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: D5644 − 18

Standard Test Method for

Rubber Compounding Materials—Determination of Particle
Size Distribution of Recycled Vulcanizate Particulate
Rubber1
This standard is issued under the fixed designation D5644; 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
1.1 This test method describes the procedures for determin-
ing average particle size distribution of recycled vulcanizate
particulate rubber by the Ro-tap sieve test method for 90 µm
(170 mesh) or larger particles.
1.2 The values stated in SI units are to be regarded as the
standard.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
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.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:2
D1566 Terminology Relating to Rubber
D5603 Classification for Rubber Compounding Materials—
Recycled Vulcanizate Particulate Rubber
E11 Specification for Woven Wire Test Sieve Cloth and Test
Sieves
E105 Practice for Probability Sampling of Materials
1
This test method is under the jurisdiction of ASTM Committee D11 on Rubber
and Rubber-like Materials and is the direct responsibility of Subcommittee D11.20
on Compounding Materials and Procedures.
Current edition approved June 1, 2018. Published July 2018. Originally approved
in 1994. Last previous edition approved in 2013 as D5644 – 01 (2013). DOI:
10.1520/D5644-18.
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.
3. Terminology
3.1 Definitions:
3.1.1 parent compound, n—original compound used in the
product.
3.1.2 recycled vulcanizate rubber, n—vulcanized rubber that
has been processed to give particulates or other forms of
different shapes, sizes, and size distributions.
3.1.3 Discussion—The words “vulcanizate” and “vulca-
nized rubber” are interchangeable. Additional terminology
associated with this classification can be found in Terminology
D1566.
4. Significance and Use
4.1 The particulate size distribution of vulcanizate particu-
late rubber is used for the purpose of assigning a product mesh
or average particle size designation.
4.2 The product designation for mesh size for the Ro-tap
method is based on the size designation screen which allows a
range for the upper limit retained of maximum 5 % for up to
850 µm (20 mesh) particles, maximum 10 % for 850 to 150 µm
(20 to 100 mesh), and maximum 15 % for 125 to 20 µm (120
to 635 mesh). No rubber particles shall be retained on the zero
screen (see Table 2, Classification D5603).
4.3 The weight percent retained on a specific screen is
noted.
5. Summary of Test Method
5.1 Ro-tap Method, Mechanical Vibratory Sieve Shaker—A
100 6 1 g specimen of the recycled rubber is combined with
a fixed amount of flowing agent (for example, hydrous mag-
nesium silicate (talc), fumed, aluminum oxide, fumed silica, or
calcium carbonate) and placed on top of a series of mesh
sieves, with the coarsest sieve being on top and the finest on the
bottom. The specimen is placed in a Ro-tap shaker for 10 to 20
min, depending on the grade of the recycled rubber. The weight
of the rubber retained on the individual sieves is then recorded
and the mesh designation of the product determined.

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 D5644 − 18
6. Apparatus
3
6.1 Mechanical Sieve Shaker —This is a mechanically
operated sieve shaker that imparts a uniform rotary and tapping
motion to a stack of 200 mm (7.9 in.) sieves in accordance with
6.2. The sieve shaker should be adjusted to accommodate a
stack of sieves, receiver pan, and cover plate. The bottom stops
should be adjusted to give a clearance of 1.5 mm (0.06 in.)
between the bottom plate and the screens so that the screens
will be free to rotate. The sieve shaker machine shall be
powered with an electric motor operating 28.75 to 29.17 Hz
(1725 to 1750 rpm). This will produce 2.33 to 2.60 Hz and 280
to 320 rotary motions/min. The cover plate shall be fitted with
a cork stopper that shall extend from 3.00 to 9.00 mm (0.118
to 0.354 in.) above the metal recess. At no time, shall rubber,
wood, or other material other than cork be permitted.
6.2 Standard Sieves, stainless steel or brass, 200 mm (7.9
in.) in diameter in accordance with Specification E11. The
sieve set should include a lid and a bottom pan.
6.3 Digital Scale with Tare Function, with a sensitivity of
weighing at a minimum 0.1 g.
6.4 Brushes:
6.4.1 A soft brass wire brush for cleaning sieves 425 µm
(40) mesh and coarser.
6.4.2 A nylon bristle brush for cleaning sieves finer than 425
µm (40) mesh.
6.5 Glass or Metal Measuring Cup, with a capacity of 500
cm3 (1 pint).
6.6 Glass Wide-Mouth Jar with Lid, with capacity of 500
cm3 (1 pint).
6.7 Rubber Balls, 4 with a diameter from 25 to 50 mm (1 to
2 in.) or plastic rings with a height of 20 6 3 mm, an outside
diameter of 60 6 3 mm, and an inside diameter of 58 6 3 mm.
The height of the balls or rings must be less than the depth of
the screens being used. Use two balls or two plastic rings per
test screen as per 7.1.5. Balls and rings are not to be used
simultaneously.
6.8 Flow Agent (same as 5.1), usually some mixture of
magnesium silicate, silica, magnesium oxide, magnesium-
aluminum silicate with at least 90 % of the particles being less
than 40 µm (approximately 400 mesh) in size.
7. Procedure
7.1 Selection and Preparation of Test Screens:
7.1.1 Select test screens appropriate to the particle size
distribution of the product being tested. A set of two to six
sieves and a receiver pan are normally used. The actual number
of sieves is to be agreed upon by vendor and customer.
7.1.2 Verify each screen has been cleaned of all particles on
both sides of screen with brush (see 6.4).
3
The Ro-Tap Sieve Shaker meets the specified conditions and has been found
satisfactory for this purpose and is available from many scientific laboratory
suppliers.
4
Available from various sieve manufacturing suppliers.
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7.1.3 Stack test screens in order of increasing mesh size
with smallest number on top (coarsest) and highest number on
bottom (finest).
7.1.4 Add bottom receiver pan to stack.
7.1.5 Verify rubber balls or plastic rings are in place in test
screens; For products of 425 µm (40 mesh) or finer, add two
rubber balls or two plastic rings per sieve. For products coarser
than 425 µm (40 mesh), the use of rubber balls or plastic rings
as an agitation aid is optional. Rubber balls and plastic rings
are not to be mixed on any test screen.
7.2 Preparation of Specimen:
7.2.1 Obtain approximately 150 to 200 g of vulcanizate
particulate rubber from the lot (refer to Practice E105).
7.2.2 Place an empty glass or metal measuring cup on
digital scale. Press tare feature to determine tare weight of
measuring cup.
7.2.3 Using the glass or metal measuring cup weigh 100 g of
specimen to the nearest gram.
7.2.4 Transfer 100 g of specimen into glass jar as defined in
6.6.
7.3 Preparation of Flow Agent:
7.3.1 Place empty glass or metal measuring cup on digital
scale; press tare feature to determine tare weight of measuring
cup.
7.3.2 Using the empty glass or metal measuring cup weigh
flow agent per product gradation designation. For products
designated coarser than 300 µm (50 mesh), weigh 5.0 6 0.1 g
of flow agent. For products designated 300 µm (50 mesh) or
finer, weigh 15.0 6 0.1 g of flow agent.
7.3.3 Add flow agent to specimen in glass jar as defined in
6.6 and seal glass jar with lid.
7.3.4 Thoroughly shake the glass jar for a minimum of 1
min until agglomerates are broken and flow agent is uniformly
mixed or dispersed.
7.4 Remove specimen and flow agent from glass jar and
place on top screen. Place cover on top of stack.
7.5 Place the stack in the shaker.
7.6 Activate the shaker for 10 min for products designated
coarser then 300 µm (50 mesh). For products designated 300
µm (50 mesh) or finer, activate the shaker for 20 min.
7.7 After the shaker completes the appropriate cycle, re-
move the stack.
7.8 Determine and Record Results:
7.8.1 Place empty glass or metal measuring cup on digital
scale; press tare feature to determine tare weight of measuring
cup;
7.8.2 Starting with the top sieve, remove the screened
fraction by gently tapping its contents to one side and pouring
the contents into the metal or glass measuring cup and
recording its mass to the nearest 0.1 g. Record any mass less
than 0.1 g as trace.
7.8.3 Brush any material adhering to the bottom of the
screen onto the next finer screen.
7.8.4 Empty the glass or metal measuring cup and set the
specimen aside.
 D5644 − 18
7.8.5 Repeat 7.8.1 – 7.8.4 until all sieves in the stack and the
bottom pan have been emptied, weighed, and recorded. This
gives the weight retained on each screen.
8. Calculation
8.1 The sum of the masses of each fraction from the sieves
and the bottom pan shall not be less than the original mass of
the specimen plus mass of flow agent less 2 g, or greater than
the original mass of the specimen plus 100 % of flow agent
added. Repeat test if either of these conditions occurs.
8.2 To calculate the relative fractions of the samples that are
retained on each screen and the pan, create a list of all screens
used in the procedure including the top screen (zero screen)
and pan.
8.2.1 Adjacent to each entry on the list, record the retained
weight on each screen and pan. Sum total of the values for each
screen including the pan to obtain the total weight retained
from the test sample.
8.2.2 For each entry on the list, divide the retained weight in
grams by the total weight of the test sample and multiply by
100 to put the results in the form of percent of the sample
retained on each screen and the pan. Round the result to the
nearest 0.1 %.
8.2.3 Record this percentage for each screen and pan. The
percent passed for each screen and pan is calculated by
subtracting the percent retained from 100 % for the first screen.
Each screen following the first screen is calculated by subtract-
ing the percent retained of that screen from the previous screen
percent passed for all remaining screens including the pan.
8.3 The top screen (zero screen) selected shall be one in
which no rubber particles are retained. This “zero percent
retained screen” is designated in Classification D5603 Table 2
(see Note 1).
8.4 The second screen in the sieve deck is for product
designation and can contain a maximum 5 % for up to 850 µm
(20 mesh) particles, maximum 10 % for 850 to 150 µm (20 to
100 mesh), and maximum 15 % for 125 to 20 µm (120 to 635
mesh) (see Note 1).
NOTE 1—An example of 8.3 and 8.4 is if an 850-µm (20 mesh) sieve
contains zero rubber particles and a 600-µm (30-mesh) sieve contains 3 %
rubber particles, then the proper product designation for this material is
600-µm (30-mesh) particulate rubber product.
9. Report
9.1 Report the following information: Product Technical
Data Sheet or Sieve Analysis (Identify Name of Report)
9.1.1 Name of Company, address and phone if applicable.
9.1.2 Date of test.
9.1.3 Name of person that tested material.
9.1.4 Proper identification of specimen provided for testing.
9.1.4.1 Nominal size: SI Units or Mesh Size.
9.1.4.2 Sieves Used (that is, SI Standard, U.S. Sieve; W.S.
Tyler).
9.1.4.3 ASTM Grade #1 to #8 and definition of grade per
ASTM D5603.
9.1.4.4 Cryogenic or ambient/mechanical.
9.1.4.5 Descriptive Appearance before testing.
9.1.4.6 Packaging.
9.1.5 Proper identification of sample weight.
9.1.6 Proper identification of flow agent weight.
9.1.7 Identification of each sieve used.
9.1.8 The residue mass (Designated Weight Retained) per
test screen.
9.1.9 The mass on the bottom pan.
9.1.10 Total all the Weight findings to determine the total
mass of specimen including flow agent.
9.1.11 Identify designated percent retained (see 8.2.2 for
calculations).
9.1.12 Identify Percent passed (see 8.2.3 for calculation).
9.1.13 Identify whether specimen passed or failed test or
identify mesh size of specimen.
9.1.14 Identify free metal percent.
9.1.15 Identify free fiber percent.
9.1.16 Example of “Reporting” Results of Pass.
10. Precision and Bias
10.1 Round-robin testing will be conducted and precision
and bias statements will be balloted for inclusion when testing
is completed.
11. Keywords
11.1 particle size distribution; recycled vulcanizate particu-
late rubber; ultrasonic light optical microscopic technique

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