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An American National Standard

Designation: D 5662 – 99

Standard Test Method for


Determining Automotive Gear Oil Compatability with Typical
Oil Seal Elastomers1
This standard is issued under the fixed designation D 5662; 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 3. Terminology
1.1 This laboratory test method2 covers the determination of 3.1 Definitions of Terms Specific to This Standard:
the compatibility of automotive gear oils with specific nitrile, 3.1.1 dumbbell, n—the specific cut shape (Die C) of an
polyacrylate, and fluoroelastomer oil seal materials. elastomer as explained in Section 13 of Test Methods D 412.
1.2 Users of this test method should obtain Test Methods 3.1.2 formulation, n—the specific chemical composition
D 412, D 471, and D 2240 and become familiar with their use used in manufacturing a seal elastomer or a reference oil.
before proceeding with this test method. 3.1.3 percent ultimate elongation, n—the stretch length at
1.3 The values stated in either SI units or inch pound units rupture of an elastomer dumbbell oil-aged by running this
are to be regarded separately as standard. The values stated in procedure minus the rupture stretch length of an untested
each system are not exact equivalents; therefore, each system dumbbell, all divided by rupture stretch length of the untested
shall be used independently of the other. dumbbell and then multiplied by 100.
1.4 This standard does not purport to address all of the 3.1.4 percent volume change, n—the change in volume of a
safety concerns, if any, associated with its use. It is the test specimen as explained in Section 10 of Test Method D 471.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4. Summary of Test Method
bility of regulatory limitations prior to use. 4.1 Non-reference oils are tested using a modified version of
Test Method D 471 on specific elastomer compounds. Mea-
2. Referenced Documents sured quantities are percent ultimate elongation changes (fur-
2.1 ASTM Standards: ther referred to as just percent elongation changes), durometer
D 412 Test Methods for Vulcanized Rubber and Thermo- Type A hardness changes, and percent volume changes. Ref-
plastic Rubbers and Thermoplastic Elastomers—Tension3 erence oils are run concurrently in the same oil bath to measure
D 471 Test Method for Rubber Property—Effect of Liq- consistency from one test to another.
uids3 4.2 The duration of these tests is 240 h. Table 1 shows the
D 2240 Test Method for Rubber Property—Durometer types of seal materials and their associated test reference oils
Hardness3 and temperatures. The reference oils are available from the
D 5704 Test Method for Evaluation of the Thermal and ASTM Test Monitoring Center (TMC).5 The seal materials are
Oxidative Stability of Lubricating Oils Used for Manual available through a Central Parts Distributor (CPD).6
Transmissions and Final Drive Axles4
D 5760 Specification for Performance of Manual Transmis- 5. Significance and Use
sion Gear Lubricants4 5.1 There are several major causes of automotive lubricant-
related seal failures. This test method addresses only those
failures caused by excessive elastomer hardening, elongation
1
This test method is under the jurisdiction of ASTM Committee D-2 on loss, and volume swell and attempts to determine the likeli-
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.B0.03 on Gear Lubricants. hood that an oil might cause premature sealing system failures
Current edition approved June 10, 1999. Published August 1999. in field use. This test method may be used as a requirement of
Originally published as D 5662 – 95. Last previous edition D 5662 – 98.
2
a performance specification, such as Specification D 5760.
Until the next revision of this test method, the ASTM Test Monitoring Center
will update changes in this test method by means of Information Letters; these can
be obtained from the ASTM Test Monitoring Center, 6555 Penn Ave., Pittsburgh, Pa
5
15206–4489. Attention: Administrator. This edition incorporates revisions in all Reference oils are available from the ASTM Test Monitoring Center, 6555 Penn
Information Letters through No. 98–1. Ave., Pittsburgh, PA 15206-4489.
3 6
Annual Book of ASTM Standards, Vol 09.01. The Central Parts Distributor for this procedure is Test Engineering Inc., 12758
4
Annual Book of ASTM Standards, Vol 05.03. Cimarron Path, Suite 102, San Antonio, TX 78249.

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

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D 5662 – 99
TABLE 1 Seal Materials, Reference Oils, and Test Temperatures 7.2.1 Information and location of the current CPD is also
Seal Material Reference Oils
Test available from the TMC.
Temperature 7.3 Specific reference seal elastomers used are a nitrile (NI),
Nitrile No. 161, No. 162 100°C a polyacrylate (PA), and a fluoroelastomer (FL). Notation of
Polyacrylate No. 160, No. 161 150°C
Fluoroelastomer No. 160, No. 161 150°C
the numbering system is established by the TMC as follows:
[Type] Y – X
where:
5.2 Another major cause of seal failure is the formation of Type = NI, PA, FL,
carbon, varnish, and sludge-like deposits on the seal lip. The Y = specific formulation of the elastomer type, and
deposit-forming characteristics of automotive gear oils are X = batch number of the particular formulation.
evaluated in Test Method D 5704. That procedure is intended 7.4 The shelf life for the seal elastomers is two years from
in part to evaluate the potential for oils to cause premature seal the date the batch was cured. Invalidate any test with a seal
failure in field service. cure date older than two years.
7.4.1 Store the elastomers in a cool, dark, and dry place. The
6. Apparatus preferred method of storage is a refrigerator maintained at 38
6.1 Specific test equipment as outlined in Test Methods to 42°F (3 to 6°C).
D 412, D 471, and D 2240 is required. 7.5 The shelf life of reference oils is typically five years
6.1.1 Hardness Durometer—See Test Method D 2240. unless the TMC, through their analysis, specifies otherwise.
6.1.1.1 Calibration—Calibrate the hardness durometer an- 7.6 Wetting solution of Aerosol OT—0.1 % sodium diocytl
nually. Use an outside source, with standards traceable to sulfosuccinate, made by a 1.0 % dilution of a 10 % solution
National Institute for Standards Technology (NIST) for annual with reagent water.
calibration. Perform checks with internal standards weekly.
Checks with internal standards shall be within 6 3 points. 8. Procedure
Calibrate internal standards annually, using an outside source, 8.1 The testing laboratory shall conduct reference oil tests
with standards traceable to NIST. concurrently with the non-reference oil in the same oil bath.
6.1.2 Tension Testing Machine—See Test Method D 412. Reference oils shall perform within a specific range prescribed
Set the testing machine rate of grip separation for the percent and evaluated by TMC for validity and updated as needed.
elongation change determinations at 8.5 6 0.8 mm/s. 8.2 Prior to cutting specimens and prior to performing
6.1.2.1 Calibration—Calibrate the tension testing machine elongation tests for initial properties, allow 3 h for the
annually. Annual calibration shall be performed by the manu- elastomer to warm to 23+ 2°C, as required by Test Method
facturer, using NIST traceable standards. D 412. Referring to the procedure in Test Method D 412, use
6.1.3 Glass Tubes, having an outside diameter of 38 mm and Die C to cut a set of twelve dumbbell specimens out of the
an overall length of 300 mm. The tube is fitted loosely with an elastomer sheets as required for each reference and non-
aluminum foil-covered stopper. reference oil tested.
6.1.4 Balance—Use any commercially available balance 8.2.1 Cut the dumbbells parallel to the grain using the same
capable of weighing samples to the nearest 1.0 mg. unaltered dies for the entire lot. When cutting dumbbells, only
6.1.4.1 Calibration—Calibrate the balance annually. Use an cut one thickness at a time to avoid any dimensional variations.
outside source, with standards traceable to NIST for annual 8.2.2 Cut all elastomer specimens, including those used for
calibration. Perform checks with internal standards monthly, measuring initial properties, from the same elastomer batch.
using NIST traceable weights. The difference between the Use these dumbbells for measuring the percent elongation
weights and balance shall be < 0.5 mg. Calibrate internal changes.
standards annually, using an outside source, with standards 8.2.3 Next, cut twelve 25 by 50 by 2.0 6 0.1-mm (1 by 2 by
traceable to NIST. 0.08 6 0.005-in.) rectangular specimens for the percent vol-
ume change and hardness testing.
7. Reagents and Materials 8.2.4 Finally, cut twelve more NI, PA, and FL dumbbells for
7.1 Specific reference test oils are maintained and distrib- the purpose of determining initial elongation properties.
uted by the TMC.5 The oils used are labeled No. 160, No. 161,
and No. 162, or current equivalent. To receive the test oils and
TABLE 2 Elastomer Specimens Required
seal materials, individual laboratories shall commit to furnish-
ing the TMC with reference data developed using these Nitrile Polyacrylate Fluoroelastomer
Purpose
reference materials. The TMC is also responsible for managing Dumb- Speci- Dumb- Speci- Dumb- Speci-
bells mens bells mens bells mens
a system that ensures the performance and formulation con-
cerning these reference oils. Oil No. 160 0 0 12 12 12 12
Oil No. 161 12 12 12 12 12 12
7.2 The CPD is responsible for maintaining the numbering Oil No. 162 12 12 0 0 0 0
and tracking system for the seal elastomer batches used. Non-reference 12 each 12 each 12 each 12 each 12 each 12 each
Certain specific information concerning these reference mate- Initial Properties 12 0 12 0 12 0
Totals for a Single 48 36 48 36 48 36
rials is available only to the CPD. This information is used to Non-reference
ensure batch-to-batch consistency.

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D 5662 – 99
8.2.5 Use Table 2 as a guide to determine the number of
elastomer specimens required.
8.2.6 Randomly select sets of twelve dumbbells and twelve
rectangular specimens for testing from the different sheets of
test elastomers.
8.2.7 Use the following water displacement procedure in
accordance with Test Method D 471 to conduct the initial and
final volume measurements. Weigh the coupon in air, M1, to
the nearest 1 mg. Making sure there are no air bubbles clinging
to the surface, immerse the rectangular specimen into a 1.0 %
wetting solution of aerosol OT before weighing it in distilled
water, M2, at ambient temperature.
8.2.8 Ensure that initial elastomer properties of hardness
and volume are determined prior to the start of testing. Initial
elongation properties are determined just prior to running the
end of test dumbbells because of instrument calibration. FIG. 2 Test Tube Arrangement
8.3 Fill the test tubes with 150 65 mL of non-reference or
reference oil as appropriate.
8.3.1 See Table 1 for combinations of reference test oils and 8.5 At the end of the test period, remove the specimens from
seal materials required for testing. Test the non-reference oil the hot oil using the wire hanger and place them on a clean
using one or more of the three different seal elastomers. absorbent towel. Allow the specimens to cool for no longer
8.4 Use four test tubes for each elastomer/oil combination. than 30 min.
In each tube, suspend from a stainless steel wire hanger bent at 8.5.1 Remove the specimens from the wire hanger, and
a 90° angle (dimensions shown in Fig. 1) three rectangular place them on a clean absorbent towel. Remove the excess oil
specimens and three dumbbells in each of the four tubes. Place with a clean absorbent towel, and begin testing.
3.0 to 5.0-mm spacers in between the specimens to aid in the 8.6 Complete testing for durometer Type A hardness, per-
separation. The spacer material shall not affect the liquid or the cent volume, and percent elongation changes within 2 h of
rubber. removal from the test oil.
8.4.1 Fig. 2 shows the arrangement of spacers and test 8.7 Observe the following notes/modifications to Test
specimens. Method D 471.
8.4.2 Top the test tube with a stopper wrapped in aluminum 8.7.1 Report percent change in elongation (see Test Method
foil. D 412) and percent volume change (see Test Method D 471)
8.4.3 See Table 1 for the combinations of reference test oils from the original using the same water displacement procedure
and seal materials required for testing. Test the non-reference described in 8.2.7.
oil using one or more of the three different seal elastomers with 8.7.2 Report durometer Type A hardness change points from
the same batch of elastomers as being used for the reference original (see Test Method D 2240).
oil. 8.7.2.1 On a hard horizontal surface, stack the three rectan-
8.4.4 Place the tubes randomly in an oil bath capable of gular specimens on top of each other to obtain the 6-mm
maintaining a test oil temperature (see Table 1) within 61°C thickness required by Test Method D 2240. Hardness readings
for a period of 240 6 0.5 h. are to be taken 1 s after the pin makes contact with the
8.4.5 Conduct all reference and non-reference oil testing on elastomer. Take three readings on each side of the rectangular
each seal elastomer in the same oil bath. Complete reference specimen and report the average of all six readings.
oil and non-reference oil tests for each seal elastomer within 8 8.7.2.2 After taking the first set of measurements, rotate the
h of each other to be considered the same test. bottom specimen to the top of the stack and take a second set
of measurements.
8.7.2.3 Rotate the bottom specimen to the top one more time
to obtain the third set of measurements.
8.7.3 For each data set, calculate the average value and the
sample standard deviation using the equation:
s 5 @num#1@den#N – 1 @end#Ni51 ~xi – x!2 (1)

where:
s = sample standard deviation,
N = number of data points in the set,
XI = individual data set value,
? A/X! = mean of the data set, and
I = index to denote one of a set of data.
Change in volume, % = [(M3 – M4)–(M1 – M2)]/(M1 –
FIG. 1 Wire Hanger M2)3 d 3 100

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D 5662 – 99

where: 9.1.4 End of test date,


M1 = the original weight in air, 9.1.5 Elastomer batch date and code,
M2 = the original weight in water, 9.1.6 Oil bath identification, and
M3 = the end of test weight in air, 9.2 Report to the TMC the information identified in 9.1 for
M4 = the end of test weight in water, and the reference oils only.
d = the density of the medium in which the specimen was
weighed. In this case water is used, so the multipli- 10. Precision and Bias
cation is by 1. 10.1 Precision data are being developed for this test method.
8.8 Excessive Data Variability—Criteria for determining Test precision is established on the basis of reference oil test
test validity, consistent with accepted industry standards, are results (for operationally valid tests) monitored by the ASTM
currently being developed by the task force in conjunction with TMC. The research report contains industry precision data as
the TMC. Should the reference test be determined to be invalid, of Nov. 19, 1993.7 See also Annex A1.
repeat all testing on that particular oil/elastomer pair. 10.2 No estimate of the bias for this procedure is possible
because the performance results for an oil are determined only
9. Report under the specific conditions of the test and no absolute
9.1 Use the Final Report Forms (Annex A2) to report both standards exist.
the reference oil and non-reference oil test results. Report the
data as specified in the Data Dictionary (Annex A3). Report the 11. Keywords
following information: 11.1 compatibility; elastomer; elongation change; gear oil;
9.1.1 Percent elongation changes (see Test Methods D 412), hardness change points; oil seal; volume change
9.1.2 Percent volume changes (see Test Method D 471),
9.1.3 Type A durometer hardness change points (see Test
Method D 2240), 7
Available from ASTM Headquarters. Request RR: D02-1348.

ANNEXES

(Mandatory Information)

A1. THE ROLE OF THE TEST MONITORING CENTER

A1.1 The ASTM Test Monitoring Center (TMC) is a are balloted in Subcommittee D02.B. This ballot is reviewed at
nonprofit organization located at 6555 Penn Ave., Pittsburgh, the Subcommittee D02.B meeting, and the actions taken are
PA 15206-4489. It is staffed to administer engineering studies; then considered by Committee D-2. In this way, the ASTM due
conduct laboratory visits; perform statistical analyses of tests; process procedures are applied to the Information Letters.
to blend, store, and ship reference oils; and to provide A1.2.2 The review of an Information Letter prior to its
associated administrative functions connected with the refer- original issue will differ in accordance with its nature. In the
encing and calibration of various lubricant tests. The TMC case of an Information Letter that does not affect test results,
maintains a close connection with test sponsors, test develop- such as notification of a part number change, the TMC is
ers, the surveillance panels, and the testing laboratories. The authorized to issue an Information Letter. A survey or study
management of these functions is vested in the Test Monitoring conducted by the Surveillance Panel resulting in a recommen-
Board, whose members are elected by Subcommittee D02.B. dation for a change in hardware or procedure may result in the
The TMC operates under the ASTM Charter and its associated issuance of an Information Letter. If urgent changes to hard-
bylaws and regulations, the bylaws of Committee D-2 and of ware or procedure are obviously necessary, the test sponsor and
Subcommittee D02.B, and the Rules and Regulations of the the TMC may issue an Information Letter and present it for
Test Monitoring Board. The operating income of the TMC is approval, with the background and data, for approval by the
obtained from fees levied on the reference oils supplied and on Surveillance Panel prior to the next semiannual D-2 meeting.
the conduct of the calibration tests. These fees are set by A1.2.3 Authority for the issue of Information Letters was
Subcommittee D02.B and are regularly reviewed. given by the Committee on Technical Committee Operations
(COTCO) in 1984, as follows:
A1.2 Information Letters: NOTE A1.1—“COTCO recognizes that D-2 has a unique and complex
A1.2.1 It occasionally becomes necessary to change a test situation. The use of Information Letters is approved provided that each
letter (at its initial issue) contains a disclaimer to the effect that it has not
procedure and to notify test laboratories of the change before
obtained ASTM consensus. These Information Letters should be moved to
the change can be considered by Subcommittee D02.B on such consensus as rapidly as possible.”
Automotive Lubricants or Committee D-2 on Petroleum Prod-
ucts and Lubricants. In such a case the TMC will issue an A1.3 Test Monitoring Center Memoranda—In addition to
Information Letter. Subsequently, prior to each semi-annual the Information Letter system, the TMC will provide informa-
Committee D-2 meeting, the accumulated Information Letters tion to the Surveillance Panel and to participating laboratories

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D 5662 – 99
in the form of ASTM TMC memoranda. These memoranda are test performance, results, or precision and bias.
used to convey such information as batch approvals for test
parts or materials, to clarify misunderstandings concerning the A1.4 Precision Data—Test precision is established on the
test procedure, to provide notes and suggestions for the basis of reference oil (calibration) test results monitored by the
collection and analysis of special data for which the TMC may ASTM TMC. Current data may be obtained from the TMC.
call for, or for any other matters having no direct effect on the

A2. FINAL REPORT FORMS

A2.1 The final report forms for reporting reference and through Form 6) are used for the three types of elastomer
non-reference oil test results are provided as Figs. A2.1-A2.8. materials.
Three sets of reference and non-reference forms (Form 1

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D 5662 – 99

FIG. A2.1 Test Report Cover

6
D 5662 – 99

FIG. A2.2 Reference Oil Results - Fluoroelastomer

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D 5662 – 99

FIG. A2.3 Non-reference Oil Test Results - Fluoroelastomer

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D 5662 – 99

FIG. A2.4 Reference Oil Test Results - Polyacrylate

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D 5662 – 99

FIG. A2.5 Non-reference Oil Test Results - Polyacrylate

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D 5662 – 99

FIG. A2.6 Reference Oil Test Results - Nitrile

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D 5662 – 99

FIG. A2.7 Non-reference Oil Test Results - Nitrile

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D 5662 – 99

FIG. A2.8 Comments

A3. DATA DICTIONARY

A3.1 The data dictionary is given in Figs. A3.1-A3.5.

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D 5662 – 99

FIG. A3.1 Data Dictionary

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D 5662 – 99

FIG. A3.2 Data Dictionary

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D 5662 – 99

FIG. A3.3 Data Dictionary Repeating Field Specifications

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D 5662 – 99

FIG. A3.4 Data Dictionary Repeating Field Specifications

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D 5662 – 99

FIG. A3.5 Data Dictionary Repeating Field Specifications

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D 5662 – 99

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

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