Designation: D 4894 – 07

Standard Specification for

Polytetrafluoroethylene (PTFE) Granular Molding and Ram
Extrusion Materials 1
This standard is issued under the fixed designation D 4894; 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* 2. Referenced Documents

1.1 This specification covers granular resins and test meth- 2.1 ASTM Standards: 2
ods for polytetrafluoroethylene (PTFE) that have never been D 618 Practice for Conditioning Plastics for Testing
preformed or molded and are normally processed by methods D 638 Test Method for Tensile Properties of Plastics
similar to those used in powder metallurgy or ceramics, or by D 792 Test Methods for Density and Specific Gravity (Rela-
special extrusion processes. These PTFE resins are homopoly- tive Density) of Plastics by Displacement
mers of tetrafluoroethylene, or, in some cases, modified ho- D 883 Terminology Relating to Plastics
mopolymers containing not more than one percent by weight of D 1895 Test Methods for Apparent Density, Bulk Factor,
other fluoromonomers. The usual methods of processing ther- and Pourability of Plastic Materials
moplastics generally are not applicable to these materials D 3295 Specification for PTFE Tubing, Miniature Beading
because of their viscoelastic properties at processing tempera- and Spiral Cut Tubing
tures. The materials included herein do not include mixtures of D 3892 Practice for Packaging/Packing of Plastics
PTFE resin with additives such as colorants, fillers or plasti- D 4441 Specification for Aqueous Dispersions of Polytet-
cizers; nor do they include reprocessed or reground resin or any rafluoroethylene
fabricated articles. The methods and properties included are D 4591 Test Method for Determining Temperatures and
those required to identify the various types of resins. Addi- Heats of Transitions of Fluoropolymers by Differential
tional procedures are provided in the Appendix for further Scanning Calorimetry
characterization of the resins. D 4745 Specification for Filled Compounds of Polytet-
1.2 The values stated in SI units as detailed in IEEE/ASTM rafluoroethylene (PTFE) Molding and Extrusion Materials
SI-10 are to be regarded as the standard, and the practices of D 4895 Specification for Polytetrafluoroethylene (PTFE)
IEEE/ASTM SI-10 are incorporated herein. Resin Produced From Dispersion
1.3 The following precautionary caveat pertains only to the E 11 Specification for Wire Cloth and Sieves for Testing
Specimen Preparation section, Section 9, and the Test Methods Purposes
section, Section 10, of this specification: This specification E 177 Practice for Use of the Terms Precision and Bias in
does not purport to address all of the safety concerns, if any, ASTM Test Methods
associated with its use. It is the responsibility of the user of this IEEE/ASTM SI-10 Standard for Use of the International
standard to establish appropriate safety and health practices System of Units (SI): The Modern Metric System
and determine the applicability of regulatory limitations prior 2.2 ISO Standards: 3
to use. See Notes 3 and 9 for specific cautionary statements. ISO 12086-1 Plastics—Fluoropolymer Dispersions and
NOTE 1—Information in this specification is technically equivalent to
Moulding and Extrusion Materials—Part 1: Designation
related information in ISO 12086-1 and ISO 12086-2. System and Basis for Specification

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 [email protected]. For Annual Book of ASTM
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Standards volume information, refer to the standard’s Document Summary page on
Materials. the ASTM website.
3
Current edition approved Sept. 1, 2007. Published October 2007. Originally Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
approved in 1989. Last previous edition approved in 2004 as D 4894 - 04. 4th Floor, New York, NY 10036.

*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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 D 4894 – 07
TABLE 1 Detail Requirements for Tests on ResinsA
Particle Size, Average Diameter, Melting Peak Temperature
Type Grade Bulk Density, g/L Water Content, max, %
µm Initial °C Second °C
A
I 1 700 6 100 500 6 150 0.04 327 6 10
A
2 675 6 50 375 6 75 0.04 327 6 10
A
II ... ... <100 0.04 327 6 10
A
III 1 400 6 125 <100 0.04 327 6 10
A
2 850 6 100 500 6 150 0.04 327 6 10
A
IV 1 650 6 150 550 6 225 0.04 327 6 10
A
2 >800 ... 0.04 327 6 10
A
3 580 6 80 200 6 75 0.04 327 6 10
V ... 635 6 100 500 6 250 0.04 327 6 10 327 6 10
A
VI ... 650 6 150 800 6 250 0.04 327 6 10
A
>5°C above the second melting peak temperature.

ISO 12086-2 Test Methods for Fluoropolymers 4.1.1 Type I—Resin used for general-purpose molding and
ram extrusion.
3. Terminology 4.1.2 Type II—Finely divided resin with an average particle
3.1 Definitions: size less than 100 micrometres.
3.1.1 The terminology given in Terminology D 883 is ap- 4.1.3 Type III—Modified resins, either finely divided or
plicable to this specification. free-flowing, typically used in applications requiring improved
3.2 Descriptions of Terms Specific to This Standard: resistance to creep and stress-relaxation in end-use.
3.2.1 bulk density—the mass (in grams) per litre of resin 4.1.4 Type IV—Free-flowing resins. Generally made by
measured under the conditions of the test. treatment of finely divided resin to produce free-flowing
3.2.2 extended specific gravity (ESG)—the specific gravity agglomerates.
of a specimen of PTFE material molded as described in this 4.1.5 Type V—Presintered. Resin that has been treated
specification and sintered (g.v.) for an extended period of time, thermally at or above the melting point of the resin at
compared to the sintering time for the measurement of standard atmospheric pressure without having been previously pre-
specific gravity (SSG), using the appropriate sintering schedule formed.
given in this specification. 4.1.6 Type VI—Resin, not presintered, but for ram extrusion
3.2.3 lot, n—one production run or a uniform blend of two only.
or more production runs. NOTE 2—See Tables 1 and 2 for division of Types by Grades, and
3.2.4 preforming—compacting powdered PTFE material footnotes to Tables 1 and 2 (and Table X2.1 in Appendix X2.) for former
under pressure in a mold to produce a solid object, called a classifications.
preform, that is capable of being handled. Molding and 4.2 A line callout system is used to specify materials in this
compaction are terms used interchangeably with preforming standard. The system uses predefined cells to refer to specific
for PTFE. aspects of this specification, illustrated as follows:
3.2.5 reground resin—that produced by grinding PTFE Specification
material that has been preformed but has never been sintered. Standard Number Block : Type : Grade : Class : Special notes
3.2.6 reprocessed resin—that produced by grinding PTFE : : : : :
material that has been both preformed and sintered. Example: ASTM III 2
3.2.7 sintering—as it applies to PTFE, a thermal treatment D 4894 – 04
during which the PTFE is melted and recrystallized by cooling
with coalescence occurring during the treatment. For this example, the line callout would be ASTM
3.2.8 skiving—a machining operation during which a con- D 4894 – 04, III2, and would specify a granular polytetrafluo-
tinuous film of PTFE material is peeled from the lateral surface roethylene that has all of the properties listed for that Type and
of a cylindrical sintered molding. Grade in the appropriate specified properties, Tables, or both,
3.2.9 standard specific gravity (SSG)—the specific gravity in this specification. In this case there is no Class item so the
of a specimen of PTFE material molded as described in this cell position for class is left blank. A comma is used as the
specification and sintered using the appropriate sintering separator between Standard Number and Type. Separators are
schedule given in this specification. not needed between Type, Grade, and Class.4 Provision for
3.2.10 thermal instability index (TII)—a measure of the Special Notes is included so that other information will be
decrease in molecular weight of PTFE material which has been provided when required. An example would be in Specification
heated for a prolonged period of time. D 3295 where dimensions and tolerances are specified for each
AWG size within Type and Class. When Special Notes are
4. Classification used, they shall be preceded by a comma.
4.1 This specification covers the following six types of
PTFE generally used for compression molding or ram extru-
sion, or both: 4
See the ASTM Form and Style Manual, available from ASTM Headquarters.

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 D 4894 – 07
TABLE 2 Detail Requirements for Tests on Molded Specimens
Standard Specific Gravity Tensile Strength min
Type Grade Thermal Instability Index, max Elongation at break min %
min max MPa psi
I 1 50 2.13 2.18 13.8 2000 140
2 50 2.13 2.18 17.2 2500 200
II ... 50 2.13 2.19 27.6 4000 300
III 1 50 2.14 2.22 28.0 4060 450
2 50 2.14 2.18 20.7 3000 300
IV 1 50 2.13 2.19 25.5 3700 275
2 50 2.13 2.19 27.6 4000 300
3 50 2.15 2.18 27.6 4000 200
V ... NAA NAA NAA NAA NAA NAA
VIB ... NAA NAA NAA NAA NAA NAA
A
NA: Not Applicable by molding techniques included in this specification.
B
Extrusions of this resin show different degrees of clarity from the others.

5. Mechanical Properties plug height to allow the resin in the die can be leveled by
5.1 The resins covered by this specification shall conform to drawing a straightedge in contact with the top of the die across
the requirements prescribed in Tables 1 and 2 when tested by the top of the die cavity. Insert the die in a suitable hydraulic
the procedures specified herein. Table 1 lists tests to be carried press and apply pressure gradually (Note 3) until a total of 34.5
out on resins. Table 2 lists tests requiring specimens molded as MPa [5000 psi] is attained. Hold this pressure for 3 min.
described in Section 9. Remove the disk identification on the disk at this time.
NOTE 3—As a guide, increasing the pressure at a rate of 3.45 MPa [500
6. Other Requirements psi]/min is suggested until the desired maximum pressure is attained.
6.1 The resin shall be uniform and shall contain no additives
9.1.3 Sinter the preforms in accordance with Table 3 (Note
or foreign material.
4).
6.2 The color of the material as shipped by the seller shall
9.1.3.1 Use Procedure B for Types I, II and IV and Proce-
be white.
dure C for Type III.
7. Sampling NOTE 4—Although the rate of heating application is not critical, the
7.1 Sampling shall be statistically adequate to satisfy the cooling cycle is most important and the conditions cited in these
requirements of 11.4 procedures must be followed very closely. If they are not followed, the
crystallinity of the disks and the resulting physical properties will be
markedly changed. Therefore, the use of a programmed oven is recom-
8. Number of Tests
mended for the most precise sintering cycle control so that the hood
8.1 Lot inspection shall include tests for bulk density, window will be left down during the entire sintering procedure, the latter
particle size and standard specific gravity. Periodic tests shall being an important safety consideration.
consist of all the tests specified in Tables 1 and 2 and shall be 9.2 Test Specimens for Standard Specific Gravity (SSG) and
made at least one per year. Extended Specific Gravity (ESG):
8.2 The tests listed in Tables 1 and 2, as they apply, are 9.2.1 A cylindrical preforming die, 28.6 mm [11⁄8 in.]
sufficient to establish conformity of a material to this specifi- internal diameter by at least 76.2 mm [3 in.] deep, is used to
cation. One set of tests specimens as prescribed in Section 7 prepare the preforms. End plug clearances shall be sufficient to
shall be considered sufficient for testing each sample. The ensure escape of air during pressing. The test resin shall be near
average of the results for the specimens tested shall conform to ambient temperature prior to molding (Note 5).
the requirements of this specification.
NOTE 5—For maximum precision, the weighing and preforming opera-
9. Specimen Preparation tions shall be carried out at 23 6 2°C [73.4 6 3.6°F] (the “near ambient”
temperature referred to herein). These operations shall not be preformed at
9.1 Test Disks: temperatures below 21°C [70°F] due to the crystalline transition that
9.1.1 Use the die shown in Fig. 1 for the molding of test occurs in PTFE in this temperature region which leads to possible cracks
disks. The test resin shall be near ambient temperature prior to in sintered specimens and differences in specimen density (as well as
molding (Note 5). Warning—PTFE can evolve small quanti- changes in other physical properties). Problems caused by the effects of
ties of gaseous products when heated above 204°C [400°F]. temperature on the specific gravity or density of PTFE will be minimized
Some of these gases are harmful. Consequently, exhaust when the measurement is made using immersion procedures if a sensitive
ventilation must be used whenever the resins are heated above thermometer (for example, one reading 60.1°C) is used in the liquid and
the temperature is adjusted to be at least 22°C.
this temperature, as they are during the sintering operations
that are a part of this specification. Since the temperature of 9.2.2 Weigh out 12.0 6 0.1 g of resin and place it in the die.
burning tobacco exceeds 204°C [400°F], those working with Screen non-free-flowing resins through a No. 10 sieve. Break
PTFE resins should ensure that tobacco is not contaminated. up compacted resins by hand-shaking cold resin in a half-filled
9.1.2 Screen 14.5 g (for tensile properties) or 7.25 g (for sealed glass container. Condition the resin in the sealed glass
electrical properties discussed in Appendix X1.7) of PTFE container in a freezer or dry-ice chest. After breaking up resin
resin through a No. 10 hand sieve into the die. Adjust the lower lumps, allow the sealed container to equilibrate to near ambient

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 D 4894 – 07

FIG. 1 Assembly and Details of Die for Molding Test Specimens

TABLE 3 Sintering Procedures

B C D E F G H I
Initial temperature, °C [°F] 290 [554] 290 [554] 238 [460] 238 [460] 290 [554] 238 [460] 238 [460] 238 [460]
Rate of heating, °C/h [°F/h] 120 6 10 120 6 10 60 6 5 60 6 5 120 6 10 60 6 5 60 6 5 60 6 5
[216 6 18] [216 6 18] [108 6 9] [108 6 9] [216 6 18] [108 6 9] [108 6 9] [108 6 9]
Hold temperature, °C [°F] 380 6 6 357 6 8 371 6 6 360 6 6 380 6 6 357 6 8 380 6 6 371 6 6
[716 6 10] [675 6 15] [700 6 10] [685 6 10] [716 6 10] [675 6 5] [716 6 10] [700 6 10]
Hold time, min 30 + 2, −0 30 + 2, −0 240 6 15 240 6 15 360 6 5 240 6 15 960 6 15 120 6 5
Cooling rate, °C/h [°F/h] 60 6 5 60 6 5 60 6 5 60 6 5 60 6 5 60 6 5 60 6 5 60 6 5
[108 6 9] [108 6 9] [108 6 9] [108 6 9] [108 6 9] [108 6 9] [108 6 9] [108 6 9]
Final or second hold temperature, °C 294 6 6 294 6 6 238 6 6 238 6 6 294 6 6 238 6 6 238 6 6 238 6 6
[°F]
[561 6 10] [561 6 10] [460 6 10] [460 6 10] [561 6 10] [460 6 10] [460 6 10] [460 6 10]
Second hold time, min 24 + 0.5, −0 24 + 0.5, −0 NAA NAA 24 + 0.5, −0 NAA NAA NAA
Period to room temperature, min, h 1⁄ 2 1 ⁄2 6 6 1 ⁄2 6 6 6
A
NA, Not applicable.

temperature. Then screen and weigh the 12.0 6 0.1-g sample.

Insert the die in a suitable hydraulic press and apply pressure
gradually (Note 3) until a pressure of 34.5 MPa [5000 psi] is
attained. Hold this pressure for 2 min. Remove the preform
from the die. Write the sample identification number using an
appropriate marker that will not effect the PTFE during
sintering on the preform at this time.
9.2.3 Sinter the preforms in accordance with Table 3 (Note
4).
9.2.3.1 For SSG specimens use Procedure B for Types I, II
and IV and Procedure C for Type III.
9.2.3.2 For ESG specimens use Procedure F for Types I, II
and IV and Procedure G for Type III.
NOTE 6—Improved precision in SSG and ESG test results has been
obtained with the use of an upright, cylindrical oven and an aluminum
sintering rack. The cylindrical oven has an inside diameter of 140 mm [5.5
in.] and an inside depth of 203 mm [8 in.] plus additional depth to
accommodate a 50.8-mm [2-in.] thick cover, and is equipped with suitable
heaters and controllers to sinter specimens in accordance with the
Procedures in Table 3. The rack, as shown in Fig. 2, allows preforms to be
placed symmetrically in the center region of the oven. Place six preforms
FIG. 2 SSG Samples Sintering Rack
on each of the middle oven rack shelves (if six or fewer preforms are to
be sintered, place them on the middle rack, filling in with “dummies” as
needed). Place “dummies” on the top and bottom shelves. Specimens must be spaced evenly in a circle on each shelf, with none of them touching. An

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 D 4894 – 07

FIG. 4 Sectioned PTFE Test Billet

FIG. 3 Preforming of PTFE Test Billet

34.5 MPa [5000 psi] for Type I and 17.2 MPa [2500 psi] for
Types II, III and IV. Hold under maximum pressure for 2 to 5
oven load must be no less than 18 pieces including “dummies.” “Dum- min. Release the pressure by gradually “cracking” the pressure
mies” are defined as normal 12-g specimens that have previously been release valve without an apparent movement of the press
through the sintering cycle. “Dummies” must only be used for an
additional two or three thermal cycles, due to eventual loss of thermal
platens. Remove the top pusher and force the preform verti-
stability and physical form. cally out of the mold shell using a continuous, smooth
movement.
9.2.4 Remove all flash from each specimen so that no air
bubbles will cling to the edges when the specimen is immersed NOTE 7—Remove the mold in a careful smooth movement from the die
in the solution for weighing during the standard specific gravity to prevent cracking.
and thermal instability index tests. It is recommended for this 9.3.3 Sinter the preform in accordance with Table 3 (Note
section and during testing that cotton gloves be worn while 4).
handling test specimens. 9.3.3.1 Use Procedure D for Types I, II and IV and
9.3 Test Billets: Procedure E for Type III—except for ESG specimens.
9.3.1 Use test specimens cut or skived from billets may be 9.3.3.2 For ESG specimens use Procedure H for Types I, II,
used as alternatives to the test disks described in 9.1 and 9.2 for and IV and Procedure I for Type III.
Types I, II, III and IV resins. 9.3.4 Divide the test billet into sections by making trans-
9.3.2 Mold test billets in a mold similar to Fig. 3, having an verse cuts by machining, or by a suitable alternate procedure,
inside diameter of 57 mm [2.25 in.] and of sufficient height to in accordance with Fig. 4. Use a saw for the rough cuts
contain the resin sample. Plug clearance shall be sufficient to between Sections I and II and between sections III and IV, but
ensure escape of air during pressing. A 254-mm [10-in.] mold Faces C and D must be prepared by machining. Prepare five
cavity fill depth will produce a billet approximately 76 mm [3 test specimens for the determination of tensile properties from
in.] long from a resin charge of 400 6 50 g. Vary the billet 0.8-mm [1⁄32-in.] thick slices machined from Section II, Face C,
length in accordance with the testing to be done. The test resin and machine a slice of suitable thickness for standard specific
shall be near ambient temperature prior to molding (Note 4). gravity measurements as described in 10.5. Care shall be taken
9.3.2.1 Adjust the lower plug position using a support ring to avoid wedge-shaped cuts. Use the remainder of Section II to
to position the mold shell so that the resin level will not come prepare tape specimens by skiving 0.13 mm (5 mils) thick.
within 13 mm [0.5 in.] of the top of the mold cavity. Add the Discard the initial five revolutions of skived tape before taking
resin to the mold, insert the top plug, and apply hand pressure. the test sample. Use the tape for the determination of tensile
Remove the support ring, and place the mold in a hydraulic properties, as an alternative to machined disks. If electrical
press. properties, discussed in the Appendix, are to be determined on
9.3.2.2 Apply an initial pressure of 3.45 MPa [500 psi] tape, Sections II and III must be left together in order that a
610 % and hold for 1 to 2 min. Increase the pressure smoothly tape of sufficient width is obtained to allow the cutting of a
to the final preforming pressure in 3 to 5 min. Do not allow the 50.8-mm [2-in.] diameter electrical test specimen.
mold shell to contact either press platen at any time during this 9.4 Conditioning Test Specimens:
preforming step. The final pressure attained, if not recom- 9.4.1 For tests of tensile properties and all tests requiring the
mended by the manufacturer of the particular material, shall be measurement of specific gravity condition the test specimens in

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 D 4894 – 07
between the initial and second melting peak temperatures is
greater than 5°C [9°F], as seen in Table 1. If peak temperatures
are difficult to discern from the curves, that is, if the peaks are
rounded rather than pointed, straight lines shall be drawn
tangent to the sides of the peak. Where these lines intersect
beyond the peak shall be taken as the peak temperature. Where
more than one peak occurs during the initial melting test, the
presence of any peak corresponding to the second melting peak
temperature indicates the presence of some previously melted
material.
10.2 Bulk Density:
10.2.1 Significance and Use—Bulk density gives some
indication of how a resin will perform during feeding of
molding and ram extrusion equipment. PTFE resins have a
tendency to compact during shipment and storage, and even
though the material is broken up by screening or some other
means, original “as produced” results are not guaranteed.
Because of this tendency to pack under small amounts of
FIG. 5 Melting Characteristics by Thermal Analysis compression or shear, Test Method D 1895 is not applicable to
these resins. The procedure given in the following paragraphs
must be used to measure this property.
general accordance with Procedure A of Practice D 618, with 10.2.2 Apparatus:
the following deviations therefrom: a) the aging period shall be 10.2.2.1 Funnel—A funnel arrangement as shown in Fig. 6.
a minimum of 4 h immediately prior to testing, b) the 10.2.2.2 Feeder 5—A feeder with a No. 8 wire screen placed
laboratory temperature shall be 23 6 2°C [73.4 6 3.6°F], and over approximately the top two-thirds of the trough. The funnel
c) there shall be no requirement respecting humidity. The other shall be mounted permanently in the feeder outlet.
tests require no conditioning of the molded test specimens. 10.2.2.3 Controller 6
9.5 Test Conditions: 10.2.2.4 Volumetric Cup and Cup Stand (Fig. 7)—The
9.5.1 Tests shall be conducted at the standard laboratory volumetric cup shall be calibrated initially to 250 mL by filling
temperature of 23 6 2°C [73.4 6 3.6°F]. See Note 5 for it with distilled water, placing a planar glass plate on top,
additional details. Since these resins do not absorb water, the drying the outside of the cup, and weighing. The net weight
maintenance of constant humidity during testing is not re- shall be 250 6 0.5 g. The top and bottom faces of the
quired. volumetric cup and the cup stand shall be machined plane and
parallel.
10. Test Methods 10.2.2.5 Leveling Device—The leveler (Fig. 8) shall be
10.1 Melting Characteristics by Thermal Analysis: affixed permanently to the table and adjusted so that the
10.1.1 Significance and Use—Most of the PTFE resins that sawtooth edge of the leveler blade passes within 0.8 mm [1⁄32
fall within the scope of this specification have never been in.] of the top of the volumetric cup.
melted (the only exception is Type V resin). These resins have 10.2.2.6 Work Surface—The work surface for holding the
higher melting peak temperatures on initial melting than on volumetric cup and leveler shall be essentially free from
second or subsequent meltings. Since PTFE resins that have vibration. The feeder, therefore, must be mounted on an
been melted prior to use behave differently from those that adjoining table or wall bracket.
have not, the melting characteristics of resins provide impor- 10.2.2.7 Balance—The balance having an extended beam
tant distinctions among them. Melting peak temperatures (see shall have a capacity of 500 g and a sensitivity of 0.1 g or
Fig. 5) are used to make these distinctions, and determine equivalent.
conformance of a resin to the melting peak temperature 10.2.3 Procedure:
requirements given in Table 1 of this specification. A resin that 10.2.3.1 Place the clean, dry volumetric cup on the extended
has been melted is not compatible with this specification, beam of the balance and adjust the tare to zero. Select about
except for Type V. 500 mL of the resin to be tested, place it on the feeder screen
10.1.2 Apparatus—Use apparatus described in Test Method and vibrate all of the resin through the screen and back into the
D 4591. sample container twice to break up any lumps. Put the cup in
10.1.3 Procedure: the cup stand and place the assembly such that the distance of
10.1.3.1 Measure melting peak temperatures in accordance free polymer fall from the feeder outlet to the top rim of the cup
with the procedures given in Method D 4591. An initial
melting peak temperature above the melting peak temperature
5
obtained on the second and subsequent melting (defined as the A “Vibra-Flow” Feeder, Type FT01A, Available from FMC Corporation,
Material Handling Division, FMC Building, Homer City, PA 15748, has been found
second melting peak temperature) indicates that the resin was satisfactory for this purpose.
not melted before the test. The second melting peak tempera- 6
A “Syntron” controller, Type SCR1B, available from FMC Corporation,
ture occurs at about 327°C [621°F]. Usually the difference address as shown in footnote 12, has been found satisfactory for this purpose.

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 D 4894 – 07

FIG. 6 Details of Funnel for Bulk Density Test

FIG. 7 Volumetric Cap and Cap Stand for Bulk Density Test

shall be 38.1 6 3.2 mm [11⁄2 6 1⁄8 in.]. Increased fall causes 10.2.5 Precision and Bias—A precision statement for use
packing in the cup and higher Bulk Density values. Set the with this procedure is under development. The procedure in
controller so that the cup is filled in 20 to 30 s. Pour the sample this test method has no bias because the value of bulk density
on the vibrating screen and fill the cup so that the resin forms is defined only in terms of a test method.
a mound and overflows. Let the resin settle for about 15 s and 10.3 Particle Size:
then gently push the cup and its stand beneath the leveler. 10.3.1 Significance and Use—The fabrication of PTFE
Exercise care to avoid agitation of the resin and cup before resins either by molding or extrusion is affected significantly
leveling. Weigh the resin to the nearest 0.1 g. by particle (or agglomerate) size and size distribution. (See
10.2.4 Calculation—Calculate the bulk density as follows: Appendix X1. for further details on particle characteristics.)
Grams of resin345bulk density ~grams per litre! The average particle size of PTFE resins is determined by

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 D 4894 – 07

FIG. 8 Leveler Stand for Bulk Density Test

fractionation of the material with a series of sieves. Fraction- 10.3.4.3 Remove the top sieve and place it in the hood to
ation is facilitated by spraying with perchloroethylene which dry.
breaks up lumps and prevents clogging of the sieve openings. 10.3.4.4 Repeat the procedure specified in 10.3.4.2 and
Warning—Perchloroethylene is under investigation by gov- 10.3.4.3 until all the sieves have been sprayed. Air-dry the
ernment agencies and industry for its carcinogenic effects. sieves in the hood for 30 min or longer, or oven-dry at 90°C
Protective nitrile or butyl gloves shall be worn to prevent skin [194°F] for 15 min and then cool to room temperature. Remove
contact and adequate ventilation provided to remove the the resin from each sieve by tapping on a piece of paper as
vapors. shown in Fig. 9 (b). Pour each fraction into a tared beaker and
NOTE 8—Caution:
weigh to 60.1 g (See Note 9).
10.3.4.5 Record the weight of resin on each sieve.
10.3.2 Apparatus: 10.3.4.6 Clean the sieve by inverting it over filter paper and
10.3.2.1 Balance—capable of weighing to 60.1 g. spraying with perchloroethylene. Take care to prevent the resin
10.3.2.2 Sieves—U.S. Standard Sieve Series, 203-mm from getting into the perchloroethylene.
[8-in.] diameter conforming to Specification E 11. Sieve Num-
10.3.5 Calculation—Calculate the net percentage of resin
bers shall be selected from Table 4.
on each sieve as follows:
10.3.2.3 Ventilated Hood.
10.3.2.4 Beakers—Six tared, 150-mL beakers. Net percentage on sieve Y
5 F 3 weight of resin in grams on sieve Y.
NOTE 9—As an alternative, sieves are tared, dried, and weighed on a
balance to avoid transferring of fractionated samples to the tared beakers.
where:
10.3.2.5 Apparatus for Sieving and Spraying—A suggested
F = 2 for 50-g sample, and
arrangement of an apparatus for recirculating perchloroethyl- F = 10 for 10-g sample.
ene is shown in Fig. 9 (a). This must be located in a ventilated
10.3.5.1 Calculate the cumulative percentage of resin on
hood or adequately ventilated area.
each sieve as follows:
10.3.3 Reagents—Perchloroethylene, 20 L [5 gal]. The use
of other liquids, their applicability and hazards associated with Cumulative percentage on sieve Y 5 sum of net percentages on sieve Y
and sieves having numbers smaller than Y.
their use must be thoroughly investigated.
10.3.4 Procedure:
10.3.4.1 Select the appropriate sample size and combination NOTE 10—Example—Cumulative percentage on 500 µm (No. 35) sieve
of sieves from Table 4 for the type of resin under test. Adjust for a Type V resin = net percentage on 1.00 mm (No. 18) plus net
the flow rate of the perchloroethylene to 6 6 0.5 L/min. percentage on 710 µm (No. 25) plus net percentage on 500 µm (No. 35)
sieves.
10.3.4.2 Place the weighed resin on the top sieve and spray
it with perchloroethylene for 1 6 0.2 min. The shower-head 10.3.5.2 Plot the cumulative percentage versus the sieve
shall be about level with the top of the sieve and be moved in opening size (or sieve number) on log-probability paper as
a circular fashion. Take care to break up all of the lumps and shown in the sample plot (Fig. 10). The sieve numbers and
to wash the material from the sides of the sieve. sieve opening sizes in micrometres are indicated below the

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 D 4894 – 07
TABLE 4 Sieving RequirementsA
Type
Sieve Number (opening)
I IIB III 1B III 2 IV V VI
14 (1.40 mm) X X X X
18 (1.00 mm) X X X X X
25 (710 µm) X X X X X X X
35 (500 µm) X X X X X
45 (355 µm) X X X X X
60 (250 µm) X X X X
80 (180 µm) X X X X X
120 (125 µm) X
170 (90 µm) X X
200 (75 µm) X X
230 (63 µm) X X
270 (53 µm) X X
325 (45 µm) X X
400 (38 µm) X X X
Sample size, g
10 6 0.1 X X
50 6 0.1 X X X X X
A
It is suggested that the sieves and sample size checked in a “Type Grade”
column be used when performing the sieve analysis on that particular type grade.
B
A discussion of the particular characteristics of finely divided resins is found in
Appendix X1.

Sieve. Sieve Opening, µm Sieve Sieve Opening, µm

No. No.
FIG. 9 Apparatus for Particle Size Test 14 1400
18 1000 80 180
25 710 120 125
figure. Draw the best straight line through the points and read 35 500 170 90
45 355 200 75
the Particle Size at the 50 % cumulative percentage point (d50). 60 250 230 63
10.3.5.3 Calculate the Particle Size, Average Diameter, 270 53
d as follows: 325 45
400 38
d = d50 (micrometres)
10.3.6 Precision and Bias: FIG. 10 Sample Plot of Cumulative Percent Versus Sieve
10.3.6.1 Because the resin particles have complex shapes, Opening Size for Determination of Particle Size
and because on each sieve there is a distribution of particle
sizes, the values for particle size and particle size distribution
obtained will be only relative numbers. The 95 % confidence stable and that have regular spherical type shape particles.
limits based on a limited series of tests are 62.8 % for the Also, it is recommended that each manufacturing processor do
average particle size. Since there is no accepted reference an analysis to determine their own correlation.
material suitable for determination of the bias for this test 10.4 Water Content:
procedure, no statement on bias is being made. 10.4.1 Significance and Use—The presence of an excessive
10.3.7 Alternative methods for particle size are available. amount of water in PTFE resin has a significant adverse effect
Light Scattering Instruments/Light Defraction Instruments (see upon the processing characteristics of the resin and the quality
ISO 12086-2, 8.6.4) and Electron Zone Sensing Instruments, of products made using the resin. A sample of PTFE resin of
which is a resistance-variation tester, (see ISO 12086-2, 8.6.3) known weight is dried in a vacuum oven in a tared aluminum
are used as long as there is a direct correlation to the Particle weighing dish. When the resin is dry, it is removed from the
Size Analysis in 10.3 of this specification. oven, placed in a desiccator, allowed to cool, and then
10.3.7.1 This alternative method is very dependent on reweighed. Water content is calculated from the weight lost
particle shape and is only recommended for processes that are during drying.

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 D 4894 – 07
10.4.2 Apparatus: 10.5.2.3 If specimens from 9.3.3.1 are to be tested, use the
10.4.2.1 Balance, capable of weighing to the nearest 0.0001 center portion of the sintered billet (Section II of Fig. 4). From
g. it, cut an approximately cubical shape which weighs at least 10
10.4.2.2 Vacuum Oven. g [for example, a cube about 17 mm [0.67 in.] on a side].
10.4.2.3 Aluminum Weighing Dishes, with lids. 10.5.2.4 Make specific gravity determinations in accordance
10.4.3 Procedure (Note 11): with the procedures described in Test Methods D 792, Method
A-1. Add two drops of a wetting agent7 to the water in order to
10.4.3.1 Wash the aluminum weighing dishes with water
reduce the surface tension and ensure complete wetting of the
and rinse with acetone. When the acetone has evaporated from
specimen.
the dishes, dry them thoroughly in an oven at 50 to 80°C [122
10.6 Thermal Instability Index (TII):
to 176°F], then store in a desiccator until ready for use. Obtain
10.6.1 Significance and Use—This test method compares
the tare weight, B, of an aluminum weighing dish, plus lid, to
the SSG of a resin (determined in 10.5) to its Extended Specific
the nearest 0.0001 g. Place 35 to 40 g of PTFE resin in the tared
Gravity (ESG) (determined here). Specimens used to deter-
aluminum weighing dish and record the weight (including lid),
mine ESG are identical to those used to determine SSG, except
A, to the nearest 0.0001 g (Note 11). Dry to constant weight in
for the differences in thermal history described in 9.2.3 and
a vacuum oven (635 mm [25 in.] Hg) at 150°C [302°F], with
9.3.3. The specific gravity of a specimen prepared in accor-
the dish lid removed. Remove the dish from the oven, replace
dance with all of the requirements of 9.2.3.2 or 9.3.3.2 defines
the lid on the weighing dish, and allow to cool in the desiccator
the ESG for that resin specimen.
for at least 30 min. Reweigh the dish (plus the resin and lid),
10.6.2 Procedure:
C, and calculate the weight loss.
10.6.2.1 Determine, in accordance with 10.5.2.4, the spe-
NOTE 11—Select one sample from each group of samples and run cific gravity of specimens prepared in 9.2.3.2 or 9.3.3.2.
duplicate water content determinations on it. If the difference between the 10.6.2.2 If specimens from 9.2.3.2 are to be tested, use them
duplicate results exceeds 0.01 %, the entire group of samples must be run as is.
over.
10.6.2.3 If specimens from 9.3.3.2 are to be tested, use the
NOTE 12—When a group of samples is run at the same time, it is good
center portion of the billet (Section III of Fig. 4).
practice to place the lids from the weighing dishes directly under their
corresponding dishes while the samples are drying in the oven. This 10.6.3 Calculation—Calculate the thermal instability index
eliminates the possibility of introducing errors in the tare weights. Also, (TII) as
overnight drying in a circulating air oven is used if the data are shown to TII 5 ~ESG 2 SSG! 3 1000
be equivalent to those obtained with the above procedure.
10.4.4 Calculation: 10.7 Tensile Properties:
10.4.4.1 Calculate the water content as follows: 10.7.1 Procedure:
water content, % 5 ~A 2 C!/~A 2 B! 3 100 10.7.1.1 Cut five tensile specimens from a disk prepared in
accordance with all of the requirements of 9.1.3.1 (or from a
billet prepared in accordance with all of the requirements of
where: 9.3.3.1 and cut or skived as in 9.3.4), with the microtensile die
A = weight of resin, dish, and lid, g, before drying described in Fig. 11. Determine the tensile strength in accor-
B = weight of dish and lid, g and, dance with the procedures described in Test Method D 638,
C = weight of resin, dish, and lid after drying, g. except that the initial jaw separation shall be 22.2 6 0.13 mm
10.4.5 Precision and Bias: [0.875 6 0.005 in.], and the speed of testing shall be 50 mm [2
10.4.5.1 The precision of this test is 60.0063 % (two sigma in.]/min. Clamp the specimen with essentially equal lengths in
limits). Since there is no accepted reference material for each jaw. Determine elongation at break from the chart,
determining the bias in this test procedure, no statement on bias expressed as a percentage of the initial jaw separation.
is being made. 10.7.2 Precision and Bias:
10.5 Standard Specific Gravity (SSG): 10.7.2.1 A precision and bias statement for use with this
10.5.1 Significance and Use—The specific gravity of an procedure is under development and will be included when it
article made from a PTFE resin is affected both by the has been approved by the balloting process.
particular resin used and by the way the resin is processed.
Therefore, a test method that measures the specific gravity of 11. Inspection and Certification
an article prepared in a precisely defined way provides valuable 11.1 Inspection and certification of the material supplied
resin characterization data. The specific gravity of a specimen with reference to this specification shall be for conformance to
of PTFE resin prepared in accordance with all of the require- the requirements specified herein.
ments of 9.2.3.1 or 9.3.3.1 defines the SSG for that resin 11.2 Lot-acceptance inspection shall be the basis on which
specimen. acceptance or rejection of the lot is made. The lot-acceptance
10.5.2 Procedure: inspection shall consist of the following:
10.5.2.1 Determine, in accordance with 10.5.2.4, the spe-
cific gravity of specimens prepared in 9.2.3.1 or 9.3.3.1.
10.5.2.2 If specimens from 9.2.3.1 are to be tested, use them 7
Examples of suitable wetting agents are “Glim” detergent, B. J. Babbitt, Inc.;
as is. “Joy” detergent, Proctor and Gamble, Inc.; and “Triton” X-100, Rohm and Haas Co.

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 D 4894 – 07

FIG. 11 Microtensile Die

11.2.1 Bulk density, 11.4 Certification shall be that the material was manufac-
11.2.2 Particle size, tured by a process in statistical control, sampled, tested, and
11.2.3 Water content, and inspected in accordance with this classification system, and
11.2.4 Standard Specific Gravity. that the average values for the lot meet the requirements of the
11.3 Periodic check inspection with reference to a specifi- specification (line callout).
cation shall consist of the tests for all requirements of the 11.5 A report of test results shall be furnished when re-
material under the specification. Inspection frequency shall be quested. The report shall consist of results of the lot-acceptance
adequate to ensure the material is certifiable in accordance with inspection for the shipment and the results of the most recent
11.4. periodic-check inspection.

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 D 4894 – 07
12. Packaging and Package Marking 12.3 All packing, packaging, and marking provisions of
12.1 Packaging—The resin shall be packaged in standard Practice D 3892 shall apply to this specification.
commercial containers so constructed as to ensure acceptance
by common or other carriers for safe transportation to the point 13. Keywords
of delivery, unless otherwise specified in the contract or order. 13.1 fluoropolymers; granular polytetrafluoroethylene;
12.2 Package Marking—Shipping containers shall be polytetrafluoroethylene; PTFE
marked with the name of the resin, type, and quantity contained
therein.

SUPPLEMENTARY REQUIREMENTS

The following supplementary requirements shall apply only when specified by the purchaser in the
contract or order.

S1. Ordering Information—The purchase order shall state

this ASTM designation and year of issue, and which type and
grade is desired.

APPENDIX

(Nonmandatory Information)

X1. ADDITIONAL USEFUL TESTS

TABLE X1.1 D 150 Test Methods for A-C Loss Characteristics and Per-
Specification
Specification Property
mittivity (Dielectric Constant) of Solid Electrical Insulating
Test Additional Information Available Materials
Measured
Reference
D 2990 Test Methods for Tensile, Compressive, and Flex-
10.5 Standard Specific Dimensional change during molding
Gravity (shrinkage and growth) ural Creep and Creep-Rupture of Plastics
10.1 Melting Characteristics Heats of fusion and crystallization D 3293 Specification for PTFE Resin Molded Sheet8
by Thermal Analysis
10.3 Particle Size (a) Average Particle Size for resins
D 3294 Specification for PTFE Resin Molded Basic
smaller than those covered by the Shapes8
standard specification D 3308 Specification for PTFE Resin Skived Tape8
(b) Percent coarse particles (percent
>63 µm) in small particle size resins D 3369 Specification for TFE-Fluorocarbon Resin Cast
10.7 Tensile Properties Yield stress and tangent modulus at Film8
rupture
Electrical Properties:
Dielectric constant X1.3 Dimensional Changes During Molding (Shrinkage
Dissipation factor and Growth)
Dielectric breakdown voltage
Dielectric strength X1.3.1 Measure the inside diameter (ID) to 60.00254 mm
Tensile creep strain [0.0001 in.] of the die used to make the preform in 9.1, 9.2, or
9.3. Measure the diameter and height at the preform. After the
piece has been sintered and cooled to ambient temperature,
X1.1 Scope measure the diameter and height of the sintered piece.
X1.1.1 In addition to their use for specification purposes, X1.3.2 Calculation:
the tests described in this specification have utility for charac- X1.3.2.1 Percent mold shrinkage = [(diameter of sintered
terizing PTFE resins. Other useful properties of PTFE can be piece/ID) − 1] 3 100
measured by adding a few details to the specification tests. The X1.3.2.2 Percent preform shrinkage = [(diameter of sintered
purpose of this Appendix is to provide the details needed to piece/diameter of preform) − 1] 3 100
determine these additional characteristics. The scope is sum- X1.3.2.3 Percent growth = [(height of sintered piece/height
marized in Table X1.1. of preform) − 1] 3 100
X1.2 Referenced Documents
X1.2.1 ASTM Standards:
X1.2.1.1 The following standards are referenced herein, in 8
Specifications for other forms of polytetrafluoroethylene may be found in
addition to those already listed in Section 1.1 of the Standard: Specifications D 4441 and D 4895.

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 D 4894 – 07
X1.3.2.4 Positive values reflect an increase in the dimension diameter ( d ) plus 1 sigma and ( d ) minus 1 sigma. Calculate
during sintering. Negative values reflect a decrease in the a distribution factor (DF) and skewness (SKEW) as follows:
dimension during sintering. DF 5 d16/d50

X1.4 Size and Distribution of Size of Particles or SKEW 5 DF/~d50/d84!

Agglomerates in PTFE Resins
X1.4.1 Average Size of Fine-Particle Size PTFE—Wet- X1.4.3.2 Precision and Bias—Because the resin particles
sieve analysis, while having disadvantages, can be used to have complex shapes, and because on each sieve there is a
measure the average size of Type II and Type III PTFE resins. distribution of particle sizes, the values for particle size and
The procedure of 10.3 shall be followed using the set of sieves particle size distribution obtained will be only relative num-
listed in Table 4 and a sample size of 10.0 g. bers. The 95 % confidence limits based on a limited series of
X1.4.2 Material Retained on 63-µm (No. 230) Sieve: tests are 62.8 % for the average particle size and 66 % for the
X1.4.2.1 Scope—A wet sieving is performed with the ap- particle size distribution function. Since there is no accepted
paratus used for the determination of particle size, except that reference material suitable for determination of the bias for this
only three sieves are employed. This method is applicable to test procedure, no statement on bias is being made.
ultrafine resins such as Type II resins. The resin is sieved on a
63 µm (No. 230) sieve by spraying with perchloroethylene X1.5 Yield Behavior and Tangent Modulus at Rupture
which breaks up agglomerates and prevents clogging of the X1.5.1 Most of the PTFE resins covered in this standard do
sieve openings (See Note 7). not show a yield stress as defined in Test Method D 638. Rather
X1.4.2.2 Apparatus—Same as in 10.3.2, except that the than the stress-strain curve having a zero slope, the rate of
following sieves are used: U.S. Standard Sieves, 850 µm (No. increase of stress with strain decreases and then increases
20), 63 µm (No. 230), and 45 µm (No. 325). again. An approximate yield stress shall be reported as the
X1.4.2.3 Procedure: stress at the intersection of the two lines that best represent the
X1.4.2.4 Weigh 10 6 0.01 g of resin. Assemble the sieves initial “linear” part of the stress strain curve and the second
as shown in Fig. 10 (a). Adjust the flow rate of the perchloro- “linear” part of the curve.
ethylene to 6 6 0.5 L/min. X1.5.2 Tangent Modulus at Rupture—The shapes of tensile
X1.4.2.5 Place the weighed sample on the 850 µm (No. 20) stress-strain curves for PTFE resins are highly dependent on
sieve and spray with perchloroethylene for exactly 1 min using the crystallinity of the test specimen. Values for tensile strength
a timer. This step assists in breaking up agglomerates. Move and elongation at break do not reflect these shapes clearly. The
the shower-head in a circular fashion, taking care to break up value of the tangent to the recorded stress-strain curve mea-
all the agglomerates and to wash the material from the sides of sured as the best straight line from the point of rupture back
the sieve. along the curve is a convenient measure of the relative
X1.4.2.6 Remove the 850 µm (No. 20) sieve and spray the crystallinity of the test specimen. High values for the tangent
63 µm (No. 230) sieve for exactly 6 min, using a timer. Wash modulus at rupture (>7.6 MPa [1200 psi]) indicate relatively
the material to the side of the sieve during the last minute. low crystalline contents. As the crystallinity increases, the
X1.4.2.7 Dry the sieve and retained resin in an oven for 20 tangent modulus at rupture decreases until it approaches zero at
min or longer at 80 to 120°C [176 to 248°F]. The No. 20 sieve high levels of crystallinity.
does not require drying.
X1.4.2.8 Remove the material from the 63 µm (No. 230) X1.6 Heats of Fusion and Crystallization
sieve by inverting on a piece of filter paper and tapping to free X1.6.1 If the melting characteristics of the PTFE resin, as
dry polymer. Use a stiff brush to help free all the material from determined by Section 10.1, are determined by differential
the sieve. Pour the dried resin into a tared weighing dish and scanning calorimetry (DSC) rather than in DTA mode, addi-
weigh to 60.01 g. Alternatively, determined the tare weight of tional quantitative information will be obtained on the nature of
the resin retained on the sieve from the difference between the the resin.
gross weight after sieving and the tare weight of the sieve X1.6.2 Following the procedures given in Test Method
before sieving. A balance with a sensitivity of about 0.01 g is D 4591 for determining heats of fusion (delta Hf) and heat of
required for good precision. crystallization (delta Hc), measure and report delta Hf for the
X1.4.2.9 Calculation—the percentage of resin retained on initial and second endotherms and delta Hc for the exotherm
the No. 230 sieve is calculated as follows: that is observed during controlled cooling between the two
Amount retained, % 5 ~weight retained/sample weight! 3 100 heating steps. These heats of transition, especially delta Hc,
provide additional characterization of crystalline content and
X1.4.3 Distribution of Particle or Agglomerate Sizes in relative molecular weight of PTFE resins.
PTFE Resin:
X1.4.3.1 Procedure—Using the graph plotted in accordance X1.7 Electrical Properties
with 10.3.5.2 or 10.3.5.3, draw the best smooth curve through X1.7.1 Determine dielectric constant and dissipation factor
the data points and read the values for the sizes at cumulative in accordance with Test Method D 150. Determine dielectric
percentages of 16 and 84. These values, identified as d16 and breakdown voltage and dielectric strength in accordance with
d84, are, respectively, the size of the resin at the average Test Method D 150. Typical property values for dielectric

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 D 4894 – 07
TABLE X1.2 Typical Electrical Properties from Tests on Molded accordance with Test Method D 2990. Conditions of test shall
Specimens be 5.52 MPa [800 psi] stress at the Standard Laboratory
Type II Type III Temperature of 23 6 2°C [73.4 6 3°F] for a test duration of a
Dielectric constant, max, 1 kHz 2.1 2.1 minimum of 100 h. Typical values for moldings of Type III
Dissipation factor, max, 1 kHz 0.0003 0.0003 resins would be a maximum of 4.0 % tensile creep strain after
100 h.
X1.8.2 Mold test sheets for Type III resins for tensile creep
constant and dissipation factor are listed in Table X1.2. measurements in a picture frame mold having inside dimen-
Standards for dielectric strength of sheet, basic shapes, skived sions of 203 mm [8.0 in.] square and of sufficient height to
tape, and film are described in Specifications D 3293, D 3294, contain the sample. A frame 102 mm [4 in.] in height has been
D 3308, and D 3369, respectively. found adequate when using 25-mm [1-in.] thick pusher plugs
to produce a sheet approximately 3 mm [1⁄8 in.] in thickness
X1.8 Tensile Creep from a resin charge of 300 g. Take care to level the resin charge
X1.8.1 Determine the tensile creep of Type III materials on in the mold. The molded sheet thickness shall be 3 mm [1⁄8 in.].
Test Method D 638 Type II tensile bars die cut or machined X1.8.3 Sinter the preform in accordance with procedure E
from the sheets produced in X1.8.2. Make measurements in of Table 3.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D 4894 - 04) that may impact the use of this standard. (September 1, 2007)

(1) Expanded ranges of Bulk Density from 850 6 50 to 850 6 (4) Expanded ranges of Initial Melting Peak Temperature from
100 of Type III Grade 2 in Table 1. 335°C to >5°C above the second melting point temperature,
(2) Expanded ranges of Particle Size from 500 6 100 to 500 and expand Second Melting Peak Temperature from 327 6
6 150 of Type III Grade 2 in Table 1 for adding new material. 5°C to 327 6 10°C of Type VI in Table 1 to represent
(3) Expanded ranges of Initial Melting Peak Temperature from commercial material.
335°C to >5°C above the second melting point temperature, (5) Added Sieving Requirements of Type III Grade 2 and Type
and expand Second Melting Peak Temperature from 327 6 VI to Table 4.
5°C to 327 6 10°C of Type III Grade 2 in Table 1 for adding
new material.

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

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