An American National Standard

Designation: D 6546 – 00

Standard Test Methods for

and Suggested Limits for Determining Compatibility of
1
Elastomer Seals for Industrial Hydraulic Fluid Applications
This standard is issued under the fixed designation D 6546; 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 D 395 Test Methods for Rubber Property—Compression

1.1 These test methods cover the procedure for measuring Set
physical properties of elastomer seals in the form of O-rings D 412 Test Methods for Vulcanized Rubber and Thermo-
after exposure to industrial hydraulic fluids and thermal aging. plastic Elastomers—Tension
The measured properties are then compared to the physical D 471 Test Method for Rubber Property–Effect of Liquids
properties of elastomer seals that have not been exposed to the D 1414 Test Methods for Rubber O-Rings
industrial hydraulic fluids and thermal aging. The changes in D 2000 Classification System for Rubber Products in Auto-
these properties form a basis for assessing compatibility when motive Applications
these changes are compared against the suggested limits in D 2240 Test Method for Rubber Property—Durometer
Table 1. Hardness
1.2 While these test methods involve the use of O-rings, D 3677 Test Methods for Rubber—Identification by Infra-
they can also be used to evaluate the compatibility of the red Spectrophotometry
elastomeric compounds of specialty seals with industrial hy- D 3767 Practice for Rubber—Measurement of Dimensions
draulic fluids and their resistance to thermal aging. The D 5028 Test Method for Curing Properties of Pultrusion
compounds can be molded into O-rings for evaluation pur- Resins by Thermal Analysis
poses. E 1131 Test Method for Compositional Analysis by Ther-
1.3 These test methods provide procedures for exposing mogravimetry
O-ring test specimens to industrial hydraulic fluids under 2.2 SAE Standard:3
definite conditions of temperature and time. The resulting AS568A O-ring Sizes
deterioration of the O-ring material is determined by compar- 3. Terminology
ing the changes in work function, hardness, physical proper-
ties, compression set, and seal volume after immersion in the 3.1 Definitions:
test fluid to the pre-immersion values. 3.1.1 batch—all the O-rings molded from the same lot of
1.4 This standard does not purport to address all of the material and presented for inspection at one time.
safety concerns, if any, associated with its use. It is the 3.1.2 compound—a fully formulated elastomer material
responsibility of the user of this standard to establish appro- containing all fillers and cross- linking agents.
priate safety and health practices and determine the applica- 3.1.3 fluid saturation effect—the absorption of fluid by the
bility of regulatory limitations prior to use. elastomer until an equilibrium swell value is reached at a
1.5 The values stated in SI units are to be regarded as the particular temperature.
standard. The values given in parentheses are for information 3.1.4 O-ring—a rubber seal of homogeneous composition
only. molded in one piece to the configuration of a torus with circular
cross section.
2. Referenced Documents [Link] Discussion—O-rings are used as both dynamic and
2.1 ASTM Standards: 2 static seals. The size of the O-ring is normally designated by a
dash number corresponding to the size tables listed in AS568A.
The dimensions for the O-rings used in these test methods are
1
These test methods are under the jurisdiction of ASTM Committee D02 on listed in Annex A2.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 3.1.5 ultimate elongation—the amount of stretch that the
[Link].09 on Compatibility.
Current edition approved April 10, 2000. Published June 2000. O-ring is exposed to before breaking.
2
For referenced ASTM standards, visit the ASTM website, [Link], or
contact ASTM Customer Service at service@[Link]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available from Society of Automotive Engineers, 400 Commonwealth Drive,
the ASTM website. Warrendale, PA 15096.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 D 6546 – 00
TABLE 1 Property Change Limits
Time, h Maxi- Maxi- Hardness Maxi- Maxi- Maxi- Maxi-
mum mum Change, mum mum mum mum
Volume Volume Shore A Tensile Elongation Work Compres-
Swell, Shrinkage, Points Strength Change, Function sion Set,
% % Change, % Change, %
% %
24 15 −3 67 −20 −20 612 ...
70 15 −3 67 −20 −20 612 20
100 15 −3 68 −20 −20 612 20
250 15 −4 68 −20 −20 612 25
500 20 −4 610 −25 −25 617 30
1000 20 −5 610 −30 −30 620 35

3.1.6 work function—work done on a test specimen to cause previous immersion period. If the changes in the physical
20 % deformation. properties have deteriorated beyond the suggested limits, then
further testing is not required. The tolerance for any immersion
4. Significance and Use period shall be 6 1 % of the immersion period.
4.1 When more than one elastomer seal material is tested,
the test methods yield comparative data on which to base 7. Test Fluids
judgements as to expected service quality. Suggested in-service 7.1 For reliable compatibility assessments, it is desirable to
property change limits are provided. Property changes beyond use the fluid with which the elastomer will come in contact in
these limits will indicate limited service life of the elastomer actual service. For comparative tests, samples of fluid from the
seal. same drum or shipment shall be used.
4.2 These test methods attempt to simulate service condi-
tions through controlled aging and evaluation of property 8. Test Specimen
changes but may not give any direct correlations with actual 8.1 The test specimens shall be O-rings molded from the
part performance since actual service conditions vary widely. same compound batch from which the actual seals will be
These test methods yield comparative data and indications of molded. The test samples should approximate the cross section
property changes of the elastomeric seal material under ideal of the actual seal to be used so that the fluid saturation effect is
service conditions. These test methods can be used for quality properly considered. The test samples should be either -021,
control purposes, for engineering assessments, for service -120, -214, or -320 O-rings, in accordance with AS568A.
evaluation, and for manufacturing control. The information These have an approximate inside diameter of 25.4 mm (1 in.)
from these test methods can be used to anticipate expected and represent the most popular cross sections of seals used in
service quality. industrial systems. The actual dimensions of each O-ring size
are listed in Annex A2.
5. General Test Methods 8.2 Test specimens shall be wiped clean of external con-
5.1 Except as otherwise specified, the test methods for taminants prior to testing by using a clean dry wipe.
rubber O-rings referred to in 5.1.1-5.1.6, which are applicable
in general to vulcanized rubber, shall be complied with as 9. Suggested Compatibility Test Limits
required and are hereby made a part of these test methods. 9.1 For a critical seal application, property change limits, as
5.1.1 Tension Test—Test Methods D 412 and D 1414. described in Table 1, should be observed.
5.1.2 Compression Set—Test Methods D 395 and D 1414. 9.2 All values are in reference to soak time in the opera-
5.1.3 Fluid Aging—Test Method D 471 and Test Methods tional fluid at the operating temperature of the application.
D 1414. Values reflect changes from the determined pre-immersion
5.1.4 Hardness—Test Method D 2240. original physical property values of the test specimens.
5.1.5 Compositional Analysis—Test Methods D 3677 and 9.3 If the changes are within these limits, the elastomer
Test Method E 1131. should be considered compatible. Once a seal material is found
5.1.6 Degree of Cure—Test Method D 5028. to be compatible, all seals for that system should be ordered by
5.2 In case of conflict between the provisions of the ASTM specific compound or specification and not by Classification D
test methods referenced in 5.1.1-5.1.6 and the detailed provi- 200 call out number or generic polymer designation.
sions of the test methods in Test Methods D 6546, the latter
shall take precedence. 10. Procedure for Change in Volume
10.1 Apparatus:
6. Test Conditions 10.1.1 Test Container, a Mason jar (quart size) fitted with a
6.1 Temperature—The test temperature shall be the maxi- lid to prevent liquid and vapor from escaping. The lid shall not
mum sustained temperature anticipated in service. contaminate the test liquid. Cover the lid with aluminum foil.
6.2 Immersion Periods—The following immersion periods 10.1.2 Heating Device, a forced air oven, aluminum block
are recommended: 24 h, 72 h, 100 h, 250 h, 500 h, and 1000 h. heater, or oil bath heater. Maintain the temperature within 6
The final immersion period will depend upon the results of the 1°C (1.8°F).

2
 D 6546 – 00
10.1.3 Test Specimen—The test specimen shall consist of an effective seal when the system is restarted. In those cases in
entire O-ring. The same specimen may be used for all tests with which a positive volume change was obtained in 10.2 and long
hardness and volume determinations made prior to stress-strain system down times are anticipated, it is recommended that
tests. Place the test specimen in the test liquid so that it is not volume shrinkage be determined. To perform this optional test
distorted or in contact with the sides of the test container or method, additional O-rings will have to be tested in accordance
with the other test specimens. Test a minimum of three test with 10.2 and then tested in accordance with 10.3 since the
specimens at one time. It is also important that only O-rings of normal test for volume change is immediately followed by the
one size and one material compound be placed in the test destructive tensile test.
container. 10.3.2 The test specimen shall consist on an entire O-ring.
10.1.4 Analytical Balance, an analytical balance capable of The specimen must first be submitted for the volume swell test.
allowing a test specimen to be weighed whether in air or while This specimen is only to be used for this test sequence and not
submerged in water. for any other testing.
10.2 Volume Change—Test three specimens. 10.3.3 Place the test specimen from the volume swell test in
10.2.1 Weigh each test specimen in air, M1, to the nearest 1 a forced-air oven that allows air circulation around the test
mg, and then weigh each specimen immersed in water, M2, at specimen, and maintain the oven at a test temperature of 23 6
room temperature. It is important that all air bubbles clinging 1°C (73.4 6 1.8°F) for 22 6 0.25 h. At the end of the required
to the test specimen be removed before reading the weight in period, remove the specimen from the oven and allow it to air
water. Blot the specimen dry. cool.
10.2.2 Suspend the specimens in the glass jar by the use of 10.3.4 Weigh each test specimen in air, M5, and then weigh
corrosion-resistant wire. Separate the specimens by bending each specimen immersed in water, M6.
small loops in the wire or by locating them in different 10.3.5 The change in volume or shrinkage is calculated as
locations so that they do not contact each other. follows:
10.2.3 Suspend the specimen vertically so that 25.4 mm (1 ~ M5 2 M 6 ! 2 ~ M3 2 M 4 !
in.) of test fluid is between the lower extremity of the specimen DV, % 5 3 100 (2)
~ M3 2 M 4 !
and the bottom of the apparatus. Add enough test fluid to cover
the specimen to a depth of 25.4 mm (1 in.) over the upper where:
extremity of the specimen. M3 = initial mass of volume swell specimen in air after
10.2.4 Place the test apparatus in the heating device adjusted immersion, g,
to maintain the sample at the test temperature for the required M4 = initial mass of volume swell specimen in water after
length of time. At the end of the required immersion period, immersion, g,
remove the specimen from the apparatus. Cool the specimen to M5 = mass of volume swell specimen in air after dry out, g,
room temperature by immersing it in a cool, fresh amount of and
M6 = mass of volume swell specimen in water after dry
the test fluid for 45 min.
out, g.
10.2.5 At the end of the cooling period, remove the speci-
men from the fluid, wipe with a cloth dipped in acetone, and
11. Changes in Tensile Strength, Work Function,
blot dry. Weigh each test specimen in air, M3, and then weigh
Elongation, and Hardness
each specimen immersed in water, M4.
10.2.6 Some oils can be very viscous and may be difficult to 11.1 Original Properties—The original tensile strength,
remove with an acetone wipe. Since these oils do not readily work function, ultimate elongation, and hardness shall be
volatize, specimens exposed to these oils can be cooled by determined using a duplicate set of specimens of O-rings of the
suspending them for 45 min in air at room temperature shielded same cross section as those that are to be immersed in the test
from draft. This will allow the majority of the oil to drip off the fluid. The O-rings shall be from the same batch as those that are
surface of the specimen. Then proceed with the acetone wipe to be immersed in the test fluid.
and weighing process described in 10.2.5. Report when this 11.2 Properties After Exposure to the Test Fluid, for deter-
alternate method of specimen cooling is used. mining the tensile strength, work function, ultimate elongation,
10.2.7 The change in volume is calculated as follows: and hardness of specimens after immersion in the test fluid at
the test temperature. At the end of the required immersion time,
~ M3 2 M 4 ! 2 ~ M1 2 M 2 !
DV, % 5 3 100 (1) remove the specimens, and if necessary, cool them to room
~ M1 2 M2 !
temperature in a fresh sample of the same fluid for 45 min. At
where: the end of the cooling period, remove the specimen from the
M1 = initial mass of specimen in air, g, fluid, wipe it with a cloth dipped in acetone, and blot dry.
M2 = initial mass of specimen in water, g, Immediately determine the hardness, tensile strength, work
M3 = mass of specimen in air after immersion, g, and function, and ultimate elongation in accordance with the
M4 = mass of specimen in water after immersion, g. following test methods, using the original cross-sectional area
10.3 Volume Shrinkage-Simulated Dry Out (Optional Test of the untreated specimens.
Method)—Test three specimens. 11.2.1 Three specimens shall be tested. The test specimen
10.3.1 In some situations when long downtimes are ex- shall consist of the entire O-ring. These specimens must first be
pected, the O-ring should not shrink beyond 5 % of its previous submitted to the volume swell test and cannot be used for any
volume change value since this can affect its ability to be an other testing since physical property tests are destructive.

3
 D 6546 – 00
11.3 Hardness Change—Measure the hardness in accor- where:
dance withTest Methods D 1414, Section 16, using a micro- DT = tensile strength change (%),
hardness tester. Select the mean value from the multiple T2 = tensile strength after immersion, and
readings taken on each O-ring, and then select the mean value T1 = tensile strength prior to immersion.
for all the O-rings. (The mean value for hardness measure- 11.5 Elongation Change:
ments is the numerical mean value; thus if five readings are 11.5.1 Testing Machine—Same as for tensile strength
obtained, for example, 70A, 69A, 69A, 72A, and 71A, the change.
numerical mean would be 70.2 or 70A since shore hardness is 11.5.2 Test Specimen—Same as for tensile strength change.
always reported in whole numbers.) The mean value for all 11.5.3 Procedure—Same as for tensile strength change,
O-rings shall be recorded. Measurements are to be taken before except record the center-to-center distance (D) between the
and after exposure to fluid. spools at rupture to the nearest 2.54 mm (0.1 in.).
11.3.1 The hardness change is calculated as follows: 11.5.4 Calculations:
DH 5 H2 2 H1 (3)
[Link] Ultimate elongation is calculated as follows:
~2D 1 G 2C!
where: E, % 5 C 3 100 (7)
DH = hardness change,
H1 = hardness before fluid exposure, and where:
H2 = hardness after fluid exposure. D = distance between centers of the spool grips at the time
The units are given as Shore A points and a plus or minus of rupture of the specimen,
sign should be included. A negative sign would indicate that G = circumference of one spool (spool diameter 3 3.14),
the O-ring is softening after exposure and its hardness value and
would be less than the hardness value before exposure. A C = inside circumference of the specimen (inside diameter
3 3.14)
positive sign would indicate that the O-ring is hardening after
exposure and its hardness value would be greater than the [Link] Change in elongation is calculated as follows
hardness value before exposure. E 2 2 E1
DE, % 5 E1 3 100 (8)
11.4 Tensile Strength Change:
11.4.1 Testing Machine—The testing machine shall con- where:
form to the requirements specified in Section 3 of Test Methods E2 = elongation after immersion,
D 412 with the exception of grips. Grips for testing O-rings E1 = elongation prior to immersion.
shall consist of ball-bearing spools at least 8.89 mm (0.35 in.) 11.6 Work Function (WF) Modulus Change:
in diameter and be capable of being brought within 19.05 mm 11.6.1 Testing Machine—Same as for tensile strength
(0.75 in.) center-to-center distance at closest approach. Stresses change.
within the specimen shall be minimized by rotating one spool 11.6.2 Procedure—Same as for tensile strength change.
or by lubricating the contact surface of the spools with castor 11.6.3 Calculations—Calculate the work function (WF) as
oil. the energy per unit volume at 20 % elongation. This value is
11.4.2 Test Specimen—The test specimen shall consist of an determined as the area under the stress-strain curve from 0 to
entire O-ring. 20 % strain, and the tensile tester should be programmed to
11.4.3 Procedure—Bring the grips close enough together so determine this value.
that the specimen can be installed without stretching. Separate [Link] Change in work function is calculated as follows:
the grips to remove any slack in the specimen. Exercise care WF2 2 WF1
DWF 5 WF1 3 100 (9)
that no load is placed on the specimen. Pull the specimen at a
rate of 50.8 cm/min (20 in./min). Record the breaking force
where:
value, F, at the time of rupture. DWF = change in work function,%,
11.4.4 Calculations: WF2 = work function after immersion, MPa (psi), and
[Link] Tensile strength is calculated as follows: WF1 = work function prior to immersion, MPa (psi).
T 5 F/A (4)
12. Compression Set
where: 12.1 Micrometer, for measuring the specimen thickness, in
T = tensile strength, MPa (psi), accordance with Practice D 3767, Method A1.
F = breaking force, N (lb), and
A = twice the cross-sectional area calculated from axial 12.2 Spacer Bars, to maintain the constant deflection.
thickness, W, as follows: Spacer bars for O-ring samples shall have a thickness of 9.5 6
0.02 mm (0.375 6 0.001 in.).
A 5 p W2/2 5 1.57 W2 mm2 ~in.2! (5) 12.3 Compression Device, consisting of two or more flat
steel plates between the parallel faces of which the O-ring
[Link] Tensile strength change is calculated as follows: specimens may be compressed, as shown in Fig. 1. Steel
T 2 2 T1 spacers for the required 25 % of compression shall be placed
DT 5 T1 3 100 (6)
on each side of the O-ring specimens to control their thickness

4
 D 6546 – 00

FIG. 1 Compression Device for O-ring Specimens

while compressed. The steel surfaces contacting the rubber specimens should be tested at one time. It is important that only
specimens shall be ground to a maximum roughness of 250 µm O-rings of one size and one material be placed in the
(10 µin.) and then chromium plated and polished. compression fixture.
12.4 Oven, a forced air oven capable of maintaining the test 12.10 Test Fluid—For accurate compatibility assessment, it
temperature within 6 1°C (1.8°F). is desirable to use the fluid with which the elastomer will come
12.5 Plates—The plates between which the O-ring test into contact when in service. For comparative tests, samples of
specimen is compressed shall be made of steel of sufficient fluid from the same drum or shipment shall be used.
thickness (at least 9.5 6 0.02 mm (0.375 6 0.001 in.) or 12.11 Test Container, a Mason jar (quart size), fitted with a
thicker) to withstand the compressive stresses without bending. lid to prevent liquid and vapor from escaping. The lid shall not
The surfaces against which the O-ring specimen is held shall contaminate the test liquid. Cover the lid with aluminum foil.
have a highly polished chromium-plated finish and shall be 12.12 Test Procedure—The test specimen shall be at room
cleaned thoroughly and wiped dry before each test. temperature when inserted in the compression device. Place the
assembled compression device, immersed in the test fluid, in
12.6 Original Thickness Measurement—Measure the origi-
the oven within 2 h after completion of the assembly, and allow
nal thickness of the specimen to the nearest 0.02 mm (0.001
it to remain there for the required test period at the test
in.). Place the specimen on the anvil of the micrometer so that
temperature. At the end of the test period, release the plates
the presser foot will indicate the thickness at the central portion
immediately and allow the specimens to cool to room tempera-
of the top and bottom faces. ture for 45 min in a fresh portion of the test liquid.
12.7 Application of Compressive Force—Place the O-ring 12.13 Final Thickness Measurement—After the rest period,
test specimen between the plates of the compression device measure the final thickness at the center of the test specimen in
with the spacers on each side, allowing sufficient clearance for accordance with Practice D 3767, Method A1.
the bulging of the O-ring when compressed. Where a lubricant 12.14 Calculate the compression set expressed as a percent-
is applied, it shall consist of a thin coating of the O-ring, with age of the original deflection as follows:
a lubricant having substantially no action on the rubber. For
C 5 [~to 2 tf!/~to 2 tn!# 3 100 (10)
most purposes, a silicone or fluorosilicone fluid is suitable.
Tighten the bolts so that the plates are drawn together uni- where:
formly until they are in contact with the spacers. The amount C = compression set expressed as percentage of the origi-
of compression employed shall be approximately 25 %. A nal deflection,
suitable mechanical or hydraulic device may be used to to = original thickness of specimen,
facilitate assembling and disassembling the test fixture. tf = final thickness of specimen, and
12.8 Test Temperature and Time—The test temperature shall tn = thickness of spacer bar used.
be the maximum anticipated service temperature. The test Record the value for C.
times shall be 72 h, 100 h, 250 h, 500 h, and 1000 h. In
comparative tests, use identical temperature and test periods. 13. Material Traceability and Compound Confirmation
12.9 Test Specimen—The test specimens should be O-rings 13.1 To provide full traceability of the compound being
molded from the same compound from which the actual seals qualified and to ensure that the compound and the state of cure
will be molded. The test samples should approximate the cross do not change during production, an FTIR spectrum of a
section of the actual seal to be used so that the fluid saturation randomly chosen qualification part shall be obtained in accor-
effect is properly considered. The test samples should be either dance with Test Methods D 3677. This spectrum appropriately
-021, -120, -214, or -320 O-rings. A minimum of two test dated and recorded shall remain part of the permanent record

5
 D 6546 – 00
for the qualified compound. Copies of this record should be 14.1.1 Date,
available for reference. 14.1.2 Cure date and batch number of the test specimens,
13.2 In addition, a TGA curve will be obtained for the same 14.1.3 Dates of the various periods of exposures,
sample in accordance with Test Method E 1131. This curve, 14.1.4 Immersion liquid used,
showing compositional analysis, will also be appropriately
14.1.5 Temperature of exposure,
dated and recorded and shall remain part of the permanent
record for the qualified compound. 14.1.6 Exposure period,
13.3 A Differential Scanning Calorimetry (DSC) curve, 14.1.7 All observed and recorded data, including the type of
confirming the degree of cure of the sample, will be obtained properties being reported,
in accordance with the procedure listed in Annex A1. This DSC 14.1.8 Results calculated in accordance with the preceding
curve will be properly dated and recorded and will also become procedures, and
part of the permanent record for the qualified compound. This 14.1.9 Conclusions of the tests based upon the compatibility
permanent record, documenting the qualified compound, shall limits listed in Section 9.
be used to confirm that production parts are made from the 14.2 The FTIR, TGA, and DSC results should be main-
same compound as qualified and that they are fully cured as tained on file for comparison to the results for production parts.
were the qualified elastomer parts.
13.4 To compare the FTIR spectra of production parts with 15. Precision and Bias
the qualified material, a view foil of each spectrum can be
15.1 The precision and bias of these test methods for
made and overlaid one atop the other. The major features of
measuring physical properties of new O-rings and O-rings after
both spectra should be identical. For TGA comparisons, the
exposure to industrial hydraulic fluids and thermal aging are
weight loss over specific temperature ranges for both the
essentially as specified in Test Methods D 1414, Practice
qualified elastomer sample and the production sample should
D 3677, and Test Method E 1131.
be the same and their curves identical in appearance. Identity
can again be evaluated using the view foil technique.
16. Keywords
14. Report 16.1 compatibility; density; elastomer seal; elongation; fluid
14.1 State that the test was conducted in accordance with aging; hardness; industrial hydraulic fluid; O-ring; tensile
Test Methods D 6546, and report the following: strength; volume shrinkage; volume swell; work function

ANNEXES

(Mandatory Information)

A1. TEST PROCEDURE FOR DETERMINING DEGREE OF CURE OF ELASTOMERS BY DIFFERENTIAL SCANNING
CALORIMETRY (DSC)

A1.1 Scope A1.2.5 Recording Charts, for temperature recording appa-

ratus with suitable graduation for measurements of energy
A1.1.1 This test method covers the determination of the
differential or time.
cure state of elastomers by DSC. It is based on Test Method
D 5028. This test method is applicable to elastomers with
A1.3 Calibration
adequate vulcanizers. The normal operating temperature range
is from room temperature to 250°C (482°F), but not limited to A1.3.1 Calibrate the apparatus in accordance with the
such. All elastomers should be fully cured. manufacturer’s instructions with appropriate standard refer-
ence materials at the same heating rate to be used for samples.
A1.2 Apparatus For the temperature range of this procedure, indium with a
melting point of 156°C (312.8°F) may be used.
A1.2.1 Differential Scanning Calorimeter, capable of heat-
ing a test specimen and a reference material at a controlled rate A1.4 Procedure
up to at least 20°C (68°F) per minute and of automatically
A1.4.1 Cured Elastomer Part:
recording the differential heat flow.
A1.4.1.1 Randomly select a cured elastomer part and ran-
A1.2.2 Specimen Holders, composed of clean aluminum or domly choose a small section of the part from its center, and
other high thermal conductivity material. Specimen holders weigh out 76.54 to 153.08 mg of the section.
may be of the open, covered, or sealed type. A1.4.1.2 Crimp a flat metal cover against the pan with the
A1.2.3 Nitrogen, or other inert purge gas supply. sample sandwiched between them to ensure good heat transfer.
A1.2.4 Flowmeter, for purge gas. Place the sample in the DSC cell.

6
 D 6546 – 00

FIG. A1.1 Thermogram Representative of an Uncured Elastomer

FIG. A1.2 Thermogram Representative of a Fully Cured Elastomer

A1.4.1.3 Intimate thermal contact between the sample and A1.4.1.5 Heat the sample at a rate of 10°C (50°F)/ min
the thermocouple is essential for reproducible results. under nitrogen atmosphere from ambient to a temperature high
A1.4.1.4 Purge the cell with nitrogen at 50 to 100 cc/min enough to achieve the entire exothermic curing curve. Record
(3.06 to 6.10 in.3/min) gas flow rate. the thermogram.

7
 D 6546 – 00
A1.4.1.6 Measure the heat of reaction (DHR), the shaded A1.6.1.2 Heating rate and purge gas flowrate,
area of Fig. A1.1 (see Figs. A1.1 and A1.2). A1.6.1.3 Value of DHR,
A1.6.1.4 Date of testing, and
A1.5 Calculation A1.6.1.5 Copies of the actual DSC curves.
A1.5.1 Use the resulting thermogram to determine the
exothermic heat of the curing reaction (DHR) of the cross- A1.7 Precision and Bias
linking reaction. This is used to indicate the extent of cure. A A1.7.1 Since this test method is designed to determine
fully cured material shall exhibit a DHR of 0 cal./gm (0 Btu/lb). whether a sample is fully cured or not, the heat of reaction
Fig. A1.2 depicts a fully cured material. (DHR) is the value of interest. If the value of DHR is positive,
A1.5.2 If the sample exhibits a DHR of 0 cal./gm (0 Btu/lb), then the sample is not fully cured. Calorimetric precision is
the sample is fully cured. If the sample exhibits a DHR of normally 61 % and calorimetric accuracy is also 61 %, but
greater than 0 cal./gm (0 Btu/lb) (see Fig. A1.1), run a duplicate fully cured materials have no exotherm. What is important in
sample. If the duplicate sample yields a DHR of 0 cal./gm (0 determining if a material is fully cured is the stability of the
Btu/lb), run a third sample such that two independent runs are baseline because any positive value above baseline can be
in agreement. If the duplicate sample yields a DHR greater than interpreted as an exotherm. Baseline noise for these types of
0 cal./gm (0 Btu/lb), the elastomer part is not fully cured and instruments is 0.00431 cal (0.0000171 Btu). Baseline noise
processing is not consistent. during a run can in effect create a positive indication. If the
maximum baseline noise value is divided by the minimum
A1.6 Report sample weight, 76.54 mg, than a baseline maximum deviation
A1.6.1 Report the following information: of 0.0563 cal/gm can be expected. Therefore, any test value
A1.6.1.1 Sample identification including compound and that ranged from 0 to +0.0563 cal/gm would be equivalent to
batch inside diameter and mass, fully cured material.

A2. SIZES OF O-RINGS USED IN TEST PROCEDURES

A2.1 Table A2.1 lists the actual sizes of the O-rings used in TABLE A2.1 O-ring Sizes
the test methods. The sizes are in accordance with AS568A. AS568A Inside Cross Section, in. Inside Diameter Cross
Designation Diameter (mm) Section, mm
(in.)
-021 0.926 6 0.009 0.070 6 0.003 23.52 6 0.23 1.78 6 0.08
-120 0.987 6 0.010 0.103 6 0.003 25.07 6 0.25 2.62 6 0.08
-214 0.984 6 0.010 0.139 6 0.004 24.99 6 0.25 3.53 6 0.10
-320 1.100 6 0.012 0.210 6 0.005 27.94 6 0.30 5.33 6 0.13

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