boil the mixture for 5 min, then remove the beaker
specific gravity into the desired range. from the hot plate.
8.3.2.3 Weigh 100 6 10 g dry light plastic (see 8.3.1.4) into 8.5.2.5 Discard the liquid, rinse the plastic thoroughly with
a 4-L plastic pail, then add the 52 % 2-propanol ⁄water solution water, and transfer the washed plastic to a clear plastic bag.
(see 8.3.2.1) to this container. Stir contents with a rubber 8.5.2.6 Visually determine the presence of colored plastic
spatula to wet all flakes, then allow solids to settle. under fluorescent light. Poly(vinyl chloride) and poly(vi-
8.3.2.4 Skim any plastic from the top of this solution with a nylidene chloride) dye purple, while polyesters appear as blue
small kitchen strainer. Transfer the separated material to a regions, and polyamides appear yellow or orange.
larger strainer and rinse with water. 8.6 Stain 5 Test for Nylon and Polyesters:
8.3.2.5 Pour the remaining contents from 8.3.2.3 through a 8.6.1 Add 1 mL NaCl, 2 drops of a nonionic surfactant, 0.3
large strainer and collect the 2-propanol/water solution in a g of Stain #5, and 300 mL of water to a 500-mL beaker.8
clean, dry bottle. Save this solution for reuse in other separa- 8.6.2 Add approximately 100 g of recycled plastic to the
tions. Rinse the plastic in the strainer with water to remove beaker and place the beaker on a hot plate.
residual 2-propanol. 8.6.3 Boil the mixture for at least 2 min, then remove the
8.3.2.6 If desired, dry the plastic in the strainer, then beaker from the hot plate.
characterize the material using thermal (see 7.6) or infrared 8.6.4 Pour the beaker contents into a strainer and rinse with
(see 7.7) techniques. cold water.
8.4 Extrusion/Melt Flow Test: 8.6.5 Visually examine the washed plastic under fluorescent
8.4.1 To estimate the relative level of contamination, pro- light. Nylon (polyamide) samples will turn green or blue-green,
cess the recycled plastic through a laboratory extruder polyesters will turn yellow, and paper contamination will
equipped with a filter screen. appear as red material.
8.4.2 The level of contamination is measured as a function 8.7 Solvent Extraction Procedures:
of the rate of pressure increase resulting from increased 8.7.1 Xylene Extraction:
deposits on the filter screen. 8.7.1.1 Weigh 100 g of recycled plastic into an 800-mL
8.4.3 Contaminants isolated on the screen can be character- Erlenmeyer flask and add 200 mL of p-xylene.
ized by thermal (see 7.5) or infrared (see 7.6) techniques. 8.7.1.2 Seal the flask with a cork stopper fitted with a
8.5 Chlorinated Polymer Contamination: thermometer. Adjust the thermometer so that the bulb touches
8.5.1 Flame Test (Beilstein Test): the bottom of the flask.
8.5.1.1 Start the flame of a Bunsen burner, then pick up a 8.7.1.3 Maintain a temperature of 65 6 2°C and heat the
sample of the test plastic with tweezers. solvent and sample on a hot plate for 1 h. Shake the flask every
8.5.1.2 Place the bare end of a copper wire in the flame until 2 to 3 min to mix the contents.
it heats to a dull orange color, then quickly remove the wire 8.7.1.4 After 1 h, cool the sample to room temperature.
from the flame and touch it to the sample. 8.7.1.5 Transfer a portion of the p-xylene extract to a
8.5.1.3 Press the wire into the plastic sample and allow the suitable cell and obtain an infrared spectrum of the extract
sample to melt on to the wire. versus a p-xylene reference liquid in accordance with Practice
8.5.1.4 Remove the wire from the sample, place the wire E1252. Appearance of an absorption band at 5.7 µm indicates
with the sample back into the flame, and hold the wire in the the presence of an ethylene-vinyl acetate (EVA) copolymer.
flame until the plastic sample burns off the wire. Other bands in the infrared spectrum may be characterized in
8.5.1.5 The presence of a chlorinated polymer is indicated accordance with Practice E1252.
by a strong green flame during 8.5.1.4. 8.7.2 n-Hexane Extraction:
8.5.1.6 When all samples have been tested, turn off the gas 8.7.2.1 To adapt Test Method D5227 to the characterization
to the burner and store the burner. of contaminants in recycled plastic materials, add 1 L of
8.5.2 Stain K Test: n-hexane to the resin kettle in accordance with Test Method
8.5.2.1 Prepare a Stain K master batch by adding 1.00 g D5227 and clamp the kettle assembly into a water bath
Sevron Brilliant Red B, 1.00 g Irgalan Yellow DRL, and 2.00 maintained at 49.5 6 0.5°C.
g Terasil Brilliant Blue BGN dyes6 to 1 L water heated to 82 6 8.7.2.2 Add 2.5 to 5 g of the plastic sample, replace the
5°C. Stir until dyes are completely dissolved, then remove the kettle head with a condenser, and extract the sample for 2 h.
mixture from the heat, cool, and transfer to a suitable container. NOTE 11—This procedure developed for polyolefins, may be modified
8.5.2.2 Prepare a test solution by mixing 15 mL of Stain K for use with other polymers by using higher boiling solvents and
(see 8.5.2.1), 200 mL of water, 30 mL of 5 % Tanavol extraction at higher temperatures.
solution,7 and 2 mL 5 % (volume:volume) acetic acid in a 8.7.2.3 After extraction, filter the resin kettle contents
suitable container. through a fritted porcelain funnel.

6 8
Sevron Brilliant Red dye is available from Crompton & Knowles, Charlotte, Triton N-101, available from Ashland Chemical, 729 Mauney Dr., Columbia,
NC, and the other dyes are available from CIBA-Geigy Corp., Greensboro, NC. SC 29201, is a typical nonionic surfactant used for this test. The Stain #5 reagent is
7
Tanavol reagent is available from Tanatex Sybron Corp., Wellford, SC. available from J. Belmar Inc., N. Andover, MA.

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8.7.2.4 Analyze an aliquot of the filtered extract using 254 nm with the absorbance of a solvent blank. Significant
thermal techniques (see 7.5), infrared spectroscopy (see 7.6), or absorbance at 254 nm indicates the presence of a styrenic
a suitable alternative technique such as gas chromatography to polymer or another aromatic species (for example, poly(ethyl-
identify the extracted components. ene terephthalate) or poly(butylene terephthalate)).
8.8 Polystyrene as a Contaminant:
8.8.1 Weigh 10 g of the recycled plastic sample into an 9. Report
Erlenmeyer flask and shake 2 h with 100 mL of a solvent that 9.1 Report the following information:
is transparent at 254 nm (for example, dichloromethane or 9.1.1 The types of contaminants, and
tetrahydrofuran) based on spectroscopic techniques of Practice
E169. 9.1.2 The techniques used to arrive at the identifications
8.8.2 Dilute 2.5 mL of the extract to 50 mL with the same reported in 9.1.1.
solvent.
8.8.3 Filter 5 mL of this solution through a 0.45-m filter into 10. Keywords
a 1-cm quartz cell. 10.1 compression moldings; contaminants; density separa-
8.8.4 Obtain the ultraviolet spectrum of this filtered extract tions; extrusion; post-consumer plastics; recycled plastics;
in accordance with Practice E169. Compare the absorbance at visual inspection

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APPENDIX

(Nonmandatory Information)

X1. IDENTIFICATION OF CONTAMINANTS ADDRESSED BY SPECIFIC TEST PROCEDURES

TABLE X1.1 Identification of Contaminants Addressed by Specific Test Procedures


Test Procedure (Section Number) ASTM or ISO Method Components Detected
Ash test (7.4.1) ISO 3451/1 Inorganic fillers, some metals
Chlorinated polymers (8.5) Chlorinated materials
Chromatographic analysis (7.7) Practice E355; Practice E682 Chemicals, original-use contents
Color or yellowness index (7.2.1) Test Method D1925 Colored or degraded materials
Density or specific gravity (7.3) Test Methods D792; Test Method D1505 Contamination by other polymers
Density separations, water or propanol/water (8.3) Paper, other polymers, metals
Extrusion/melt flow test (8.4; 7.2.2) Test Method D1238 Incompatible polymers, metals, dirt, insoluble material
Flame or beilstein test (8.4.1) Chlorinated materials
Haze or transmittance (7.2.1) Test Method D1003 Moisture; incompatible polymers
Inspection table (8.2.1 Visible contaminants (specks, particles)
Infrared spectroscopy (7.6) Practice E1252 Contaminant functional groups
Magnets (7.4.2) Ferrous metals
Moisture (7.1) Test Methods D789; Test Method D1003; Test Water content
Method D4019
Molded specimens or plaques (8.2.2) Paper, adhesives, poly(vinyl chloride), incompatible
polymers
Polystyrene contaminant (8.8) Polystyrene; other aromatic polymers
Product uniformity (7.4)
Solvent extraction procedures, hexane or xylene (8.7) Glues, soluble contaminants
Specimen preparation (8.1)
Stain 5 test (8.6) Nylon, polyesters, paper
Stain K test (8.5.2) Chlorinated polymers
Thermal analysis (7.5) Test Method D3418; Test Method E794 Polymer identity
Ultraviolet spectroscopy (8.8) Aromatic polymers
Visible inspection procedures (7.2; 8.2) Dirt, specks, particles, materials with color different
from bulk polymer

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5592 − 94 (Reapproved 2018)

Standard Guide for


Material Properties Needed in Engineering Design Using
Plastics1
This standard is issued under the fixed designation D5592; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

INTRODUCTION

Plastics are increasingly being used in durable applications as structural components on a basis
comparable with traditional materials such as steels and aluminum, as well as high performance
composite systems. Unlike many consumer-goods applications, where plastics typically serve as
enclosures, these durables applications primarily involve load-bearing components exposed to rather
broad varying operating environments over the life cycle of the product. This necessitates access to
material property profiles over a wide range of conditions, rather than typical values reported at room
temperature. In order to design effectively with plastics, the designer must take into account the effects
of time, temperature, rate, and environment on the performance of plastics, and the consequences of
failure.

1. Scope 1.5 The values stated in SI units are to be regarded as


standard. No other units of measurement are included in this
1.1 This guide covers the essential material properties
standard.
needed for designing with plastics. Its purpose is to raise the
awareness of the plastics community regarding the specific 1.6 This standard does not purport to address all of the
considerations involved in using the appropriate material safety concerns, if any, associated with its use. It is the
properties in design calculations. responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1.2 This guide is intended only as a convenient resource for mine the applicability of regulatory limitations prior to use.
engineering design. It should be noted that the specific oper-
NOTE 1—There is no known ISO equivalent to this standard.
ating conditions (temperature, applied stress or strain,
environment, etc. and corresponding duration of such expo- 1.7 This international standard was developed in accor-
sures) could vary significantly from one application to another. dance with internationally recognized principles on standard-
It is, therefore, the responsibility of the user to perform any ization established in the Decision on Principles for the
pertinent tests under actual conditions of use to determine the Development of International Standards, Guides and Recom-
suitability of the material in the intended application. mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.3 The applicable ISO and ASTM standard methods for the
relevant material properties are listed in this guide for the 2. Referenced Documents
benefit of design engineers. 2.1 ASTM Standards:2
1.4 It should be noted that for some of the desired D543 Practices for Evaluating the Resistance of Plastics to
properties, no ASTM or ISO standards exist. These include Chemical Reagents
D638 Test Method for Tensile Properties of Plastics
pvT data, no-flow temperature, ejection temperature, and
D695 Test Method for Compressive Properties of Rigid
fatigue in tension. In these instances, relying on available test
Plastics
methods is suggested.
D883 Terminology Relating to Plastics
D1435 Practice for Outdoor Weathering of Plastics
1
This guide is under the jurisdiction of ASTM Committee D20 on Plastics and
2
is the direct responsibility of Subcommittee D20.10 on Mechanical Properties. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2018. Published April 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1994. Last previous edition approved in 2010 as D5592 - 94 (2010). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5592-94R18. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D1894 Test Method for Static and Kinetic Coefficients of ISO 4892-2 Plastics—Methods of Exposure to Laboratory
Friction of Plastic Film and Sheeting Light Sources—Part 2: Xenon Arc Sources
D1999 Guide for Selection of Specimens and Test Param- ISO 6721-2 Plastics—Determination of Dynamic Mechani-
eters from ISO/IEC Standards (Withdrawn 2000)3 cal Properties—Part 2: Torsion Pendulum
D2565 Practice for Xenon-Arc Exposure of Plastics In- ISO 8295 Plastics—Film and Sheeting—Determination of
tended for Outdoor Applications the Coefficients of Friction
D2990 Test Methods for Tensile, Compressive, and Flexural ISO 10350.1 Plastics—Acquisition and Presentation of
Creep and Creep-Rupture of Plastics Comparable Single-Point Data— Part 1: Moulding Mate-
D2991 Test Method for Stress-Relaxation of Plastics (With- rials
drawn 1990)3 ISO 11403-1 Plastics—Acquisition and Presentation of
D3045 Practice for Heat Aging of Plastics Without Load Comparable Multipoint Data—Part 1: Mechanical Prop-
D3123 Test Method for Spiral Flow of Low-Pressure Ther- erties
mosetting Molding Compounds ISO 11403-2 Plastics—Acquisition and Presentation of
D3418 Test Method for Transition Temperatures and En- Comparable Multipoint Data—Part 2: Thermal and Pro-
thalpies of Fusion and Crystallization of Polymers by cessing Properties
Differential Scanning Calorimetry ISO 11443 Plastics—Determination of the Fluidity of Plas-
D3641 Practice for Injection Molding Test Specimens of tics Using Capillary and Slit-Die Rheometers
Thermoplastic Molding and Extrusion Materials
D3835 Test Method for Determination of Properties of 3. Terminology
Polymeric Materials by Means of a Capillary Rheometer
D4473 Test Method for Plastics: Dynamic Mechanical Prop- 3.1 Definitions:
erties: Cure Behavior 3.1.1 aging—the effect on materials of exposure to an
D5045 Test Methods for Plane-Strain Fracture Toughness environment for an interval of time (see Terminology D883).
and Strain Energy Release Rate of Plastic Materials 3.1.2 coeffıcient of friction—a measure of the resistance to
D5279 Test Method for Plastics: Dynamic Mechanical Prop-
sliding of one surface in contact with another surface.
erties: In Torsion
E6 Terminology Relating to Methods of Mechanical Testing 3.1.3 coeffıcient of linear thermal expansion—the change in
E228 Test Method for Linear Thermal Expansion of Solid linear dimension per unit of original length of a material for a
Materials With a Push-Rod Dilatometer unit change in temperature.
E1823 Terminology Relating to Fatigue and Fracture Testing 3.1.4 compressive strength—the compressive stress that a
2.2 ISO Standards:4 material is capable of sustaining. In the case of a material that
ISO 175 Plastics—Determination of the Effects of Immer- does not fail in compression by a shattering fracture, the value
sion in Liquid Chemicals for compressive strength is an arbitrary value depending upon
ISO 294-1 Plastics—Injection Moulding of Test Specimens the degree of distortion that is regarded as indicating complete
of Thermoplastic Materials—General Principles, and failure of the material (modified from Terminology E6).
Moulding of Multipurpose and Bar Test Specimens
ISO 527-1 Plastics—Determination of Tensile Properties— 3.1.5 creep—the time-dependent increase in strain in re-
Part 1: General Principles sponse to applied stress (modified from Terminology E6).
ISO 527-2 Plastics—Determination of Tensile Properties— 3.1.6 creep modulus—the ratio of initial applied stress to
Part 2: Test Conditions for Moulding and Extrusion creep strain (see Test Method D2990).
Plastics
ISO 527-4 Plastics—Determination of Tensile Properties— 3.1.7 creep rupture stress—stress to produce material failure
Part 4: Test Conditions for Isotropic and Orthotropic Fibre corresponding to a fixed time to rupture (modified from Test
Reinforced Plastic Composites Method D2990).
ISO 604 Plastics—Determination of Compressive Properties 3.1.8 critical stress intensity factor—toughness parameter
ISO 899-1 Plastics—Determination of Creep Behaviour - indicative of the resistance of a material to fracture at fracture
Tensile Creep initiation (see Test Method D5045).
ISO 899-2 Plastics—Determination of Creep Behaviour -
Flexural Creep by Three-Point Loading 3.1.9 engineering stress—stress based on initial cross sec-
ISO 2578 Plastics—Determination of Time-Temperature tional area of the specimen.
Limits After Prolonged Exposure to Heat 3.1.10 fatigue—the process of progressive localized perma-
ISO 3167 Plastics—Multipurpose Test Specimens nent deleterious change or loss of properties occurring in a
ISO 4607 Plastics—Methods of Exposure to Natural Weath- material subjected to cyclic loading conditions (modified from
ering Definitions E1823).
3.1.11 Poisson’s ratio—the absolute value of the ratio of
3
The last approved version of this historical standard is referenced on transverse strain to the corresponding axial strain resulting
www.astm.org.
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., from uniformly distributed axial stress below the proportional
4th Floor, New York, NY 10036, http://www.ansi.org. limit of the material (see Terminology D883).

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3.1.12 proportional limit—the greatest stress that a material material suppliers because of the lack of standardized reporting
is capable of sustaining without any deviation from propor- format in the plastics industry. ISO 10350.1, ISO 11403-1, and
tionality of stress to strain (Hooke’s law) (see Test Method ISO 11403-2 are intended to address the comparability of data
D638). issue only as far as single-point and multipoint data for
3.1.13 PV limit—the limiting combination of pressure and material selection. This guide attempts to serve as a means to
velocity that will cause failure of any polymer rubbing against standardize the format to report comparable data for engineer-
another surface without lubrication at a specific ambient ing design. It is essential that incorporating standardized test
temperature and tested in a specific geometry. specimen geometry and specific test conditions as recom-
mended in Guide D1999, Practice D3641, or ISO 3167 and
3.1.14 secant modulus—the ratio of engineering stress to ISO 294-1 are an integral part of the data generation.
corresponding strain at a designated strain point on the
stress-strain curve (see Test Method D638). 5. Material Properties in Engineering Design
3.1.15 shear modulus—the quotient of the shearing stress 5.1 Finite element analysis is an integral part of computer
and the resulting angular deformation of the test specimen aided design/engineering (CAD/CAE). It serves as a powerful
measured in the range of small recoverable deformations (see tool for design engineers in performing engineering analysis of
ISO 6721-2). plastics components to predict the performance. The material
3.1.16 shear strength—the maximum shear stress that a data inputs required for carrying out these analyses essentially
material is capable of sustaining. Shear strength is calculated constitute the minimum data needed in engineering design.
from the maximum load during a shear or torsion test and is 5.2 The material properties essential in engineering design
based on the original dimensions of the cross section of the can be grouped into three main categories; (1) properties
specimen (see Terminology E6). essential for structural analysis, (2) properties essential for
3.1.17 tensile modulus—the ratio of engineering stress to assessing manufacturability, and (3) properties essential for
corresponding strain below the proportional limit of a material evaluating assembly. The properties essential for structural
in tension (modified from Test Method D638). analysis are employed in assessing the structural integrity of
3.1.18 tensile stress at break—the tensile stress sustained by the designed part over its useful life or in determining the
the material at break (modified from Test Method D638). required geometry of the part to ensure structural integrity. The
properties essential for assessing manufacturability are em-
3.1.19 tensile stress at yield—the tensile stress sustained by ployed in simulating the part filling/post filling steps to
the material at the yield point (modified from Test Method optimize processing conditions and for predictions of dimen-
D638). sional stability of the manufactured part. The properties essen-
3.1.20 warpage—distortion caused by non-uniform change tial for assembly considerations are employed in evaluating the
of internal stresses (D883). ability to join/assemble the component parts.
3.1.21 yield point—the first point on the stress-strain curve 5.3 As functional requirements are often specific to each
at which an increase in strain occurs without an increase in application, the material properties essential for structural
stress (see Test Method D638). analysis can be classified into two categories—those that are
somewhat application specific and those that are not.
4. Significance and Use
5.4 Whether the individual property is application-specific
4.1 This guide is intended to serve as a reference to the or not, certain properties are directly employed in design
plastics community for material properties needed in engineer- calculations while others are employed more or less for
ing design. verification of the design limits. For example, although parts
4.2 Product datasheets or product literature typically report may fail in service under multi-axial impact loading
single-point values at ambient conditions and hence, by their conditions, the impact energy data can be used only in design
very nature, are inadequate for engineering design and struc- verification, at best. Additional examples of properties that are
tural analysis of a component or system. A detailed property useful only for design verification include fatigue (S-N) curves,
profile for the particular grade chosen for a given part not only wear factor, PV limit, retention of properties following expo-
enhances the confidence of the design engineer by allowing a sure to chemicals and solvents, and accelerated aging or UV
more realistic assessment of the material under close-to-actual exposure/outdoor weathering.
service environments but also may avoid premature failure of 5.5 Almost all structural design calculations fall under one
the designed component and potential liability litigation later. of the following types of analysis or some combination thereof:
Additionally, it would also eliminate use of larger “design beam or plate; pipe; snap fits, pressfits, threads, bearing, bolts;
safety factors” that result in “overengineering” or “overde- or buckling. The properties needed for each of these design
sign.” Not only is such overdesign unwarranted, but it adds to calculations are summarized in Table 1.
the total part cost, resulting in a good example of ineffective 5.6 In plate and beam analyses, flexural modulus is often
design with plastics and a prime target for substitution by other used in determining the beam deflection or stiffness. However,
materials. development of apparent stress gradient across the beam or
4.3 One of the problems faced by design engineers is access plate thickness in flexure fails to satisfy the basic assumptions
to comparable data among similar products from different of uniformity of stress in most material models used in

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D5592 − 94 (2018)
TABLE 1 Material Properties Needed for Engineering Design Using Plastics
I. Structural Considerations
Plate or Beam Analysis (stiffness versus deflection) Pipe Analysis (stiffness versus hoop stresses)
Tensile modulus Tensile modulus
Poisson’s ratio Poisson’s ratio
Creep modulus Critical stress intensity factor, K1c
Tensile creep rupture stress Tensile creep rupture stress
Shear strength
Snap Fits Analysis (cantilever beam deflection) Press Fits Analysis (hoop stress)
Tensile modulus Tensile modulus
Poisson’s ratio Poisson’s ratio
Creep modulus Compression modulus
Secant modulus Compression strength
Shear modulus Coefficient of friction
Tensile strength at yield Tensile strength at yield
Coefficient of friction Creep modulus
Stress relaxationA
Threads Analysis (screw pullout forces, thread stripping torque) Bearing Analysis
Shear strength Coefficient of friction
Coefficient of friction Coefficient of thermal expansion
Tensile strength at break Wear factorB
Tensile modulus PV limitB
Compressive modulus Compressive yield strength
Bolts Analysis Buckling Analysis
Compressive strength Compressive modulus
Tensile creep strain Secant modulus
Tensile creep rupture stress Creep modulus
A
Stress relaxation Poisson’s ratio
Compressive creep modulus
II. Manufacturability Considerations
Mold Filling/Cooling Analysis Shrinkage and Warpage Analysis
Viscosity—shear rate data Mold shrinkage as function of thickness, gate geometry, and processing
Flowability (thermosets) parameters
Melt densityB Coefficient of linear thermal expansion
B
Thermal conductivity No-flow temperatureB
Specific heatB Glass transition temperature
Ejection temperatureB Crystallinity
No-flow temperature Crystallization temperature
Cure kinetics (thermosets) Heat of crystallization
pvT dataB Crystallization kineticsB
Elastic modulus
Poisson’s ratio
Shear modulus
III. Assembly Considerations
Weldability
Shear strength
Density
Coefficient of friction
Thermal conductivityB
Specific heatB
Crystalline melting temperature
A
See Practice D2991.
B
No ASTM or ISO standards exist today.

engineering analysis. For this reason, tensile modulus is more consider the material properties such as properties in tension,
appropriate and is therefore recommended. creep, and coefficient of linear thermal expansion, in both
5.7 Creep and fatigue data are commonly reported in directions.
flexure. However, the most useful data to the designer is 5.10 The required materials characterizations are summa-
uniaxial loading in tension mode. rized in Table 2. Suggested conditions are intended to serve as
5.8 Material properties in molded parts are a function of a guide in establishing standardized specific test conditions for
processing conditions because of their influence on orientation the purpose of providing comparable data.
and morphology developed in the molded part. Thus the
properties measured from large molded parts may differ from 6. Data Reporting Format
those obtained with standard test specimens. Use of filled or 6.1 Standardization of format for reporting the data for
reinforced materials may magnify these differences. engineering design acquired using harmonized test methods is
5.9 Molded parts frequently display anisotropy. As a result, deemed essential for providing comparable data among similar
significant property differences between flow and the trans- products from different suppliers.
verse directions can result. The use of filled or reinforced 6.2 In the case of single-point data, the reporting format for
materials may magnify this effect. It is, therefore, essential to each property shall include average, standard deviation, and

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D5592 − 94 (2018)
TABLE 2 Material Property Characterization Requirements
Test Method Suggested Conditions
ASTM ISO
I. Structural Criteria
Properties in tension D638 ISO 527-1, ISO at 23°C, at least three elevated temperatures and one temperature below standard
527-2, and ISO laboratory conditions at standard strain rate; at three additional strain rates at 23°C
527-4
Poisson’s ratio D638 ... at 23°C, at least one elevated temperature and one temperature below standard labo-
ratory conditions
Properties in compression D695 ISO 604 at 23°C, two additional elevated temperatures and one temperature below standard
laboratory conditions
Shear modulus (DMA/DMTA) D5279 ISO 6721-2 −150°C to Tg + 20°C or Tm + 10°C at approximately 1 Hz
Creep in tension D2990 ISO 899-1 at 23°C and at least two elevated temperatures for 1000 h at three stress levels
Fatigue in tension ... ... (a) S − N curves at three Hz at 23°C; 80, 70, 60, 55, 50, and 40 % of tensile stress at
yield; R = 0.5; 1 million cycles run out.
... ... (b) a − N curves at 3 Hz at 23°C; single edge notched specimens; three stress levels;
R = 0.5.
Coefficient of friction D1894 ISO 8295 against itself and steel
Application specific
Creep in bending D2990 ISO 899-2 at 23°C and at least two elevated temperatures for 1000 h and at least three stress
levels
Creep in compression D2990 ISO 899-1 at 23°C and at least two elevated temperatures for 1000 h and at least three stress
levels
Fatigue In Bending ... ... at 23°C; fully reversed; 80, 70, 60, 55, 50, and 40 % of tensile stress at yield at ap-
proximately 3 Hz
Fracture toughness D5045 ... K1c or G1c
Solvent resistance D543 ISO 175 Retention of tensile properties exposed to specific chemicals under no strain as well as
0.1, 0.25, and 0.5 % strain
UV Exposure/Weathering D2565 ISO 4892-2 1. Xenon Arc (0.35 to 0.70 W/m2 at 340 nm; 65°C black panel; and 50 % RH at ap-
proximately 315, 630, 1260, 1890, and 2520 kJ/m2 ; borosilicate/borosilicate or equiva-
lent filters);
Retention of tensile properties, color (CIELAB, D65, 10° standard observer, specular
included), and 60° Gardner gloss.
D1435 ISO 4607 2. 45° unbacked outdoor weathering (Florida and Arizona) for 3, 6, 9, 12, 18, and 24
months;
Retention of tensile properties, color (CIELAB, D65, 10° standard observer, specular
included), and 60° Gardner gloss.
Accelerated Aging D3045 ISO 2578 Retention of instrumented impact strength and tensile properties, color and Gloss at
three temperatures for 1000 h
II. Manufacturing Criteria
Viscosity-shear rate data D3835 ISO 11403-2 and At approximately three temperatures, over shear rate range 10 to 10 000 s−1
ISO 11443

Flowability D3123 ...


Melt density ... ... at 0 MPa and processing temperature
Thermal conductivity ... ... 23°C to processing temperature
Specific heat ... ... 23°C to processing temperature
No-flow temperature ... ...
Ejection temperature ... ...
Crystallization temperature D3418 ...
Heat of crystallization D3418 ...
Glass transition temperature D3418 ...
Flowlength versus nominal wall ... ... simulations at three combinations of melt temperature and mold temperature
thickness
pvT data ... ... 23°C to processing temperature; over 0 to 200 bars
Coefficient of linear thermal E228 ... over the range − 40° to 85°C
expansion
Mold shrinkage ... ISO 294-1 at least two thicknesses as function of cavity pressure, melt temperature, mold
temperature, injection time, and fixed gate geometry
Crystallization kinetics ... ...
Cure kinetics D4473 ...

number of specimens tested. These are required to enhance the The tabulated data lend itself to extraction of the information
confidence level of the designer. for design calculations.
6.3 In the case of multipoint data, the reporting format for
each property shall be in both graphical format and tabulated 7. Keywords
data. The graphical format is desired to illustrate the behavior 7.1 computer aided design (CAD); computer aided engi-
of the material in response to changes in temperature, time, and neering (CAE); engineering design; finite element analysis;
strain rate, in a format that is concise, indicative of the trends, manufacturability; plastics; structural analysis
and compatible with the needs of design methods employed.

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