ASTM D4289-03(2008)
(Test Method)Standard Test Method for Elastomer Compatibility of Lubricating Greases and Fluids
Standard Test Method for Elastomer Compatibility of Lubricating Greases and Fluids
SIGNIFICANCE AND USE
Measurement of the changes in the volume and hardness of an elastomer that occur from immersion in a lubricating grease or fluid provides a means for evaluating relative compatibility. Much of this test method was derived from procedures described in Test Method D 471 and Federal Test Method 791C/3603.5. In contrast to these two test methods, which emphasize the evaluation of rubber and rubber-like compounds, Test Method D 4289 was developed specifically to evaluate lubricating greases and fluids, especially those used in automotive applications, although the test method can be applied to lubricants used in industrial applications as well. Excepting the Shore Durometer A, this test method requires no specialized, rubber-testing equipment. Virtually all other equipment and supplies specified in the procedure are stock items in lubricants laboratories.
The volume and hardness-change values determined by this test method do not duplicate similar changes that occur in elastomeric seals under actual service conditions. However, they can be correlated in many instances. In one such instance, the volume-change values determined by the antecedent of this test method correlated (r 2 = 0.99) with those that occurred during a vehicle test. Because of wide variations in service conditions and differences in grease and elastomer formulations, correlations between the results obtained with this test method and particular applications should be determined on an individual basis.
When the optional Reference Elastomers AMS 3217/2B (acrylonitrile-butadiene, NBR-L) and AMS 3217/3A (chloroprene, CR) are used to evaluate compatibility, the results can be used to judge a service characteristic of lubricants. In this respect, this test method is useful for lubricant specifications (for example, Specification D 4950). Similarly, this test method can be used in specifications for lubricating fluids as well.
With specifications requiring elastomers other than Reference Elastomers AMS 3...
SCOPE
1.1 This test method evaluates the compatibility of lubricating greases and fluids with coupons cut from standard elastomer sheets (Practice D 3182) or, optionally, from SAE Specification AMS 3217/2B (NBR-L) and AMS 3217/3A (CR) sheets. Compatibility is evaluated by determining the changes in volume and Durometer A hardness that occur when elastomer coupons are totally immersed in a lubricant sample for 70 h at either 100 or 150°C or as required by the lubricant specification.
1.1.1 Some lubricant specifications may require different test conditions, such as longer durations or lower or higher temperatures. In such instances, the repeatability and reproducibility values stated in Section 12 do not apply, and the user and supplier should agree on acceptable limits of precision.
Note 1—The scope of this test method now includes the evaluation of the elastomer compatibility of both lubricating fluids and greases. Testing of fluids was not included in Test Method D 4289–95 and earlier versions.
1.2 This test method can also be used as a guide to evaluate the compatibility of greases with rubber products not in standard sheet form (Practice D 3183).
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 Exception—When listed, Durometer A units shall be regarded as the standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.For specific warning statements, see 8.4-8.6.
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Designation: D4289 − 03(Reapproved 2008)
Standard Test Method for
Elastomer Compatibility of Lubricating Greases and Fluids
This standard is issued under the fixed designation D4289; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 Department of Defense.
1. Scope bility of regulatory limitations prior to use.Forspecificwarning
statements, see 8.4-8.6.
1.1 This test method evaluates the compatibility of lubricat-
ing greases and fluids with coupons cut from standard elasto-
2. Referenced Documents
mer sheets (Practice D3182) or, optionally, from SAE Speci-
2.1 ASTM Standards:
fication AMS 3217/2B (NBR-L) and AMS 3217/3A (CR)
D217Test Methods for Cone Penetration of Lubricating
sheets. Compatibility is evaluated by determining the changes
Grease
in volume and Durometer A hardness that occur when elasto-
D297Test Methods for Rubber Products—ChemicalAnaly-
mer coupons are totally immersed in a lubricant sample for 70
sis
h at either 100 or 150°C or as required by the lubricant
D412TestMethodsforVulcanizedRubberandThermoplas-
specification.
tic Elastomers—Tension
1.1.1 Some lubricant specifications may require different
D471Test Method for Rubber Property—Effect of Liquids
test conditions, such as longer durations or lower or higher
D1193Specification for Reagent Water
temperatures.Insuchinstances,therepeatabilityandreproduc-
D2240TestMethodforRubberProperty—DurometerHard-
ibilityvaluesstatedinSection12donotapply,andtheuserand
ness
supplier should agree on acceptable limits of precision.
D3182PracticeforRubber—Materials,Equipment,andPro-
NOTE 1—The scope of this test method now includes the evaluation of
cedures for Mixing Standard Compounds and Preparing
the elastomer compatibility of both lubricating fluids and greases.Testing
Standard Vulcanized Sheets
of fluids was not included inTest Method D4289–95 and earlier versions.
D3183Practice for Rubber—Preparation of Pieces for Test
1.2 This test method can also be used as a guide to evaluate
Purposes from Products
the compatibility of greases with rubber products not in
D4175 Terminology Relating to Petroleum, Petroleum
standard sheet form (Practice D3183).
Products, and Lubricants
D4950Classification and Specification for Automotive Ser-
1.3 The values stated in SI units are to be regarded as
vice Greases
standard. No other units of measurement are included in this
2.2 Federal Standards:
standard.
FederalTest Method Standard791C,Method3603.5, Swell-
1.3.1 Exception—When listed, Durometer A units shall be
ing of Synthetic Rubbers
regarded as the standard.
2.3 U.S. Air Force Specifications:
1.4 This standard does not purport to address all of the
USAF-539 Specification Bulletin for Standard Elastomer
safety concerns, if any, associated with its use. It is the
Stocks
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This test method is under the jurisdiction of ASTM Committee D02 on Standards volume information, refer to the standard’s Document Summary page on
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee the ASTM website.
D02.G0.01 on Chemical and General Laboratory Tests. Available from Standardization Documents Order Desk, Bldg. 4, Section D,
Current edition approved May 1, 2008. Published September 2008. Originally 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
approved in 1989. Last previous edition approved in 2003 as D4289–03. DOI: USAF-539isobsolete,butreproductionshavebeenfiledatASTMInternational
10.1520/D4289-03R08. Headquarters and may be obtained by requesting Research Report RR:D02-1165.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4289 − 03 (2008)
2.4 SAE Standards: 3.1.6 thickener, n—in a lubricating grease, a substance
AMS 3217AStandard Elastomer Stocks—Test Slabs composed of finely divided particles dispersed in a liquid
AMS 3217/2BTest Slabs, Acrylonitrile Butadiene (NBR- lubricant to form the product’s structure.
L)—Low Acrylonitrile, 65–75 3.1.6.1 Discussion—The thickener can be fibers (such as
AMS 3217/3ATest Slabs, Chloroprene (CR)—65–75 various metallic soaps) or plates or spheres (such as certain
non-soapthickeners)whichareinsolubleor,atmost,onlyvery
NOTE 2—USAF-539 was specified in Test Method D4289–94 and
slightly soluble in the liquid lubricant. The general require-
earlier versions. This specification is obsolete and has been replaced by
mentsarethatthesolidparticlesbeextremelysmall,uniformly
SAEStandardAMS3217A.USAF-539NBR-LhasbeenreplacedbySAE
AMS 3217/2B (NBR-L), which is virtually identical. USAF-539 CR has
dispersed, and capable of forming a relatively stable, gel-like
been replaced by the similar, but not identical, SAEAMS 3217/3A (CR).
structure with the liquid lubricant. D217
Elastomer sheets prepared to this latter specification are not known or
3.2 Definitions of Terms Specific to This Standard:
expected to provide test results identical with those of the USAF-539
counterpart.
3.2.1 coupon, n—a test piece of specified dimensions cut
NOTE 3—With respect to elastomer AMS 3217/2A, the elastomer
from standard elastomer sheets. D3182
specification has been superseded by AMS 3217/2B. Per SAE, the
3.3 Symbols:
elastomers are identical, however, the synthetic lubricant immersion fluid
used to reference the elastomer has been exchanged from ARM-200 to
3.3.1 Symbols used in the calculation of hardness change
AMS 3021. Reference fluid AMS 3021 better represents current market
(see Eq 1 in 10.1):
aviation fluids.
∆H = hardness change, Durometer A units,
2.5 ASTM Adjuncts:
H = initial hardness, Durometer A units,
i
ADJD6300 D2PP, Version 4.43, Determination of Preci-
H = final hardness, Durometer A units.
f
sion and Bias Data for Use inTest Methods for Petroleum
3.3.2 Symbols used in the calculation of relative density
Products
(see Eq 2 in 10.2) and volume change (see Eq 3 in 10.3):
3. Terminology
RD = relative density,
3.1 Definitions: ∆V = volume change, %,
M1 = initial mass of coupon in air, g,
3.1.1 elastomer, n—a natural or synthetic polymer having
M 2 = initial mass of coupon and hanger wire in water less
therubber-likepropertyofsubstantiallyrecoveringitssizeand
mass of hanger wire partially submerged in water, g,
shape after removal of a deforming force.
M3 = final mass of coupon in air, g,
3.1.2 hardness, n—of an elastomer, the resistance to defor-
M4 = final mass of coupon and hanger wire in water less
mation or indentation.
mass of hanger wire partially submerged in water, g.
3.1.2.1 Discussion—In this test method the hardness of an
4. Summary of Test Method
elastomer is measured with a Shore Durometer A (see Test
Method D2240).
4.1 A prepared elastomer coupon is measured for initial
hardness (DurometerA), density or relative density (to ensure
3.1.3 lubricant, n—any material interposed between two
thatthecouponiswithinspecifiedlimits),andvolumebywater
surfacesthatreducesthefrictionorwearbetweenthem. D4175
displacement. The coupon is immersed in test grease or fluid
3.1.4 lubricating grease, n—a semifluid to solid product of
and aged for 70 h at either 100°C (for chloroprene and similar
a dispersion of a thickener in a liquid lubricant.
flex-resistant elastomers) or 150°C (for nitrile and similar
3.1.4.1 Discussion—Thedispersionofthethickenerformsa
heat-resistant elastomers) or at other conditions as required by
two-phase system and immobilizes the liquid lubricant by
the lubricant specification. The resulting changes in hardness
surface tension and other physical forces. Other ingredients
and volume are determined.
imparting special properties are often included. D217
5. Significance and Use
3.1.5 relative density, n—the ratio of the density of a
5.1 Measurementofthechangesinthevolumeandhardness
materialattemperature, t ,tothedensityofwateratareference
of an elastomer that occur from immersion in a lubricating
temperature, t .
grease or fluid provides a means for evaluating relative
3.1.5.1 Discussion—In this test method relative density is
compatibility. Much of this test method was derived from
determined with the temperature of the elastomer and water
procedures described in Test Method D471 and Federal Test
being equal and within the range from 20 to 25°C, and the
Method791C/3603.5. In contrast to these two test methods,
temperature correction for the density of water is not applied.
which emphasize the evaluation of rubber and rubber-like
The term, relative density, replaces the synonymous, depre-
compounds,Test Method D4289 was developed specifically to
catedterm, specific gravity,usedinsomeearliereditionsofthis
evaluatelubricatinggreasesandfluids,especiallythoseusedin
test method.
automotive applications, although the test method can be
applied to lubricants used in industrial applications as well.
ExceptingtheShoreDurometerA,thistestmethodrequiresno
Available from Society of Automotive Engineers (SAE), 400 Commonwealth
specialized, rubber-testing equipment. Virtually all other
Dr., Warrendale, PA 15096-0001, http://www.sae.org.
equipment and supplies specified in the procedure are stock
Available from ASTM International Headquarters. Order Adjunct No.
ADJD6300. Originally produced in 2006. items in lubricants laboratories.
D4289 − 03 (2008)
5.2 The volume and hardness-change values determined by
this test method do not duplicate similar changes that occur in
elastomeric seals under actual service conditions. However,
theycanbecorrelatedinmanyinstances.Inonesuchinstance,
thevolume-changevaluesdeterminedbytheantecedentofthis
test method correlated (r =0.99) with those that occurred
during a vehicle test. Because of wide variations in service
conditions and differences in grease and elastomer formula-
tions, correlations between the results obtained with this test
methodandparticularapplicationsshouldbedeterminedonan
individual basis.
FIG. 1 Coupon Suspension Wire for Fluid Samples
5.3 WhentheoptionalReferenceElastomersAMS3217/2B
(acrylonitrile-butadiene, NBR-L) and AMS 3217/3A (chloro-
NOTE 5—Experience has shown that storage conditions can affect the
prene,CR)areusedtoevaluatecompatibility,theresultscanbe
shelflifeofthereferenceelastomers.Shelflifecanbeextendedbystoring
used to judge a service characteristic of lubricants. In this
elastomersinthedarkinaninertatmosphere(suchasaglassormetal,but
respect, this test method is useful for lubricant specifications
notplastic,container,forexample,vacuumdesiccator,inwhichtheairhas
been replaced by nonreactive gas (such as argon or nitrogen) at refrigera-
(forexample,SpecificationD4950).Similarly,thistestmethod
tor temperatures. Elastomers should not be stored at temperatures lower
can be used in specifications for lubricating fluids as well.
than5°Cbecauseofcrystallinityandsolubilitychangesthatcanaffecttest
5.4 With specifications requiring elastomers other than Ref- performance. Neither should they be stored at reduced pressures or in
permeable containers or wrappers which could allow them to be affected
erence Elastomers AMS 3217/2B or AMS 3217/3A, coupons
by the normal atmosphere.
cut from standard sheets (Practice D3182) should be used.
When the preparation of such coupons is not feasible, or the
7. Apparatus
lubricant specification requires the use of rubber products that
7.1 Sample Beaker, heat-resistant glass, Griffin low form,
donothaveasuitablesizeorconfigurationforuseinpreparing
approximately 50 mm in diameter by 70 mm deep (100-mL
coupons for testing (Practice D3183), this test method can be
nominal capacity), having volumetric markings.
used as a guide for evaluating compatibility.
7.2 Beaker Cover, disposable, aluminum foil weighing
NOTE4—Inasmuchastheprecisionvaluesapplyonlytotheelastomers
(moisture) dish, with crimped sides and flat, smooth bottom,
specified in Annex A1 of Test Method D4289, when a lubricant specifi-
about 0.1 mm thick, having bottom inside diameter approxi-
cationrequiressomeotherelastomer,theuserandsupplierofthelubricant
should agree to the values of acceptable precision. Such values may or
mately 52 mm and a depth of approximately 14 mm, and a
may not be the same as those of Test Method D4289. It is recommended
capacity of about 50 mL.
that the agreed upon precision values be stated in the user’s lubricant
7.3 Analytical Balance,havingasensitivityofatleast1mg,
specification.
equipped with a suspension hook and a platform to locate a
5.5 Theresultsofthistestmethodaremostapplicabletothe
hydrostatic-weighing beaker above the balance pan.
useoflubricatinggreasesandfluidsincontactwithelastomeric
seals, boots, O-rings, and similar products, where the physical
7.4 Hanger Wire, stainless steel, about 0.5-mm diameter
demands on the elastomer are not extreme. In critical applica-
(No. 25 U.S. Steel Wire Gage or Imperial Wire Gage) of
tions where the lubricant will be in contact with rubber parts
suitable length, having a fish-hook configuration, that is, with
subject to severe flexing, extreme temperatures, or similar
a suitably sized eye at one end and a hook configuration
stresses, other rubber properties, such as tensile strength and (approximately 8-mm gape) at the other.
elongation, should also be evaluated as they may be more
7.5 Coupon Suspension Wire, stainless steel, about 0.71 to
indicative of the true compatibility characteristics.
0.72-mm diameter (No. 22 U.S. Steel Wire Gage or Imperial
Wire Gage), configured as shown in Fig. 1, to suspend the
6. Interferences
coupon below the surface of a fluid sample.
6.1 (Warning—Although greases and elastomers typically
7.6 Laboratory Oven, circulating-air type, capable of main-
have long shelf lives, there is potential for change in time.
taining the test temperature within6 2.5°C and equipped with
Therefore, in order to ensure acceptable precision in this test
one or more grill-type, wire shelves.
method,neithertestgreasesnortestelastomersshouldbemore
7.7 Shore Durometer A, stand-mounted type (see Test
than approximately one year old.)
Method D2240).
6.1.1 Before testing with reference elastomers stored for
extended periods (approaching one year or more) or in an
7.8 Coupon Cutting Die, optional, as shown in Fig. 2
adverse environment (high ambient temperatures, solvent va-
(recommended).
pors, and so forth), the elastomers s
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
Designation:D4289–97 Designation:D4289–03 (Reapproved 2008)
Standard Test Method for
Elastomer Compatibility of Lubricating Greases and Fluids
This standard is issued under the fixed designation D4289; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 Department of Defense.
1. Scope
1.1 This test method evaluates the compatibility of lubricating greases and fluids with coupons cut from standard elastomer
sheets (Practice D3182) or, optionally, from SAE SpecificationAMS 3217/2A3217/2B (NBR-L) andAMS 3217/3A (CR) sheets.
Compatibility is evaluated by determining the changes in volume and DurometerAhardness that occur when elastomer coupons
are totally immersed in a lubricant sample for 70 h at either 100 or 150°C or as required by the lubricant specification.
1.1.1 Some lubricant specifications may require different test conditions, such as longer durations or lower or higher
temperatures. In such instances, the repeatability and reproducibility values stated in Section 12 do not apply, and the user and
supplier should agree on acceptable limits of precision.
NOTE 1—The scope of this test method now includes the evaluation of the elastomer compatibility of both lubricating fluids and greases. Testing of
fluids was not included in Test Method D4289–95 and earlier versions.
1.2 This test method can also be used as a guide to evaluate the compatibility of greases with rubber products not in standard
sheet form (Practice D3183).
1.3The values stated in SI and Durometer A units shall be regarded as the standard.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 Exception—When listed, Durometer A units shall be regarded as the standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.For specific hazardwarning statements, see Note 6, Note 7, and Note 88.4-8.6.
2. Referenced Documents
2.1 ASTM Standards:
D217Test Methods for Cone Penetration of Lubricating Grease
D217 Test Methods for Cone Penetration of Lubricating Grease
D297Test Methods for Rubber Products—Chemical Analysis
D412TestMethodsforVulcanizedRubberandThermoplasticElastomers—Tension TestMethodsforRubberProductsChemi-
cal Analysis
D412 Test Methods for Vulcanized Rubber and Thermoplastic ElastomersTension
D471 Test Method for Rubber Property—Effect of Liquids
D1193 Specification for Reagent Water
D2240 Test Method for Rubber Property—Durometer Hardness
D3182 Practice for Rubber—Materials, Equipment, and Procedures for Mixing Standard Compounds and Preparing Standard
Vulcanized Sheets
D3183 Practice for Rubber—Preparation of Product Pieces for Test Purposes from Products
D4175 Terminology Relating to Petroleum, Petroleum Products, and Lubricants
D4950 Classification of and Specification for Automotive Service Greases
This test method is under the jurisdiction ofASTM Committee D-2 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.G0 on
Lubricating Grease.
Current edition approved June 10, 1997. Published August 1997. Originally published as D4289–89. Last previous edition D4289–95.
This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.G0.01
on Chemical and General Laboratory Tests.
Current edition approved May 1, 2008. Published September 2008. Originally approved in 1989. Last previous edition approved in 2003 as D4289–03.
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
, Vol 05.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4289–03 (2008)
2.2 Federal Standards:
Federal Test Method Standard791C, Method3603.5, Swelling of Synthetic Rubbers
2.3 U.S. Air Force Specifications:
USAF-539 Specification Bulletin for Standard Elastomer Stocks
Annual Book of ASTM Standards, Vol 09.01.
Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Annual Book of ASTM Standards, Vol 11.01.
USAF-539 is obsolete, but reproductions have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1165.
D4289–03 (2008)
2.4 SAE Standards:
AMS 3217A Standard Elastomer Stocks—Test Slabs
AMS 3217/2A3217/2B Test Slabs, Acrylonitrile Butadiene (NBR-L)—Low Acrylonitrile, 65–75
AMS 3217/3A Test Slabs, Chloroprene (CR)—65–75
NOTE2—USAF Specification Bulletin 539 2—USAF-539 was specified in Test Method D4289–94 and earlier versions. This specification is obsolete
and has been replaced by SAE StandardAMS 3217A. USAF-539 NBR-Lhas been replaced by SAEAMS 3217/2A3217/2B (NBR-L), which is virtually
identical.USAF-539CRhasbeenreplacedbythesimilar,butnotidentical,SAEAMS3217/3A(CR).Elastomersheetspreparedtothislatterspecification
are not known or expected to provide test results identical with those of the USAF Specification539 counterpart. (CR). Elastomer sheets prepared to this
latter specification are not known or expected to provide test results identical with those of the USAF-539 counterpart.
NOTE 3—With respect to elastomer AMS 3217/2A, the elastomer specification has been superseded by AMS 3217/2B. Per SAE, the elastomers are
identical, however, the synthetic lubricant immersion fluid used to reference the elastomer has been exchanged fromARM-200 toAMS 3021. Reference
fluid AMS 3021 better represents current market aviation fluids.
2.5 ASTM Adjuncts:
ADJD6300 D2PP, Version 4.43, Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products
3. Terminology
3.1 Definitions:
3.1.1 elastomer, n—anaturalorsyntheticpolymerhavingtherubber-likepropertyofsubstantiallyrecoveringitssizeandshape
after removal of a deforming force.
3.1.2 hardness, n—of an elastomer, the resistance to deformation or indentation.
3.1.2.1 Discussion—In this test method the hardness of an elastomer is measured with a Shore DurometerA(see Test Method
D2240).
3.1.3 lubricant, n—any material interposed between two surfaces that reduces the friction or wear between them. D 4175
3.1.4 lubricating grease, n—a semifluid to solid product of a dispersion of a thickener in a liquid lubricant.
3.1.4.1 Discussion—The dispersion of the thickener forms a two-phase system and immobilizes the liquid lubricant by surface
tension and other physical forces. Other ingredients imparting special properties are often included. D 217
3.1.5 relative density, n—the ratio of the density of a material at temperature, t , to the density of water at a reference
temperature, t .
3.1.5.1 Discussion—In this test method relative density is determined with the temperature of the elastomer and water being
equal and within the range from 20 to 25°C, and the temperature correction for the density of water is not applied. The term,
relative density, replaces the synonymous, deprecated term, specific gravity, used in some earlier editions of this test method.
3.1.6 thickener, n—in a lubricating grease, a substance composed of finely divided particles dispersed in a liquid lubricant to
form the product’s structure.
3.1.6.1 Discussion—The thickener can be fibers (such as various metallic soaps) or plates or spheres (such as certain non-soap
thickeners) which are insoluble or, at most, only very slightly soluble in the liquid lubricant.The general requirements are that the
solidparticlesbeextremelysmall,uniformlydispersed,andcapableofformingarelativelystable,gel-likestructurewiththeliquid
lubricant. D 217
3.2 Definitions of Terms Specific to This Standard:
3.2.1 coupon, n—a test piece of specified dimensions cut from standard elastomer sheets (Practice sheets. D 3182).
3.3 Symbols:
3.3.1 Symbols used in the calculation of hardness change (see Eq 1 in 10.1):
DH = hardness change, Durometer A units,
H = initial hardness, Durometer A units,
i
H = final hardness, Durometer A units.
f
3.3.2 Symbols used in the calculation of relative density (see Eq 2 in 10.2) and volume change (see Eq 3 in 10.3):
RD = relative density,
DV = volume change, %,
M1 = initial mass of coupon in air, g,
M 2 = initial mass of coupon and hanger wire in water less mass of hanger wire partially submerged in water, g,
M3 = final mass of coupon in air, g,
Annual Book of ASTM Standards, Vol 05.02.
Available from Society of Automotive Engineers (SAE), 400 Commonwealth Dr., Warrendale, PA 15096-0001, http://www.sae.org.
Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Available from ASTM International Headquarters. Order Adjunct No. ADJD6300. Originally produced in 2006.
D4289–03 (2008)
M4 = final mass of coupon and hanger wire in water less mass of hanger wire partially submerged in water, g.
4. Summary of Test Method
4.1 Aprepared elastomer coupon is measured for initial hardness (DurometerA), density or relative density (to ensure that the
coupon is within specified limits), and volume by water displacement. The coupon is immersed in test grease or fluid and aged
for 70 h at either 100°C (for chloroprene and similar flex-resistant elastomers) or 150°C (for nitrile and similar heat-resistant
elastomers) or at other conditions as required by the lubricant specification. The resulting changes in hardness and volume are
determined.
5. Significance and Use
5.1 Measurement of the changes in the volume and hardness of an elastomer that occur from immersion in a lubricating grease
or fluid provides a means for evaluating relative compatibility. Much of this test method was derived from procedures described
in Test Method D471 and Federal Test Method791C/3603.5. In contrast to these two test methods, which emphasize the
evaluation of rubber and rubber-like compounds, Test Method D4289 was developed specifically to evaluate lubricating greases
andfluids,especiallythoseusedinautomotiveapplications,althoughthetestmethodcanbeappliedtolubricantsusedinindustrial
applications as well. Excepting the Shore Durometer A, this test method requires no specialized, rubber-testing equipment.
Virtually all other equipment and supplies specified in the procedure are stock items in lubricants laboratories.
5.2 The volume and hardness-change values determined by this test method do not duplicate similar changes that occur in
elastomeric seals under actual service conditions. However, they can be correlated in many instances. In one such instance, the
volume-change values determined by the antecedent of this test method correlated (r =0.99) with those that occurred during a
vehicle test. Because of wide variations in service conditions and differences in grease and elastomer formulations, correlations
between the results obtained with this test method and particular applications should be determined on an individual basis.
5.3 When the optional Reference Elastomers AMS 3217/2A3217/2B (acrylonitrile-butadiene, NBR-L) and AMS 3217/3A
(chloroprene, CR) are used to evaluate compatibility, the results can be used to judge a service characteristic of lubricants. In this
respect, this test method is useful for lubricant specifications (for example, Specification D4950). Similarly, this test method can
be used in specifications for lubricating fluids as well.
5.4 With specifications requiring elastomers other than Reference Elastomers AMS 3217/2A3217/2B or AMS 3217/3A,
coupons cut from standard sheets (Practice D3182) should be used. When the preparation of such coupons is not feasible, or the
lubricant specification requires the use of rubber products that do not have a suitable size or configuration for use in preparing
coupons for testing (Practice D3183), this test method can be used as a guide for evaluating compatibility.
NOTE 34—InasmuchastheprecisionvaluesapplyonlytotheelastomersspecifiedinAnnexA1ofTestMethodD4289,whenalubricantspecification
requires some other elastomer, the user and supplier of the lubricant should agree to the values of acceptable precision. Such values may or may not be
the same as those of Test Method D4289. It is recommended that the agreed upon precision values be stated in the user’s lubricant specification.
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 applications
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 (CautionWarning—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 Rreference E elastomers stored for extended periods (approaching one year or more) or in an adverse
environment (high ambient temperatures, solvent vapors, and so forth), the elastomers should be checked for conformance with
the requirements in Table A1.1.
NOTE 45—Experience has shown that storage conditions can affect the shelf life of the reference elastomers. Shelf life can be extended by storing
elastomers in the dark in an inert atmosphere (such as a glass or metal, but not plastic, container, for example, vacuum desiccator, in which the air has
beenreplacedbynonreactivegas(suchas
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