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Designation: D 36 – 95

AMERICAN SOCIETY FOR TESTING AND MATERIALS


100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Test Method for


Softening Point of Bitumen (Ring-and-Ball Apparatus)1
This standard is issued under the fixed designation D 36; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope viscous as the temperature rises. For this reason, softening


1.1 This test method covers the determination of the soft- points must be determined by an arbitrary and closely defined
ening point of bitumen in the range from 30 to 157°C (86 to method if results are to be reproducible.
315°F) using the ring-and-ball apparatus immersed in distilled 4.2 The softening point is useful in the classification of
water (30 to 80°C), USP glycerin (above 80 to 157°C), or bitumens, as one element in establishing the uniformity of
ethylene glycol (30 to 110°C). shipments or sources of supply, and is indicative of the
1.2 The values stated in SI units are to be regarded as the tendency of the material to flow at elevated temperatures
standard. encountered in service.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5. Apparatus
responsibility of the user of this standard to establish appro- 5.1 Rings—Two square-shouldered brass rings conforming
priate safety and health practices and determine the applica- to the dimensions shown in Fig. 1(a).
bility of regulatory limitations prior to use. 5.2 Pouring Plate—A flat, smooth, brass plate approxi-
mately 50 by 75 mm (2 by 3 in.).
2. Referenced Documents 5.3 Balls—Two steel balls, 9.5 mm (3⁄8 in.) in diameter, each
2.1 ASTM Standards: having a mass of 3.50 6 0.05 g.
C 670 Practice for Preparing Precision and Bias Statements 5.4 Ball-Centering Guides—Two brass guides for centering
for Test Methods for Construction Materials2 the steel balls, one for each ring, conforming to the general
D 92 Test Method for Flash and Fire Points by Cleveland shape and dimensions shown in Fig. 1 (b).
Open Cup3 5.5 Bath—A glass vessel, capable of being heated, not less
D 140 Practice for Sampling Bituminous Materials4 than 85 mm in inside diameter and not less than 120 mm in
D 3461 Test Method for Softening Point of Asphalt and depth from the bottom of the flare.
Pitch (Mettler Cup-and-Ball Method)5
NOTE 1—An 800-mL, low-form Griffin beaker of heat-resistant glass
E 1 Specification for ASTM Thermometers6
meets this requirement.
3. Summary of Test Method 5.6 Ring Holder and Assembly—A brass holder designed to
3.1 Two horizontal disks of bitumen, cast in shouldered support the two rings in a horizontal position, conforming to
brass rings, are heated at a controlled rate in a liquid bath while the shape and dimensions shown in Fig. 1 (c), supported in the
each supports a steel ball. The softening point is reported as the assembly illustrated in Fig. 1 (d). The bottom of the shouldered
mean of the temperatures at which the two disks soften enough rings in the ring holder shall be 25 mm (1.0 in.) above the
to allow each ball, enveloped in bitumen, to fall a distance of upper surface of the bottom plate, and the lower surface of the
25 mm (1.0 in.). bottom plate shall be 166 3 mm (5⁄8 6 1⁄8 in.) from the bottom
of the bath.
4. Significance and Use
5.7 Thermometers:
4.1 Bitumens are viscoelastic materials without sharply 5.7.1 An ASTM Low Softening Point Thermometer, having
defined melting points; they gradually become softer and less a range from − 2 to + 80°C or 30 to 180°F, and conforming to
the requirements for Thermometer 15C or 15F as prescribed in
1
This test method is under the jurisdiction of ASTM Committee D-8 on Roofing, Specification E 1.
Waterproofing, and Bituminous Materials and is the direct responsibility of 5.7.2 An ASTM High Softening Point Thermometer, having
Subcommittee D08.03 on Surfacing and Bituminous Materials for Membrane a range from 30 to 200°C or 85 to 392°F, and conforming to the
Waterproofing and Builtup Roofing.
Current edition approved Oct. 10, 1995. Published December 1995. Originally requirements for Thermometer 16C or 16F as prescribed in
published as D 36 – 62T. Last previous edition D 36 – 86 (1993)e1. Specification E 1.
2
3
Annual Book of ASTM Standards, Vol 04.02. 5.7.3 The appropriate thermometer shall be suspended in
Annual Book of ASTM Standards, Vol 05.01.
4 the assembly as shown in Fig. 1 (d) so that the bottom of the
Annual Book of ASTM Standards, Vol 04.03.
5
Annual Book of ASTM Standards, Vol 04.04. bulb is level with the bottom of the rings and within 13 mm
6
Annual Book of ASTM Standards, Vol 14.03. (0.5 in.) of the rings, but not touching them or the ring holder.

1
D 36

NOTE 1—All dimensions are in millimetres.


FIG. 1 Shouldered Ring, Ball-Centering Guide, Ring Holder, and Assembly of Apparatus Showing Two Rings

Substitution of other thermometers shall not be permittted. 6.2.1 To prevent adhesion of bitumen to the pouring plate
when casting disks, the surface of the brass pouring plate may
6. Reagents and Materials be thinly coated just before use with silicone oil or grease
6.1 Bath Liquids: (Note 5), a mixture of glycerin and dextrin, talc, or china clay.
6.1.1 Freshly Boiled Distilled Water.
NOTE 5—Caution: Isolate silicones from other bituminous testing
NOTE 2—The use of freshly boiled distilled water is essential to avoid equipment and samples to avoid contamination, and wear disposable
trapping air bubbles on the surface of the specimen which may affect the rubber gloves whenever handling silicones or apparatus coated with them.
results. Silicone contamination can produce erroneous results in other tests such as
6.1.2 USP Glycerin, or those for penetration and flash point.

NOTE 3—Caution: Glycerin has a flash point of 160°C (320°F) in 7. Sampling


accordance with Test Method D 92.
7.1 Sample the material in accordance with Practice D 140.
6.1.3 Ethylene Glycol, with a boiling point between 195 and
197°C (383 and 387°F).
8. Test Specimens
NOTE 4—Caution: Ethylene glycol is toxic when taken internally or
inhaled as a vapor. Avoid prolonged or repeated skin contact and 8.1 Do not start unless it is planned to complete preparation
inhalation of vapors. Its flash point is 115°C (239°F) in accordance with and testing of all asphalt specimens within 6 h and all coal-tar
Test Method D 92. When using this bath liquid, conduct the test in a pitch specimens within 41⁄2 h. Heat the bitumen sample with
vented laboratory hood with adequate exhaust fan capacity to ensure care, stirring frequently to prevent local overheating, until it
removal of toxic vapors. has become sufficiently fluid to pour (Note 6). Stir carefully to
6.2 Release Agents: avoid incorporation of air bubbles in the sample.
2
D 36
NOTE 6—An electric hot plate having a minimum power to unit- (9°F)/min (Note 7). Protect the bath from drafts, using shields
surface-area ratio of 37 kW/m2 has been found satisfactory for this if necessary. Do not average the rate of temperature rise over
purpose. the test period. The maximum permissible variation for any
8.1.1 Take no more than 2 h to heat an asphalt sample to its 1-min period after the first 3 min shall be6 0.5°C (61.0°F).
pouring temperature; in no case shall this be more than 110°C Reject any test in which the rate of temperature rise does not
(200°F) above the expected softening point of the asphalt. fall within these limits.
8.1.2 Take no more than 30 min to heat a coal-tar pitch
NOTE 7—Rigid adherence to the prescribed heating rate is essential to
sample to its pouring temperature; in no case shall this be more reproducibility of results. Either a gas burner or electric heater may be
than 55°C (100°F) above the expected softening point of the used, but the latter must be of the low-lag, variable output type to maintain
coal-tar-pitch. the prescribed rate of heating.
8.1.3 If the test must be repeated later, do not reheat this
9.6 Record for each ring and ball the temperature indicated
sample; use a fresh sample in a clean container to prepare new
by the thermometer at the instant the bitumen surrounding the
test specimens.
ball touches the bottom plate. Make no correction for the
8.2 Heat the two brass rings (but not the pouring plate) to
emergent stem of the thermometer. If the difference between
the approximate pouring temperature, and place them on the
the two temperatures exceeds 1°C (2°F), repeat the test.
pouring plate treated with one of the release agents.
8.3 Pour a slight excess of the heated bitumen into each
10. Calculation
ring, and then allow the specimens to cool in ambient air for at
least 30 min. For materials that are soft at room temperature, 10.1 For a given bitumen specimen, the softening point
cool the specimens for at least 30 min at an air temperature at determined in a water bath will be lower than that determined
least 10°C (18°F) below the expected softening point. From the in a glycerin bath. Since the softening point determination is
time the specimen disks are poured, no more than 240 min necessarily arbitrary, this difference matters only for softening
shall elapse before completion of the test. points slightly above 80°C (176°F).
8.4 When the specimens have cooled, cut away the excess 10.2 The change from water to glycerin for softening points
bitumen cleanly with a slightly heated knife or spatula, so that above 80°C creates a discontinuity. With rounding, the lowest
each disk is flush and level with the top of its ring. possible asphalt softening point reported in glycerin is 84.5°C
(184°F), and the lowest possible coal-tar pitch softening point
9. Procedure reported in glycerin is 82.0°C (180°F). Softening points in
9.1 Select one of the following bath liquids and thermom- glycerin lower than these translate to softening points in water
eters appropriate for the expected softening point: of 80°C (176°F) or less, and shall be so reported.
9.1.1 Freshly boiled distilled water for softening points 10.2.1 The correction for asphalt is − 4.2°C (−7.6°F), and
between 30 and 80°C (86 and 176°F); use Thermometer 15C or for coal-tar pitch is − 1.7°C (−3.0°F). For referee purposes,
15F. The starting bath temperature shall be 5 61°C (41 6 2°F). repeat the test in a water bath.
9.1.2 USP glycerin for softening points above 80°C (176°F) 10.2.2 Under any circumstances, if the mean of the two
and up to 157°C (315°F); use Thermometer 16C or 16F. The temperatures determined in glycerin is 80.0°C (176.0°F) or
starting bath temperature shall be 30 6 1°C (86 6 2°F). lower for asphalt, or 77.5°C (171.5°F) or lower for coal-tar
9.1.3 Ethylene glycol for softening points between 30 and pitch, repeat the test in a water bath.
110°C (86 and 230°F); use Thermometer 16C or 16F. The 10.3 To convert softening points slightly above 80°C
starting bath temperature shall be 5 6 1°C (41 6 2°F). (176°F) determined in water to those determined in glycerin,
9.1.4 For referee purposes, all softening points up to 80°C the correction for asphalt is + 4.2°C ( + 7.6°F) and for coal-tar
(176°F) shall be determined in a water bath and all softening pitch is + 1.7°C ( + 3.0°F). For referee purposes, repeat the test
points above 80°C (176°F) shall be determined in a glycerin in a glycerin bath.
bath. 10.3.1 Under any circumstances, if the mean of the two
9.2 Assemble the apparatus in the laboratory hood with the temperatures determined in water is 85.0°C (185.0°F) or
specimen rings, ball-centering guides, and thermometer in higher, repeat the test in a glycerin bath.
position, and fill the bath so that the liquid depth will be 105 6 10.4 Results obtained by using an ethylene glycol bath will
3 mm (41⁄8 6 1⁄8 in.) with the apparatus in place. If using vary from those using water and glycerin. The following
ethylene glycol, make sure the hood exhaust fan is turned on formulas shall be used to calculate the differences:
and operating properly to remove toxic vapors. Using forceps, Asphalt:
place the two steel balls in the bottom of the bath so they will SP ~glycerin! 5 1.026583 3 SP ~ethylene glycol! 2 1.334968°C
reach the same starting temperature as the rest of the assembly. (1)
9.3 Place the bath in ice water, if necessary, or gently heat to SP ~water! 5 0.974118 3 SP ~ethylene glycol! 2 1.44459°C (2)
establish and maintain the proper starting bath temperature for
15 min with the apparatus in place. Take care not to contami- Coal Tar:
nate the bath liquid. SP ~glycerin! 5 1.044795 3 SP ~ethylene glycol! 2 5.063574°C
9.4 Again using forceps, place a ball from the bottom of the (3)
bath in each ball-centering guide. †SP ~water! 5 1.061111 3 SP ~ethylene glycol! 2 8.413488°C
9.5 Heat the bath from below so that the temperature (4)
indicated by the thermometer rises at a uniform rate of 5°C † Editorially corrected.
3
D 36
11. Report Therefore, results of two properly conducted tests on the same
11.1 When using ASTM Thermometer 15C or 15F, report to sample of bitumen from two laboratories should not differ by
the nearest 0.2°C or 0.5°F the mean or corrected mean of the more than 2.0°C (3.5°F).7
temperatures recorded in 9.6 as the softening point. 12.2 With ethylene glycol, the following criteria shall be
11.2 When using ASTM Thermometer 16C or 16F report to used for judging the acceptability of results:
the nearest 0.5°C or 1.0°F the mean or corrected mean of the 12.2.1 Single-Operator Precision—The single-operator
temperatures recorded in 9.6 as the softening point. standard deviation has been found to be 0.72°C (1.29°F).
11.3 Report the bath liquid used in the test. Therefore, results of two properly conducted tests by the same
12. Precision and Bias operator on the same sample of bitumen should not differ by
more than 2.0°C (3.5°F).7
12.1 With distilled water or USP glycerin, the following
12.2.2 Multilaboratory Precision—The multilaboratory
criteria shall be used for judging the acceptability of results
standard deviation has been found to be 1.08°C (1.95°F).
(95 % probability):
Therefore, results of two properly conducted tests on the same
12.1.1 Single-Operator Precision—The single-operator
sample of bitumen from two laboratories should not differ by
standard deviation has been found to be 0.41°C (0.73°F).
more than 3.0°C (5.5°F).7
Therefore, results of two properly conducted tests by the same
operator on the same sample of bitumen should not differ by 12.3 Bias—The procedure in Test Method D 36 has no bias
more than 1.2°C (2.0°F).7 because the value of the softening point of the bitumen test is
12.1.2 Multilaboratory Precision—The multilaboratory defined in terms of this test method.
standard deviation has been found to be 0.70°C (1.26°F).
13. Keywords
7
These numbers represent, respectively, the (1S) and (D2S) limits as described 13.1 asphalt; ball and ring; bitumen; coal tar; softening
in Practice C 670. point

The American Society for Testing and Materials 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 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, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

4
Designation: D 41 – 94 (Reapproval 2000)e1 American Association State
Highway and Transportation Officials Standard
AASHTO No.: M116

Standard Specification for


Asphalt Primer Used in Roofing, Dampproofing, and
Waterproofing1
This standard is issued under the fixed designation D 41; 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 (e) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

e1 NOTE—Editorially switched from English dominant to SI dominant.

1. Scope (680°F) shall conform to the following requirements:


1.1 This specification covers asphaltic primer suitable for Penetration at 25°C (77°F), 100 g, 5 s 20 to 50
Matter soluble in trichloroethylene not less than 99 %
use with asphalt in roofing, dampproofing, and waterproofing
below or above ground level, for application to concrete, 4. Sampling
masonry, metal, and asphalt surfaces. 4.1 From each shipment or fraction thereof representing
1.2 The values stated in SI units are to be regarded as the primer of the same kind, select a number of packages at
standard. The values given in parentheses are for information random equivalent to the cube root of the total number of
only. packages in the lot. If the cube root as calculated proves to be
1.3 This standard does not purport to address all of the a fractional number, it shall be expressed as the next higher
safety concerns, if any, associated with its use. It is the whole number. For convenience, the following table is given,
responsibility of the user of this standard to establish appro- showing the number of samples to be selected for shipments of
priate safety and health practices and determine the applica- various sizes:
bility of regulatory limitations prior to use.
Packages in Shipment Packages Selected
2 to 8 2
2. Referenced Documents 9 to 27 3
2.1 ASTM Standards: 28 to 64 4
65 to 125 5
D 5 Test Method for Penetration of Bituminous Materials2 126 to 216 6
D 88 Test Method for Saybolt Viscosity3 217 to 343 7
D 95 Test Method for Water in Petroleum Products and 344 to 512 8
513 to 729 9
Bituminous Materials by Distillation4 730 to 1000 10
D 402 Test Method for Distillation of Cut-Back Asphaltic 1001 to 1331 11
(Bituminous) Products2 4.2 By means of a paddle, thoroughly stir the contents of
D 2042 Test Method for Solubility of Asphalt Materials in each package selected so as to bring all portions thereof into
Trichloroethylene2 uniform distribution. With an appropriate sampler, immedi-
3. Physical Requirements ately draw not less than 450 ml (1 pt) of the primer from the
center of each package, and transfer to a clean receptacle of
3.1 The primer shall conform to the following requirements: suitable size, which in turn shall be kept tightly covered, prior
Water, Vol %, max 0.5 to and immediately after the samples are being introduced.
Saybolt Furol viscosity at 25°C (77°F) 25 to 125 s
Distillation, volume % of the primer: After all the pint has been added, thoroughly agitate the
Up to 225°C (437°F) not less than 35 contents of the container, whereupon immediately transfer 0.95
Up to 360°C (680°F) not more than 65
L (1 qt) of the mixture to a clean quart can provided with a
3.2 The residue obtained from the distillation up to 360°C tightly fitting screw cap, and immediately fasten the cap in
place. This sample shall be considered as representative of the
1
This specification is under the jurisdiction of ASTM Committee D-8 on shipment and shall be transmitted to the laboratory for exami-
Roofing, Waterproofing, and Bituminous Materials and is the direct responsibility of nation, bearing a suitable tag or other means of identification.
Subcommittee D08.05 on Solvent-Bearing Bituminous Compounds for Roofing and
Waterproofing. 5. Test Methods
Current edition approved Dec. 15, 1994. Published February 1995. Originally
published as D 41 – 17 T. Last previous edition D 41 – 85. 5.1 Determine the properties enumerated in this specifica-
2
Annual Book of ASTM Standards, Vol 04.03. tion in accordance with the following test methods of the
3
Annual Book of ASTM Standards, Vol 04.04. American Society for Testing and Materials:
4
Annual Book of ASTM Standards, Vol 05.01.

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

1
D 41
5.1.1 Furol Viscosity—Test Method D 88. packages not conforming to the requirements.
5.1.2 Distillation—Test Method D 402.
5.1.3 Penetration—Test Method D 5. 7. Packaging and Package Marking
5.1.4 Soluble in Trichloroethylene—Test Method D 2042. 7.1 All products shall be packaged and labeled in accor-
5.1.5 Water—Test Method D 95. dance with applicable regulations.
6. Rejection and Resubmittal 7.2 Each package shall indicate the applicable ASTM des-
6.1 Failure to conform to any of the requirements prescribed ignation.
in this specification may constitute grounds for rejection. In the
case of rejection, the supplier shall have the right to reinspect 8. Keywords
the rejected material and resubmit the lot after removal of those 8.1 asphalt; dampproofing; primer; roofing; waterproofing

The American Society for Testing and Materials 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 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, 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).

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