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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: D4895 − 18

Standard Specification for

Polytetrafluoroethylene (PTFE) Resin Produced From
Dispersion1
This standard is issued under the fixed designation D4895; 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

2
1.1 This specification covers polytetrafluoroethylene 2.1 ASTM Standards:3
(PTFE) prepared by coagulation of a dispersion. These PTFE D618 Practice for Conditioning Plastics for Testing
resins are homopolymers of tetrafluoroethylene or modified D638 Test Method for Tensile Properties of Plastics
homopolymers containing not more than 1 % by weight of D792 Test Methods for Density and Specific Gravity (Rela-
other fluoromonomers. The materials covered herein do not tive Density) of Plastics by Displacement
include mixtures of PTFE with additives such as colors, fillers, D883 Terminology Relating to Plastics
or plasticizers; nor do they include reprocessed or reground D1708 Test Method for Tensile Properties of Plastics by Use
resin or any fabricated articles because the properties of such of Microtensile Specimens
materials have been irreversibly changed when they were D1895 Test Methods for Apparent Density, Bulk Factor, and
fibrillated or sintered. Pourability of Plastic Materials
D3892 Practice for Packaging/Packing of Plastics
1.2 The values stated in SI units as detailed in IEEE/ASTM
D4052 Test Method for Density, Relative Density, and API
SI-10 are to be regarded as standard. The values given in
Gravity of Liquids by Digital Density Meter
parentheses are for information only.
D4441 Specification for Aqueous Dispersions of Polytetra-
1.3 The following safety hazards caveat pertains only to the fluoroethylene
Specimen Preparation Section, Section 9, and the Test Methods D4591 Test Method for Determining Temperatures and
Section, Section 10, of this specification: This standard does Heats of Transitions of Fluoropolymers by Differential
not purport to address all of the safety concerns, if any, Scanning Calorimetry
associated with its use. It is the responsibility of the user of this D4894 Specification for Polytetrafluoroethylene (PTFE)
standard to establish appropriate safety and health practices Granular Molding and Ram Extrusion Materials
and determine the applicability of regulatory limitations prior E11 Specification for Woven Wire Test Sieve Cloth and Test
to use. See Warning note in 9.1.1 for a specific hazards Sieves
statement. E29 Practice for Using Significant Digits in Test Data to
NOTE 1—Information in this specification is technically equivalent to Determine Conformance with Specifications
related information in ISO 20568-1 and ISO 20568-2. E177 Practice for Use of the Terms Precision and Bias in
1.4 This international standard was developed in accor- ASTM Test Methods
dance with internationally recognized principles on standard- IEEE/ASTM SI-10 Use of the International System of Units
ization established in the Decision on Principles for the (SI): The Modern Metric System
Development of International Standards, Guides and Recom- 2.2 ISO Standards:4
mendations issued by the World Trade Organization Technical ISO 20568-1 Plastics Fluoropolymer Dispersions and Mold-
Barriers to Trade (TBT) Committee. ing and Extrusion Materials—Part 1: Designation and
Specification
ISO 20568-2 Plastics Fluoropolymer Dispersions and
Molding and Extrusion Materials—Part 2: Preparation of
1
This specification is under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic
3
Materials. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2018. Published November 2018. Originally contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
approved in 1989. Last previous edition approved in 2016 as D4895 – 16. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4895-18. the ASTM website.
2 4
Specifications for other forms of polytetrafluoroethylene are found in Specifi- Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
cations D4441 and D4894. 4th Floor, New York, NY 10036, http://www.ansi.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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D4895 − 18
Test Specimens and Determination of Properties 4. Classification
ISO 13322-2 Particle size analysis—Image analysis 4.1 This specification covers the following types of PTFE:
methods—Part 2: Dynamic image analysis methods 4.1.1 Type I and Type II—Resin produced from dispersion.
3. Terminology Each type of resin has the same requirements for bulk density,
particle size, water content, melting peak temperature, tensile,
3.1 Definitions—The definitions given in Terminology
and elongation. Each type of resin is divided into grades in
D883 are applicable to this specification.
accordance with standard specific gravity (SSG), Thermal
3.2 Definitions of Terms Specific to This Standard: Stability Index (TII), and Stretching Void Index (SVI). Grades
3.2.1 bulk density, n—the mass in grams per litre of resin are divided into classes according to extrusion pressure.
measured under the conditions of the test.
NOTE 2—See Tables 1 and 2 for details about grades and classes.
3.2.2 extended specific gravity (ESG), n—the specific grav-
ity of a specimen of PTFE material molded as described in this 4.2 A line callout system is used to specify materials in this
specification and sintered (see 3.2.7) for an extended period of specification. The system uses predefined cells to refer to
time, compared to the sintering time for the measurement of specific aspects of this specification, as illustrated as follows:
SSG (see 3.2.8), using the appropriate sintering schedule given
in this specification.
3.2.3 lot, n—one production run or a uniform blend of two Specification
or more production runs.
Standard Number Type Grade Class Special Notes
3.2.4 preforming, vb—compacting powdered PTFE material Block
under pressure in a mold to produce a solid object, called a
preform, that is capable of being handled. Molding and | | | | |
Example: Specification I 2 C
compaction are terms used interchangeably with preforming D4895 - XX
for PTFE.
3.2.5 reground resin, n—resin produced by grinding PTFE
material that has been preformed but has never been sintered.
For this example, the line callout would be Specification
3.2.6 reprocessed resin, n—resin produced by grinding D4895 - XX, I2C, and would specify a coagulated dispersion
PTFE material that has been preformed and sintered. form of polytetrafluoroethylene that has all of the properties
3.2.7 sintering, n—as it applies to PTFE, a thermal treat- listed for that type, grade, and class in the appropriate specified
ment during which the PTFE is melted and recrystallized by properties or tables, or both, in the specification identified. A
cooling with coalescence occurring during the treatment. comma is used as the separator between the standard number
3.2.8 standard specific gravity (SSG), n—the specific grav- and the type. Separators are not needed between the type,
ity of a specimen of PTFE material molded as described in this grade, and class.5
specification and sintered using the appropriate sintering
schedule given in this specification. 5. Mechanical Properties
3.2.9 strained specific gravity (strained SG), n—the specific 5.1 The resins covered by this specification shall be in
gravity of a specimen of PTFE material molded, sintered, and accordance with the requirements prescribed in Tables 1 and 2,
strained as described in this specification. when tested by the procedures specified herein.
3.2.10 stretching void index (SVI), n—a measure of the
change in specific gravity of PTFE material which has been 6. Other Requirements
subjected to tensile strain as described in this specification. 6.1 The resin shall be uniform and shall contain no additives
3.2.11 thermal instability index (TII), n—a measure of the or foreign material.
decrease in molecular weight of PTFE material which has been 6.2 The color of the material as shipped by the supplier shall
heated for a prolonged period of time. be natural white.
3.2.12 unstrained specific gravity (USG), n—the specific
gravity, prior to straining, of a specimen of PTFE material used
in the Stretching Void Index Test (see 10.9) of this specifica- 5
See the Form and Style for ASTM Standards manual, available from ASTM
tion. Headquarters.

TABLE 1 Detail Requirements for all Types,A Grades and Classes

Particle Size Melting Peak
Bulk Density, Water Content, Temperature, °C Tensile Strength, Elongation at Break,
Type Average
g/L max, % min, MPa min, %
Diameter, µm Initial Second
B
I 550 ± 150 500 ± 200 0.04 327 ± 10 19 200
B
II 550 ± 150 1050 ± 350 0.04 327 ± 10 19 200
A
The types, grades, and classes are not the same as those in previous editions of Specification D4895.
B
Greater than 5.0°C above the second melting peak temperature.

2
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D4895 − 18
TABLE 2 Detail Requirements for All Types,A Grades and Classes
Standard Specific Gravity Thermal Instability Index, Stretching Void Index,
Type Grade Class Extrusion Pressure, MPa
min max max max
I 1 A 2.14 2.18 5 to <15B 50 NAC
B 2.14 2.18 15 to <55D 50 NAC
C 2.14 2.18 15 to <75E 50 NAC
2 A 2.17 2.25 5 to <15B 50 NAC
B 2.17 2.25 15 to <55D 50 NAC
C 2.17 2.25 15 to <75E 50 NAC
3 C 2.15 2.19 15 to <75E 15 200
D 2.15 2.19 15 to <65E 15 100
E 2.15 2.19 15 to <65E 50 200
4 B 2.14 2.16 15 to <55D 15 50
II 1 A 2.14 2.25 5 to <15B 50 NAC
A
The types, grades, and classes are not the same as those in previous editions of Specification D4895.
B
Tested at a reduction ratio of 100:1 (reduction ratio is the ratio of the cross-sectional area of the preform to the cross-sectional area of the die).
C
Not applicable.
D
Tested at a reduction ratio of 400:1.
E
Tested at a reduction ratio of 1600:1.

6.3 For purposes of determining conformance, all specified NOTE 3—For maximum precision, these weighing and preforming
limits for this classification system are absolute limits, as operations 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
defined in Practice E29. performed at temperatures below 21°C (70°F) due to the crystalline
6.3.1 With the absolute method, an observed value is not transition that occurs in PTFE in this temperature region which leads to
rounded, but is to be compared directly with the limiting value. possible cracks in sintered specimens and differences in specimen density
Example: In Table 2 Type I, Grade 4, Class B, under Specific (as well as changes in other physical properties). Problems caused by the
Gravity, 2.14 shall be considered as 2.140000 and 2.16 shall be effect of temperature on the specific gravity or density of PTFE shall be
minimized when the measurement is made using immersion procedures if
considered 2.160000. a sensitive thermometer (for example, one reading 6 0.1°C) is used in the
liquid and the temperature is adjusted to be at least 22°C.
7. Sampling
9.1.2 Screen 14.5 g of PTFE resin through a No. 10 sieve
7.1 Sampling shall be statistically adequate to satisfy the into the die. Adjust the lower plug height to allow the resin in
requirements in Section 11. the die can be leveled by drawing a straightedge in contact with
the top of the die across the top of the die cavity. Insert the die
8. Number of Tests
in a suitable hydraulic press and apply pressure gradually (see
8.1 Lot inspection shall include tests for bulk density, Note 4) until a pressure of 14 MPa (2030 psi) is attained. Hold
particle size, and extrusion pressure. Periodic tests shall consist this pressure for 3 min. Remove the disk from the die. Write the
of all the tests specified in Tables 1 and 2 and shall be made at sample identification number on the preform using an appro-
least once per year. priate marker that will not affect the PTFE during sintering.
8.2 The tests listed in Tables 1 and 2, as they apply, are NOTE 4—As a guide, increasing the pressure at a rate of 3.5 MPa (500
sufficient to establish conformity of a material to this specifi- psi)/min is suggested until the desired maximum pressure is attained.
cation. One set of test specimens as prescribed in Section 9
9.1.3 Place the sintering oven in a laboratory hood (or equip
shall be considered sufficient for testing each sample. The
it with an adequate exhaust system) and sinter the preforms in
average of the results for the specimens tested shall conform to
accordance with Table 3, Procedure A (see Note 5).
the requirements of this specification.
NOTE 5—Although the rate of heat application is not critical, the
9. Specimen Preparation cooling cycle is most important and the conditions cited in this procedure
must be followed very closely. If they are not followed, the crystallinity of
9.1 Test Disks for Tensile Properties: the disks and the resulting physical properties will be markedly changed.
9.1.1 Use the die shown in Fig. 1 for the molding of test Therefore, the use of a programmed oven is recommended for the most
disks (see Note 2). Place flat aluminum disks, 0.1 to 0.4 mm precise sintering cycle control and the hood window shall be left down
(0.004 in. to 0.016 in.) thick and 76 mm (3 in.) in diameter, on during the entire sintering procedure, the latter being an important safety
consideration.
both sides of the resin. The test resin shall be near ambient
temperature prior to molding (see Note 3). (Warning—PTFE 9.2 Test Specimens for Standard Specific Gravity and Ther-
resins can evolve small quantities of gaseous products when mal Instability Index:
heated above 204°C (400°F). Some of these gases are harmful. 9.2.1 A cylindrical preforming mold, 29-mm (1.14-in.) in-
Consequently, exhaust ventilation must be used whenever ternal diameter by at least 76 mm (3 in.) deep, is used to
these resins are heated above this temperature, as they are prepare the preforms. Clearance shall be sufficient to ensure
during the sintering operations that are a part of this specifi- escape of air during pressing. Place flat aluminum foil disks,
cation. Since the temperature of burning tobacco exceeds normally 0.13 mm (0.005 in.) thick and 29 mm (1.14 in.) in
204°C (400°F), those working with PTFE resins shall ensure diameter on both sides of the resin. The test resin shall be near
that tobacco is not contaminated.) ambient temperature prior to molding (see Note 3).

3
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D4895 − 18

NOTE 1—All dimensions are in millimetres.

FIG. 1 Mold Assembly for the Preparation of Specimens for the Determination of Tensile Properties

TABLE 3 Sintering Procedures 9.2.3.1 For SSG specimens use Procedure A.

A B 9.2.3.2 For ESG specimens use Procedure B.
Initial temperature, °C (°F) 290 (554) 290 (554)
Rate of heating, °C/h (°F/h) 120 ± 10 120 ± 10 NOTE 6—Improved precision in SSG and ESG test results has been
(216 ± 18) (216 ± 18) obtained with the use of an upright, cylindrical oven and an aluminum
Hold temperature, °C (°F) 380 ± 6 380 ± 6 sintering rack. The cylindrical oven has an inside diameter of 140 mm (5.5
(716 ± 10) (716 ± 10) in.) and an inside depth of 203 mm (8 in.) plus additional depth to
Hold time, min 30 + 2, −0 360 ± 5 accommodate a 51-mm (2-in.) thick cover, and is equipped with suitable
Cooling rate, °C/h (°F/h) 60 ± 5 60 ± 5
heaters and controllers to sinter specimens in accordance with the
(108 ± 9) (108 ± 9)
Second hold temperature, °C (°F) 294 ± 6 294 ± 6
procedures in Table 3. The rack, as shown in Fig. 2, allows preforms to be
(561 ± 10) (561 ± 10) placed symmetrically in the center region of the oven. Place six preforms
Second hold time, min 24 + 0.5, −0 24 + 0.5, −0 on each of the middle oven rack shelves (if six or fewer preforms are to
Period to room temperature, min $30 $30 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
oven load must be no less than 18 pieces including “dummies.” “Dum-
mies” are defined as normal 12-g specimens that have previously been
9.2.2 Weigh out 12.0 6 0.1 g of resin and place it in the die. through the sintering cycle. “Dummies” must only be used for an
Screen resins through a No. 10 sieve. Compacted resins shall additional two or three thermal cycles, due to eventual loss of thermal
be broken up by hand-shaking cold resin in a half-filled sealed stability and physical form.
glass container. Condition the resin in the sealed glass con- 9.2.4 Remove all flash from each specimen so that no air
tainer in a freezer or dry-ice chest. After breaking up resin bubbles will cling to the edges when the specimen is immersed
lumps, allow the sealed container to equilibrate to near ambient in the solution for weighing during the standard specific gravity
temperature. Then screen and weigh the 12.0 6 0.1-g sample. and thermal instability index tests. It is recommended for this
Insert the die in a suitable hydraulic press and apply pressure section and during testing that cotton gloves be worn while
gradually (see Note 4) until a pressure of 14 MPa (2030 psi) is handling test specimens.
attained. Hold this pressure for 2 min. Remove the preform
from the die. Write the sample identification number on the 9.3 Test Disks for Stretching Void Index (SVI):
preform using an appropriate marker that will not effect the 9.3.1 Mold the disk as in 9.1.1.
PTFE during sintering. 9.3.2 Screen 29 g of PTFE resin through a 2.00-mm (No.
9.2.3 Sinter the preforms in accordance with Table 3 (see 10) sieve into the die. Adjust the lower plug to allow the resin
Note 5). to be leveled by drawing a straightedge in contact with the top

4
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D4895 − 18
deviation from the standard laboratory temperature is made
because of the necessity for maintaining test temperatures
above approximately 21°C (70°F). See Note 3 for additional
details. Since these resins do not absorb water, the maintenance
of constant humidity during testing is not required.
10. Test Methods
10.1 Melting Characteristics by Thermal Analysis:
10.1.1 Significance and Use—For PTFE resins that have
been melted prior to use, the melting peak temperature char-
acteristics of a resin provide important information about the
thermal history of the material. Melting peak temperatures (see
Fig. 3) are used to determine conformance of a resin to the
melting peak temperature requirements in Table 1 of this
specification.
10.1.2 Apparatus—Use apparatus described in Test Method
D4591.
10.1.3 Procedure—Measure melting peak temperatures in
accordance with procedures given in Test Method D4591. An
initial melting peak temperature above the melting peak
temperature obtained on the second and subsequent melting
(defined as the second melting peak temperature) indicates that
the resin was not melted before the test. The second melting
peak temperature occurs at about 327°C (621°F). The differ-
ence between the initial and second melting peak temperatures
NOTE 1—Aluminum plates tack welded to rods. is greater than 5°C (9°F). If peak temperatures are difficult to
NOTE 2—All dimensions are in millimetres. discern from the curves (that is, because the peaks are rounded
FIG. 2 Sintering Rack for SSG Specimens
rather than pointed) straight lines should be drawn tangent to
the sides of the peak. These lines intersect at the peak
of the die across the top of the die cavity. Insert the die in a temperature. Where more than one peak occurs during the
suitable hydraulic press and apply pressure gradually (see Note initial melting test, the presence of any peak corresponding to
4) until a pressure of 7 MPa (1015 psi) is attained. Hold this the second melting peak temperature indicates the presence of
pressure for 2 min, then increase the pressure to 14 MPa (2030 some previously melted material.
psi) and hold for an additional 2 min. Remove the disk from the 10.2 Bulk Density:
die. Write the sample identification number on the preform 10.2.1 Significance and Use—Bulk density gives an indica-
using an appropriate marker that will not effect the PTFE tion of how a resin performs during the filling of processing
during sintering. equipment. PTFE resins tend to compact during shipment and
9.3.3 Sinter the preforms in accordance with Table 3, storage. Because of this tendency to pack under small amounts
Procedure A (see Note 5). of compression or shear, Test Method D1895 is not applicable
9.3.4 Remove all flash from those portions of these speci-
mens that will be used for determination of specific gravities so
that no air bubbles will cling to their edges when the specimens
are immersed in liquid during these tests. It is recommended
that cotton gloves be worn while handling test specimens.
9.4 Conditioning Test Specimens:
9.4.1 For tests of tensile properties and all tests requiring the
measurement of specific gravities, condition the test specimens
in general accordance with Procedure A of Practice D618, with
the following deviations therefrom: (1) the aging period shall
be a minimum of 4 h immediately prior to testing, (2) the
laboratory temperature shall be 23 6 2°C (73.4 6 3.6°F), and
(3) there shall be no requirement respecting humidity. The
other tests require no conditioning of the molded test speci-
mens.
9.5 Test Conditions:
9.5.1 Tests shall be conducted at the standard laboratory
temperature of 23 6 2°C (73.4 6 3.6°F), unless otherwise
specified in the test methods or in this specification. This FIG. 3 Melting Characteristics by Thermal Analysis

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D4895 − 18
to these resins. The procedure given in 10.2.2 through 10.2.5 10.2.2.6 Work Surface—The work surface for holding the
must be used to measure this property. volumetric cup and leveler shall be essentially free from
10.2.2 Apparatus: vibration. The feeder, therefore, must be mounted on an
10.2.2.1 Funnel—A funnel arrangement as shown in Fig. 4. adjoining table or wall bracket.
10.2.2.2 Feeder 6—A feeder with a No. 8 wire screen placed 10.2.2.7 Balance—Balance, having an extended beam, with
over approximately the top two thirds of the trough. The funnel a capacity of 500 g and a sensitivity of 0.1 g, or equivalent.
shall be mounted permanently in the feeder outlet.
10.2.2.3 Controller 7 10.2.3 Procedure—Place the clean, dry volumetric cup on
10.2.2.4 Volumetric Cup and Cup Stand (see Fig. 5)—The the extended beam of the balance and adjust the tare to zero.
volumetric cup shall be calibrated initially to 250 mL by filling Select about 500 mL of the resin to be tested and place it on the
it with distilled water, placing a planar glass plate on top, feeder screen. Put the cup in the cup stand and place the
drying the outside of the cup, and weighing. The net weight assembly such that the distance of free-polymer fall from the
shall be 250 6 0.5 g. The top and bottom faces of the feeder outlet to the top rim of the cup shall be 39 6 3 mm
volumetric cup and the cup stand shall be machined plane and (1.5 6 0.012 in.). Increased fall causes packing in the cup and
parallel. higher bulk density values. Set the controller so that the cup is
10.2.2.5 Leveling Device—The leveler (see Fig. 6) shall be filled in 20 to 30 s. Pour the sample on the vibrating screen and
affixed permanently to the table and adjusted so that the fill the cup so that the resin forms a mound and overflows. Let
sawtooth edge of the leveler blade passes within 0.8 mm (0.031 the resin settle for about 15 s and then gently push the cup and
in.) of the top of the volumetric cup. its stand beneath the leveler. Exercise care to avoid agitation of
the resin and cup before leveling. Weigh the resin to the nearest
0.1 g.
6
A “Vibra-Flow” Feeder, Type FT01A, available from FMC Corp., Material 10.2.4 Calculation—Calculate the bulk density as follows:
Handling Division, FMC Building, Homer City, PA 15748, has been found
satisfactory for this purpose.
7
A “Syntron” controller, Type SCR1B, available from FMC Corp., address as grams of resin 3 4 5 bulk density~ grams per litre!
shown in Footnote 10, has been found satisfactory for this purpose.

NOTE 1—Funnel Material: type 304 Stainless Steel 16 Gage (1.6-mm thickness).
NOTE 2—All dimensions are in millimetres.
FIG. 4 Details of the Funnel Used for the Determination of Bulk Density

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D4895 − 18

NOTE 1—All dimensions are in millimetres.

FIG. 5 Volumetric Cup and Cup Stand for the Determination of Bulk Density

NOTE 1—Base plate must be flat and parallel. Saw blade, when mounted, must be square to and parallel with base plate within 0.13 mm from end to
end. Height of saw blade must have 0.8 mm or less clearance between blade and assembled cup and cup stand (as indicated by phantom lines). Welded
construction where indicated. Material: as noted.

NOTE 2—All dimensions are in millimetres.

FIG. 6 Leveler Stand for the Determination of Bulk Density

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D4895 − 18
10.2.5 Precision and Bias—A precision statement for use will not condense on the sample during this test. Determine the
with this procedure is under development. The procedure in weight of resin retained on each sieve.
this test method has no bias because the value of bulk density 10.3.4 Calculation:
shall be defined only in terms of a test method. 10.3.4.1 Calculate the net percentage of resin on each sieve
10.3 Particle Size: as follows:
10.3.1 Significance and Use—The fabrication of PTFE res-
ins is affected significantly by particle (or agglomerate) size net percentage on sieve Y 5 2 3 weight of resin in grams on sieve Y.
and size distribution. The average particle size of PTFE resins
is determined by fractionation of the material with a series of 10.3.4.2 Calculate the cumulative percentage of resin on
sieves. Fractionation is accomplished by mechanically shaking each sieve as follows:
the material in the assembly of sieves for a specified period.
10.3.2 Apparatus: cumulative percentage on sieve Y 5 sum of net percentages
10.3.2.1 Balance, capable of weighing to 60.1 g. on sieve Y and sieves
10.3.2.2 Sieves, U.S. Standard Sieve Series, 203-mm (8-in.) having numbers smaller than Y.
diameter conforming to Specification E11. It is suggested that NOTE 7—Cumulative percentage on 500-µm (No. 35) sieve = net
the following sieve numbers (openings) be used: 1.40 mm (14), percentage on 1.40-mm (No. 14) + net percentage on 1.00-mm (No.
1.00 mm (18), 710 µm (25), 500 µm (35), 355 µm (45), 250 µm 18) + net percentage on 710-µm (No. 25) + net percentage on 500-µm
(No. 35) sieves.
(60), and 180 µm (80). However, other configurations of sieves
may be used to give equivalent results. 10.3.4.3 Plot the cumulative percentage versus the sieve
10.3.2.3 Sieve Shaker—A mechanical sieve shaking device opening size (or sieve number) on log-probability paper as
capable of imparting uniform rotary and tapping action. shown in the sample plot (see Fig. 7). The sieve numbers and
10.3.2.4 Freezer—Any commercial ice freezer. (A dry-ice sieve opening sizes in micrometres are indicated below the
chest may be used.) figure. Draw the best straight line through the points and read
10.3.3 Procedure: the particle size at the 50 % cumulative percentage point (D50).
10.3.3.1 Place 50 6 0.1 g of the sample in an aluminum 10.3.4.4 Calculate the particle size, average diameter, d50, as
pan, and cool the pan and contents to less than 10°C (50°F). follows:
10.3.3.2 Measure the tare weight of each of the sieves listed
in 10.3.2.2. Place the conditioned sample on the top sieve of d 5 d 50~ micrometres!
the assembly and shake in the sieve shaker for 10 6 0.5 min.
The dewpoint temperature of the sieving room must be less 10.3.5 Precision and Bias—The test precision is 63.2 %
than the temperature of the conditioned sample so that water (two sigma limits) for the combination of 710 + 500 + 355-µm

Sieve No. Sieve Opening, µm

14 1400
18 1000
25 710
35 500
45 355
60 250
80 180
FIG. 7 Log Probability Plot for Sieve Analysis

8
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D4895 − 18
(25 + 35 + 45) sieve fractions for a resin where this combina- water content, % 5 ~ A 2 C ! / ~ A 2 B ! 3 100
tion of sieves retains, on the average, 78 % of the sample. Since
where:
there is no accepted reference material suitable for determining
the bias for this test procedure, no statement on bias is being A = weight of resin, dish, and lid, g
made. B = weight of dish and lid, g, and
C = weight of resin, dish, and lid after drying, g.
10.3.6 Alternative methods for particle size are available.
Light Scattering Instruments/Light Diffraction Instruments (see 10.4.5 Precision and Bias—The precision of this test is
ISO 12086-2, 8.6.5) and Electron Zone Sensing Instruments, 60.0063 percentage points (two sigma limits). Since there is
which are resistance-variation testers, (see ISO 12086-2, no accepted reference material suitable for determining the bias
8.6.4), and Dynamic Image Analysis Method (see ISO for this test, no statement on bias is being made.
13322-2) are used as long as there is a direct correlation to the 10.4.6 Alternative Method for Determination of Water Con-
Particle Size Analysis in 10.3 of this specification. tent by Karl Fischer Reagent8:
10.3.6.1 This alternative method is very dependent on 10.4.6.1 Weigh 35 6 1 g of resin into a glass-stoppered
particle shape and is only recommended for processes that are flask containing about 50 mL of pretitrated methanol. Shake to
stable and that have regular spherical type shape particles. mix with a swirling motion for a few minutes. Titrate with
Also, it is recommended that each manufacturing processor do standardized Karl Fischer Reagent9 to a visual or electrometric
an analysis to determine their own correlation. end point.
10.4 Water Content: 10.5 Standard Specific Gravity (SSG):
10.4.1 Significance and Use—The presence of an excessive 10.5.1 Significance and Use—The specific gravity of an
amount of water in PTFE resin has a significant adverse effect article made from a PTFE resin is affected both by the
upon the processing characteristics of the resin and the quality particular resin used and by the way the resin is processed.
of products made using the resin. A sample of PTFE resin of Therefore, a test method that measures the specific gravity of
known weight is dried in a vacuum oven in a tared aluminum an article prepared in a precisely defined way provides valuable
weighing dish. When the resin is dry, it is removed from the resin characterization data. The specific gravity of a specimen
oven, placed in a desiccator, allowed to cool, and then of PTFE resin prepared in accordance with all of the require-
reweighed. Water content is calculated from the weight lost ments of 9.2.3.1 defines the SSG for that resin specimen.
during drying. 10.5.2 Procedure:
10.5.2.1 Determine, in accordance with 10.5.2.2, the spe-
NOTE 8—If volatiles other than water are suspected, use the alternative
method described in 10.4.6. cific gravity of specimens prepared in 9.2.3.1.
10.5.2.2 Make specific gravity determinations in accordance
10.4.2 Apparatus: with the procedures described in Test Methods D792, Method
10.4.2.1 Balance, capable of weighing to the nearest 0.0001 A. Add two drops of a wetting agent10 to the water in order to
g. reduce the surface tension and ensure complete wetting of the
10.4.2.2 Oven. specimen.
10.4.2.3 Aluminum Weighing Dishes, with lids.
10.4.3 Procedure (see Note 8)—Wash the aluminum weigh- 10.6 Thermal Instability Index (TII):
ing dishes with water and rinse with acetone. When the acetone 10.6.1 Significance and Use—The TII gives an indication of
has evaporated from the dishes, dry them thoroughly in an how a resin resists degradation during extended periods of
oven at 50 to 80°C (122 to 176°F), then store in a desiccator heating at sintering temperatures. This test method compares
until ready for use. Obtain the tare weight, B, of an aluminum the SSG of a resin (determined in 10.5) to its extended specific
weighing dish, plus lid, to the nearest 0.0001 g. Place 35 to 40 gravity (determined here). Specimens used to determine ESG
g of PTFE resin in the tared aluminum weighing dish and are identical to those used to determine SSG, except for the
record the weight (including lid), A, to the nearest 0.0001 g differences in thermal history described in 9.2.3. The specific
(see Note 9). Dry in an oven for two hours at 150°C (302°F), gravity of a specimen of PTFE resin prepared in accordance
with the dish lid removed. Remove the dish from the oven, with all of the requirements of 9.2.3.2 defines the ESG for that
replace the lid on the weighing dish, and allow to cool in the resin specimen.
desiccator for at least 30 min. Reweigh the dish (plus the resin 10.6.2 Procedure—Determine, in accordance with 10.5.2.2,
and lid), C, and calculate the weight loss. the specific gravity of specimens prepared in 9.2.3.2.
10.6.3 Calculation—Calculate the thermal instability index
NOTE 9—Select one sample from each group of samples and run
(TII) as follows:
duplicate moisture determinations on it. If the difference between the
duplicate results exceeds 0.01 percentage points, the entire group of
samples must be run over. TII 5 ~ ESG 2 SSG! 3 1000
NOTE 10—When a group of samples is run at the same time, it is good
practice to place the lids from the weighing dishes directly under their
corresponding dishes while the samples are drying in the oven. This 8
Details of this method are found in Mitchell, J., Jr. and Smith, D. M.
eliminates the possibility of introducing errors in the tare weights. Also, “Aquametry,” 2nd Ed., published by Interscience Publishers, Inc., New York, NY
overnight drying in a circulating air oven may be used if the data can be 1977.
9
shown to be equivalent to those obtained with the above procedure. Karl Fischer Reagent (Catalog No. So-K-3) is available from the Fischer
Scientific Co., Pittsburgh, PA.
10.4.4 Calculation—Calculate the water content as follows: 10
Examples of suitable wetting agents are “Glim” detergent, B. J. Babbitt, Inc.,
“Joy” detergent, Proctor and Gamble, Inc; and “Triton” X-100, Rohm and Hass Co.

9
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D4895 − 18
10.7 Tensile Properties: 10.8.1 Significance and Use—Processing of the PTFE resins
10.7.1 Procedure—Cut five tensile specimens from the disk covered by this specification normally involves “paste extru-
prepared in accordance with all of the requirements of 9.1, sion” of a blend of the resin with a volatile liquid, as indicated
using the microtensile die described in Fig. 8,11 which is in 1.1. The pressure that must be applied to such a blend to
exactly the same as Fig. 1 of Test Method D1708. Determine extrude it is affected by several processing conditions which
the tensile strength in accordance with the procedures de- include the nature and amount of deformation imparted to the
scribed in Test Method D638, except that the initial jaw blend during extrusion (usually characterized by the reduction
separation shall be 22.0 6 0.13 mm (0.875 6 0.005 in.), and ratio), the type and amount of liquid used, and the extrusion
the speed of testing shall be 50 mm (2 in.)/min. Clamp the temperature. When such a blend is extruded under well-defined
specimen with essentially equal lengths in each jaw. Determine processing conditions, the pressure required to affect extrusion
elongation at break from the chart, expressed as a percentage of (extrusion pressure) provides significant characteristic infor-
the initial jaw separation. mation about the resin itself.
10.7.2 Precision and Bias—A precision and bias statement 10.8.2 Apparatus—Recommended apparatus:
for use with this procedure is under development and will be
10.8.2.1 Paste Extruder (Fig. 9)—One paste extruder that is
included when it has been approved by the balloting process.
used is a vertically disposed, breech-loading extruder with a
10.8 Extrusion Pressure: 32-mm (1.26 in.) inside diameter extrusion cylinder. The barrel
length is approximately 305 mm (12 in.), which is not critical
11
so long as it will hold enough lubricated resin to extrude for
A steel rule type of die, available from Admiral Steel Rule Die, 133 Railroad
Ave., Garden City Park, NY 11040, has been found satisfactory for this purpose. An
about 5 min. The ram is 32 mm (1.26 in.) outside diameter,
international source is Stansvormenfabriek Veryloet B. V., Postbus 220, Gantelweg with a ring groove near its free end to hold an O-ring that
15, 3350 AE Papendrecht, Holland. makes a tight seal between the ram and extruder cylinder. The
extruder is equipped with devices for sensing and recording
pressure on the face of the ram. The range of the pressure
sensing device shall be greater than 70 MPa (10 000 psi).
Temperature-controlling equipment maintains the extruder at
30 6 1°C. A system (hydraulic or screw) drives the ram at a
speed of about 18 mm/min (0.7 in./min) to give an output rate
of 19 g/min on a dry-resin basis (about 23.5 g/min of lubricated
resin) during the extrusion pressure test. The extruder also has
a fast-speed drive (speed not precisely controlled) to run the
ram rapidly into the cylinder cavity prior to the extrusion
pressure test. The extruder-die assembly slides on tracks from
under the ram to allow easy access for loading and cleaning the
cylinder. An alternative muzzle-loaded paste extruder shall be
used which has a detachable die assembly. The die assembly is
detached, a preformed charge of resin is inserted up into the
cylinder and the die assembly is reattached.
10.8.2.2 Extrusion Dies (Fig. 10)—Interchangeable extru-
sion dies, each having 30° included angles, give the desired
reduction ratios when dimensioned as follows:

Reduction Ratio Die Orifice

(Inside Diameter), Land Length, Die Length,
mm (in.) mm (in.) mm (in.)
100 to 1 3.18 (0.125) 25.35 (0.998) 78.66 (3.0)
400 to 1 1.59 (0.0625) 4.78 (0.188) 61.06 (2.3)
1600 to 1 0.79 (0.0312) 0.38 (0.015) 58.15 (2.2)

NOTE 11—Reduction ratio in this specification is the ratio of the

cross-sectional area of the extruder cylinder to the cross-sectional area of
the die. This must not be confused with another definition wherein
reduction ratio is the ratio of the cross-sectional area of the extruder
cylinder to the cross-sectional area of the sintered extrudate.
10.8.2.3 Miscellaneous Apparatus—Equipment is needed
for weighing, blending, conditioning (at 30°C) and preforming,
NOTE 1—All dimensions are in millimetres. as well as extruded cleaning.
FIG. 8 Microtensile Die 10.8.3 Procedure:

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D4895 − 18

FIG. 9 Paste Extruder for Determining Extrusion Pressure

10.8.3.1 Screen the dry resin through a 4.75-mm (No. 4) of lubricant. Shake the jar briefly to minimize the wetting of
sieve onto a clean, dry, lint-free sheet of paper. the jar wall with liquid.
10.8.3.2 Transfer 200 6 0.5 g of the screened resin to a 10.8.3.4 Blend the mixture by placing the jar on rubber-
clean, dry glass jar about 92 mm (3.625 in.) in diameter coated mill rolls and rolling it at 30 r/min for 25 6 5 min, by
(approximately 1-L capacity) having an airtight closure, or into fastening the jar to a windmill type blender14 and blending for
a V-blender of laboratory size. 20 6 1 min, or by blending the mixture in the V-blender for
10.8.3.3 Determine the density of the lubricant, a kerosene- 15 6 5 min. If a V-blender has been used, drop the resin from
type hydrocarbon liquid.12 Determine the density at 25°C using it into a jar of approximately 1-L capacity and seal the jar.
Test Method D4052, a commercial density meter that will give 10.8.3.5 After blending, store the jar with its contents at
four significant figures for the density,13 or a technically 30 6 1°C for a minimum of 2 h. A water bath has been found
equivalent procedure. Calculate the mass of lubricant required to be satisfactory. This enables the lubricant to diffuse to the
by multiplying the density by 60.00 mL. Add the calculated interior of individual particles and surfaces not reached during
mass 60.01 g of the lubricant to the resin in the jar or blender. the blending process.
It is convenient to make this addition while the jar containing 10.8.3.6 Place the proper extrusion die for the desired
the powder is on a balance that has a sensitivity at least as good reduction ratio (given in 10.8.2.2) in the paste extruder.
as the 60.01 g required for the test. Avoid wetting the walls of 10.8.3.7 Resin Preform—To preform the resin for the
the blending vessel with the liquid as this impairs mixing. breech-loading paste extruder of 10.8.2.1, slide the extruder-
When a jar is used the lid shall be taped in place to prevent loss die assembly forward, mount a 32-mm (1.26-in.) inside diam-
eter extension tube about 610 mm (24 in.) in length at the
breech end of the extruder cylinder. Quickly pour the lubri-
12
Isopar K, available from Exxon Co., has been found satisfactory for this cated resin through a funnel into the extension and force the
purpose.
13
A Mettler/Paar DMA 40 density meter has been found suitable for determining
14
density to the required precision. A Gilson spinning wheel mixer has been found suitable for this purpose.

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D4895 − 18
10.8.4 Precision and Bias—The test precision and bias are
to be determined by round-robin testing.
10.9 Stretching Void Index:
10.9.1 Significance and Use—This test method compares
the unstrained specific gravity (USG) of a resin to its strained
specific gravity (strained SG). The specific gravity of a
specimen of PTFE resin prepared in accordance with all of the
requirements of 9.3 defines the USG for that resin specimen.
The SVI gives one indication of the potential for induced void
content of a solid fabricated resin product in use. Such void
content may contribute to a susceptibility to the formation of
cracks and failures under conditions of extreme stretching and
stress or in some environments when stressed. Similar failures
have also been associated, at times, with improper processing
techniques.
10.9.2 Procedure:
10.9.2.1 Determine, in accordance with 10.5.2.2, the spe-
cific gravity of specimens prepared in 9.3. This is the USG for
the specimen.
10.9.2.2 Cut tensile specimens from the disk prepared in 9.3
using the microtensile die shown in Fig. 8. Clamp the specimen
in a tensile testing machine with essentially equal lengths in
each jaw. The initial jaw separation shall be 12.5 6 0.1 mm
(0.5 6 0.005 in.). Strain the specimen at a constant rate of 5.0
mm (0.2 in.)/min until it breaks. This strain rate and initial jaw
separation yield a strain rate of 40 % ⁄min, based on the original
gage length of the specimen. If elongation at break is less than
Reduction Ratio Die Orifice (Diameter) Land Length Die Length 200 %, discard the result and repeat 10.9.2.2.
100 to 1 3.18 25.35 78.66
400 to 1 1.59 4.78 61.06
10.9.2.3 Cut off a portion of the stretched part of the
1600 to 1 0.79 0.38 58.15 specimen. Determine, in accordance with 10.5.2.2, the specific
gravity of this strained specimen (strained SG).
NOTE 1—All dimensions are in millimetres. 10.9.3 Calculation—Calculate the stretching void index
FIG. 10 Extruder Die Assembly for Extrusion Pressure Apparatus
(SVI) as follows:

resin into the extruder cylinder with a tamping rod. Apply the SVI 5 ~ USG 2 strained SG! 3 1000
force with hand pressure and a very slow, even stroke. To
preform the resin for the muzzle-loading paste extruder of 11. Inspection
10.8.2.1, mount a 32-mm (1.26-in.) inside diameter preforming
tube about 610 mm (24 in.) in length with its cross section 11.1 Inspection and certification of the material supplied
resting against a flat, smooth surface. Quickly pour the with reference to this specification shall be for conformance to
lubricated resin through a funnel into the tube and force the the requirements specified herein.
resin down in the tube. The force may be applied with a 11.2 Lot-acceptance inspection shall be the basis on which
hydraulically controlled tamping device to compact the resin acceptance or rejection of the lot is made. The lot-acceptance
with a slow, even stroke to a minimum of 690 kPa (100 psi) on inspection shall consist of the following:
the resin. Remove the preform from the preforming tube, insert 11.2.1 Bulk density,
the preform up into the cylinder of the extruder, and attach the 11.2.2 Particle size, and
die assembly. 11.2.3 Melting point.
10.8.3.8 Use the fast-speed drive to run the ram down into
the cylinder cavity. When the first bit of beading emerges from 11.3 Periodic check inspection with reference to a specifi-
the orifice, stop the descent of the ram. cation shall consist of the tests for all requirements of the
10.8.3.9 Immediately change to slow-speed drive, start the material under the specification. Inspection frequency shall be
pressure-recording system, and extrude the lubricated resin at a adequate to ensure the material is certifiable in accordance with
rate of 19.0 6 1.0 g/min (dry-resin basis). 11.4.
10.8.3.10 Record the pressure developed at the face of the 11.4 Certification shall be that the material was manufac-
ram in contact with the resin in the cylinder as a function of tured by a process in statistical control, sampled, tested and
time. The extrusion pressure is the average pressure required to inspected in accordance with this classification system, and
extrude the sample as measured between the third and fourth that the average values for the lot meet the requirements of the
minutes of the extrusion. specification (line callout).

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D4895 − 18
11.5 A report of test results shall be furnished when re- 12.2 Package Marking—Shipping containers shall be
quested. The report shall consist of results of the lot-acceptance marked with the name of the resin, type, and quantity contained
inspection for the shipment and the results of the most recent therein.
periodic-check inspection.
12.3 All packing, packaging, and marking provisions of
12. Packaging and Package Marking Practice D3892 shall apply to this specification.
12.1 Packaging—The resin shall be packaged in standard
commercial containers so constructed as to ensure acceptance 13. Keywords
by common or other carriers for safe transportation to the point 13.1 coagulated dispersion polytetrafluoroethylene; fluo-
of delivery, unless otherwise specified in the contract or order. ropolymers; polytetrafluoroethylene; PTFE

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 should state

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

APPENDIX

(Nonmandatory Information)

X1. EXPANSION TEST FOR EXTRUDED TUBING

X1.1 Significance and Use X1.3 Procedure

X1.1.1 Processing of the PTFE resins covered by this X1.3.1 The procedure is as given in 10.8.3, except that
specification almost always includes extrusion of a blend of the preforming is done in a separate mold shell having a 31.6-mm
resin with a volatile liquid. The quality of the extrudate is (1.245-in.) inside diameter, and fitted with a central die rod
affected by several processing conditions which include the having the same diameter as the extruder guide tube and
nature and amount of deformation imparted during extrusion, suitable end plugs. Pour the lubricated resin into one end of the
the type of resin, the type and amount of liquid used, and the vertical preform mold, and tap the side of the mold shell to
extrusion temperature. When the blend is extruded into a tube level the resin. Place the top mold plug in the mold, and apply
under well-defined processing conditions, characterization of a minimum pressure of 690 kPa (100 psi) to the resin.
the resultant tube using suitable test procedures provides X1.3.2 Remove the preform from the mold and wrap in
significant characteristic information about the resin. aluminum foil for 4 h. This is to provide uniform distribution
of lubricant within the preform.
X1.2 Apparatus
X1.3.3 When the extruder is ready for extrusion, unwrap the
X1.2.1 Use the extruder shown in Fig. 9 and described in preform and quickly insert it into the extruder cylinder over the
10.8.2.1 (or equivalent apparatus), except that a guide tube guide tube. Attach the mandrel tip to the guide tube, then close
which extends through the center of the ram and into the die is the extruder cylinder and attach the die assembly.
attached to the hydraulic cylinder and a mandrel tip is screwed X1.3.4 Proceed in accordance with 10.8.3.8 and 10.8.3.9.
onto this guide tube. The guide tube has an outside diameter of Pass the extruded tubing vertically downward through an
15 mm (0.59 in.), and the mandrel tip has an outside diameter electrically heated air oven designed to produce a higher
of 0.4 mm (0.016 in.) over a land length of 0.4 mm. When used temperature in the lower half of the oven than in the upper half.
in combination with the 0.8-mm (0.031-in.) orifice given in The lubricant is vaporized in the upper half of the oven at about
10.8.2.2, a reduction ratio of 1600 to 1 is produced. This setup 120 to 150°C (248 to 302°F). Adjust the temperature in the
will yield a sintered tube with an outside diameter of about lower half of the oven so that the tubing passing through it is
0.76 mm (0.03 in.), and an inside diameter of about 0.4 mm. in the gel (completely transparent) for about 100 mm (4 in.). As
X1.2.2 Use the miscellaneous apparatus described in the tubing emerges from the oven it is allowed to cool in air,
10.8.2.3. and is then coiled on a suitable spool.

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D4895 − 18
X1.3.5 Connect one end of the extruded tubing to a source glass tube. If this does not occur, increase the nitrogen pressure
of nitrogen that shall apply at least 345-kPa (50-psi) internal slowly until expansion occurs.
pressure to the tubing. Make sure that there is at least 15 m (50
ft) of tubing. Clamp the free end of the tubing and push it X1.3.6 As the expanded tubing emerges from the glass tube
through a heated glass tube having an inside diameter of 1.65 allow it to cool in air and coil it up on a suitable spool. If a flaw
mm (0.065 in.). Apply 345-kPa pressure to the PTFE tubing, appears and the expanded tubing loses nitrogen pressure,
and move the PTFE tubing through the heated glass tube at a clamp off the tubing downstream of the flaw and continue.
rate that allows the PTFE tubing to reach 340°C (644°F) in the X1.3.7 The expanded tubing is inspected visually for flaws
last 75 to 100 mm (3 to 4 in.) of the glass tube (that is, the and stretch marks.
PTFE tubing becomes transparent). As the PTFE tubing
becomes transparent it expands against the inner surface of the NOTE X1.1—This test is not appropriate for all resins.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D4895 - 16)
that may impact the use of this standard. (November 1, 2018)

(1) Changed ISO 12086-1 and ISO 12086-2 to ISO 20568-1 (3) Changed cup height 98.40 mm – 98.45 mm to 97.40 mm –
and ISO 20568-2 in Note 1. 97.45 mm in Fig. 5.
(2) Changed ISO 12086-1 to ISO 20568-1 and changed ISO
12086-2 to ISO 20568-2 in 2.2.

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

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14