ASTM D4289-97

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4289 – 97 An American National Standard
Standard Test Method for
Elastomer Compatibility of Lubricating Greases and Fluids
This standard is issued under the fixed designation D 4289; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D 297 Test Methods for Rubber Products—Chemical
Analysis
1.1 This test method evaluates the compatibility of lubricat-
D 412 Test Methods for Vulcanized Rubber and Thermo-
ing greases and fluids with coupons cut from standard elas-
plastic Elastomers—Tension
tomer sheets (Practice D 3182) or, optionally, from SAE
D 471 Test Method for Rubber Property—Effect of Liq-
Specification AMS 3217/2A (NBR-L) and AMS 3217/3A (CR)
uids
sheets. Compatibility is evaluated by determining the changes
D 1193 Specification for Reagent Water
in volume and Durometer A hardness that occur when elas-
D 2240 Test Method for Rubber Property—Durometer
tomer coupons are totally immersed in a lubricant sample for
Hardness
70 h at either 100 or 150°C or as required by the lubricant
D 3182 Practice for Rubber—Materials, Equipment, and
specification.
Procedures for Mixing Standard Compounds and Prepar-
1.1.1 Some lubricant specifications may require different
ing Standard Vulcanized Sheets
test conditions, such as longer durations or lower or higher
D 3183 Practice for Rubber—Preparation of Pieces for Test
temperatures. In such instances, the repeatability and reproduc-
Purposes from Products
ibility values stated in Section 12 do not apply, and the user and
D 4175 Terminology Relating to Petroleum, Petroleum
supplier should agree on acceptable limits of precision.
Products, and Lubricants
NOTE 1—The scope of this test method now includes the evaluation of
D 4950 Classification of and Specification for Automotive
the elastomer compatibility of both lubricating fluids and greases. Testing
Service Greases
of fluids was not included in Test Method D 4289 – 95 and earlier
2.2 Federal Standard:
versions.
Federal Test Method Standard 791C, Method 3603.5,
1.2 This test method can also be used as a guide to evaluate
Swelling of Synthetic Rubbers
the compatibility of greases with rubber products not in
2.3 U.S. Air Force Specification:
standard sheet form (Practice D 3183).
539 Specification Bulletin for Standard Elastomer Stocks
1.3 The values stated in SI and Durometer A units shall be
2.4 SAE Standards:
regarded as the standard.
AMS 3217A Standard Elastomer Stocks—Test Slabs
1.4 This standard does not purport to address all of the
AMS 3217/2A Test Slabs, Acrylonitrile Butadiene (NBR-
safety concerns, if any, associated with its use. It is the
L)—Low Acrylonitrile, 65–75
responsibility of the user of this standard to establish appro-
AMS 3217/3A Test Slabs, Chloroprene (CR)—65–75
priate safety and health practices and determine the applica-
NOTE 2—USAF Specification Bulletin 539 was specified in Test
bility of regulatory limitations prior to use. For specific hazard
Method D 4289 – 94 and earlier versions. This specification is obsolete
statements, see Note 6, Note 7, and Note 8.
and has been replaced by SAE Standard AMS 3217A. USAF-539 NBR-L
has been replaced by SAE AMS 3217/2A (NBR-L), which is virtually
2. Referenced Documents
identical. USAF-539 CR has been replaced by the similar, but not
2.1 ASTM Standards:
identical, SAE AMS 3217/3A (CR). Elastomer sheets prepared to this
D 217 Test Methods for Cone Penetration of Lubricating
Grease
Annual Book of ASTM Standards, Vol 09.01.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 05.02.
Annual Book of ASTM Standards, Vol 05.03.
1 7
This test method is under the jurisdiction of ASTM Committee D-2 on Available from Standardization Documents Order Desk, Bldg. 4, Section D,
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
D02.G0 on Lubricating Grease. USAF Specification Bulletin 539 is obsolete, but reproductions are available by
Current edition approved June 10, 1997. Published August 1997. Originally requesting RR: D02-1165 from ASTM Headquarters.
published as D 4289 – 89. Last previous edition D 4289 – 95. Available from Society of Automotive Engineers, 400 Commonwealth Drive,
Annual Book of ASTM Standards, Vol 05.01. Warrendale, PA 15096.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 4289
latter specification are not known or expected to provide test results
M1 = initial mass of coupon in air, g,
identical with those of the USAF Specification 539 counterpart.
M2 = initial mass of coupon and hanger wire in water less
mass of hanger wire partially submerged in water, g,
3. Terminology
M3 = final mass of coupon in air, g,
3.1 Definitions:
M4 = final mass of coupon and hanger wire in water less
3.1.1 elastomer, n—a natural or synthetic polymer having
mass of hanger wire partially submerged in water, g.
the rubber-like property of substantially recovering its size and
4. Summary of Test Method
shape after removal of a deforming force.
3.1.2 hardness, n—of an elastomer, the resistance to defor-
4.1 A prepared elastomer coupon is measured for initial
mation or indentation.
hardness (Durometer A), density or relative density (to ensure
3.1.2.1 Discussion—In this test method the hardness of an
that the coupon is within specified limits), and volume by water
elastomer is measured with a Shore Durometer A (see Test
displacement. The coupon is immersed in test grease or fluid
Method D 2240).
and aged for 70 h at either 100°C (for chloroprene and similar
3.1.3 lubricant, n—any material interposed between two
flex-resistant elastomers) or 150°C (for nitrile and similar
surfaces that reduces the friction or wear between them.
heat-resistant elastomers) or at other conditions as required by
D 4175
the lubricant specification. The resulting changes in hardness
3.1.4 lubricating grease, n—a semifluid to solid product of
and volume are determined.
a dispersion of a thickener in a liquid lubricant.
5. Significance and Use
3.1.4.1 Discussion—The dispersion of the thickener forms a
two-phase system and immobilizes the liquid lubricant by 5.1 Measurement of the changes in the volume and hardness
surface tension and other physical forces. Other ingredients
of an elastomer that occur from immersion in a lubricating
imparting special properties are often included. D 217 grease or fluid provides a means for evaluating relative
3.1.5 relative density, n—the ratio of the density of a
compatibility. Much of this test method was derived from
material at temperature, t , to the density of water at a reference procedures described in Test Method D 471 and Federal Test
temperature, t .
Method 791C/3603.5. In contrast to these two test methods,
3.1.5.1 Discussion—In this test method relative density is which emphasize the evaluation of rubber and rubber-like
determined with the temperature of the elastomer and water compounds, Test Method D 4289 was developed specifically to
being equal and within the range from 20 to 25°C, and the evaluate lubricating greases and fluids, especially those used in
temperature correction for the density of water is not applied. automotive applications, although the test method can be
The term, relative density, replaces the synonymous, depre- applied to lubricants used in industrial applications as well.
cated term, specific gravity, used in some earlier editions of this Excepting the Shore Durometer A, this test method requires no
test method. specialized, rubber-testing equipment. Virtually all other
3.1.6 thickener, n—in a lubricating grease, a substance equipment and supplies specified in the procedure are stock
composed of finely divided particles dispersed in a liquid items in lubricants laboratories.
lubricant to form the product’s structure. 5.2 The volume and hardness-change values determined by
this test method do not duplicate similar changes that occur in
3.1.6.1 Discussion—The thickener can be fibers (such as
various metallic soaps) or plates or spheres (such as certain elastomeric seals under actual service conditions. However,
they can be correlated in many instances. In one such instance,
non-soap thickeners) which are insoluble or, at most, only very
the volume-change values determined by the antecedent of this
slightly soluble in the liquid lubricant. The general require-
test method correlated (r = 0.99) with those that occurred
ments are that the solid particles be extremely small, uniformly
during a vehicle test. Because of wide variations in service
dispersed, and capable of forming a relatively stable, gel-like
conditions and differences in grease and elastomer formula-
structure with the liquid lubricant. D 217
tions, correlations between the results obtained with this test
3.2 Definitions of Terms Specific to This Standard:
method and particular applications should be determined on an
3.2.1 coupon, n—a test piece of specified dimensions cut
individual basis.
from standard elastomer sheets (Practice D 3182).
5.3 When the optional Reference Elastomers AMS 3217/2A
3.3 Symbols:
(acrylonitrile-butadiene, NBR-L) and AMS 3217/3A (chloro-
3.3.1 Symbols used in the calculation of hardness change
prene, CR) are used to evaluate compatibility, the results can be
(see Eq 1 in 10.1):
used to judge a service characteristic of lubricants. In this
respect, this test method is useful for lubricant specifications
DH = hardness change, Durometer A units,
(for example, Specification D 4950). Similarly, this test method
H = initial hardness, Durometer A units,
i
can be used in specifications for lubricating fluids as well.
H = final hardness, Durometer A units.
f
5.4 With specifications requiring elastomers other than Ref-
3.3.2 Symbols used in the calculation of relative density
erence Elastomers AMS 3217/2A or AMS 3217/3A, coupons
(see Eq 2 in 10.2) and volume change (see Eq 3 in 10.3):
cut from standard sheets (Practice D 3182) should be used.
RD = relative density,
Verdura, T. M., “Evaluating Compatibility of Greases with Elastomeric Seals,”
DV = volume change, %,
NLGI Spokesman, Vol 42, 1978, pp. 20–29.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 4289
When the preparation of such coupons is not feasible, or the (approximately 8-mm gape) at the other.
lubricant specification requires the use of rubber products that 7.5 Coupon Suspension Wire, stainless steel, about 0.71 to
do not have a suitable size or configuration for use in preparing 0.72-mm diameter (No. 22 U.S. Steel Wire Gage or Imperial
coupons for testing (Practice D 3183), this test method can be Wire Gage), configured as shown in Fig. 1, to suspend the
used as a guide for evaluating compatibility. coupon below the surface of a fluid sample.
7.6 Laboratory Oven, circulating-air type, capable of main-
NOTE 3—Inasmuch as the precision values apply only to the elastomers
taining the test temperature within6 2.5°C and equipped with
specified in Annex A1 of Test Method D 4289, when a lubricant
one or more grill-type, wire shelves.
specification requires some other elastomer, the user and supplier of the
7.7 Shore Durometer A, stand-mounted type (see Test
lubricant should agree to the values of acceptable precision. Such values
may or may not be the same as those of Test Method D 4289. It is
Method D 2240).
recommended that the agreed upon precision values be stated in the user’s
7.8 Coupon Cutting Die, optional, as shown in Fig. 2
lubricant specification.
(recommended).
5.5 The results of this test method are most applicable to the
use of lubricating greases and fluids in contact with elastomeric
seals, boots, O-rings, and similar products, where the physical
demands on the elastomer are not extreme. In critical applica-
tions where the lubricant will be in contact with rubber parts
subject to severe flexing, extreme temperatures, or similar
stresses, other rubber properties, such as tensile strength and
elongation, should also be evaluated as they may be more
indicative of the true compatibility characteristics.
6. Interferences
6.1 Caution—Although greases and elastomers typically
have long shelf lives, there is potential for change in time.
Therefore, in order to ensure acceptable precision in this test
method, neither test greases nor test elastomers should be more
than approximately one year old.
6.1.1 Before testing with Reference Elastomers stored for
extended periods (approaching one year or more) or in an
FIG. 2 Coupon Cutting Die (Optional)
adverse environment (high ambient temperatures, solvent va-
pors, and so forth), the elastomers should be checked for
conformance with the requirements in Table A1.1.
8. Reagents and Materials
NOTE 4—Experience has shown that storage conditions can affect the
8.1 Purity of Reagents—It is intended that reagent grade
shelf life of the reference elastomers. Shelf life can be extended by storing
chemicals be used in all tests. Unless otherwise indicated, all
elastomers in the dark in an inert atmosphere (such as a glass or metal, but
reagents shall conform to the specifications of the Committee
not plastic, container, for example, vacuum desiccator, in which the air has
on Analytical Reagents of the American Chemical Society,
been replaced by nonreactive gas (such as argon or nitrogen) at refrigera-
where such specifications are available. Other grades may be
tor temperatures. Elastomers should not be stored at temperatures lower
than 5°C because of crystallinity and solubility changes that can affect test
used, provided it is first ascertained that the reagent is of
performance. Neither should they be stored at reduced pressures or in
permeable containers or wrappers which could allow them to be affected
by the normal atmosphere.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
7. Apparatus
listed by the American Chemical Society, see Analar Standards for Laboratory U.K.
7.1 Sample Beaker, heat-resistant glass, Griffin low form,
Chemicals, BDH Ltd., Poole, Dorset, and the
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