ASTM D4289-13(2014)e1
(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
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 Method 791C/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 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.
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 2 = 0.99) with those that occurred during a vehicle test.7 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 3217/2C (acrylonitrile-butadiene, NBR-L) and AMS 3217/3B (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...
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 Specification AMS 3217/2C (NBR-L) and AMS 3217/3B (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 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).
1.3 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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´1
Designation: D4289 − 13 (Reapproved 2014)
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 U.S. Department of Defense.
ε NOTE—AMS 3217/3B references were updated editorially in October 2014.
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 3217/2C (NBR-L) and AMS 3217/3B (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-
D2240Test Method for Rubber Property—Durometer Hard-
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
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of the ASTM website.
Subcommittee D02.G0.01 on Chemical and General Laboratory Tests. Available from Standardization Documents Order Desk, Bldg. 4, Section D,
Current edition approved Oct. 1, 2014. Published November 2014. Originally 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
approved in 1989. Last previous edition approved in 2013 as D4289–13. DOI: USAF-539isobsolete,butreproductionshavebeenfiledatASTMInternational
10.1520/D4289-13R14E01. 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
´1
D4289 − 13 (2014)
2.4 SAE Standards: temperature correction for the density of water is not applied.
AMS 3217AStandard Elastomer Stocks—Test Slabs The term, relative density, replaces the synonymous, depre-
AMS 3217/2CTest Slabs, Acrylonitrile Butadiene (NBR- catedterm, specific gravity,usedinsomeearliereditionsofthis
L)—Low Acrylonitrile, 65–75 test method.
AMS 3217/3BTest Slabs, Chloroprene (CR)—65–75
3.1.6 thickener, n—in a lubricating grease, a substance
composed of finely divided particles dispersed in a liquid
NOTE 2—USAF-539 was specified in Test Method D4289–94 and
earlier versions. This specification is obsolete and has been replaced by lubricant to form the product’s structure.
SAE Standard AMS 3217A. USAF-539 NBR-L was replaced by SAE
3.1.6.1 Discussion—The thickener can be fibers (such as
AMS 3217/2C (NBR-L), which is virtually identical. USAF-539 CR has
various metallic soaps) or plates or spheres (such as certain
been replaced by the similar, but not identical, SAEAMS 3217/3B (CR).
non-soapthickeners)whichareinsolubleor,atmost,onlyvery
Elastomer sheets prepared to this latter specification are not known or
slightly soluble in the liquid lubricant. The general require-
expected to provide test results identical with those of the USAF-539
counterpart.
mentsarethatthesolidparticlesbeextremelysmall,uniformly
NOTE 3—With respect to elastomer AMS 3217/2A, the elastomer
dispersed, and capable of forming a relatively stable, gel-like
specification was superseded byAMS 3217/2B. Per SAE, the elastomers
structure with the liquid lubricant. D217
are identical, however, the synthetic lubricant immersion fluid used to
reference the elastomer has been exchanged from ARM-200 to AMS
3.2 Definitions of Terms Specific to This Standard:
3021.ReferencefluidAMS3021betterrepresentscurrentmarketaviation
3.2.1 coupon, n—a test piece of specified dimensions cut
fluids.
from standard elastomer sheets. D3182
NOTE 4—With respect to elastomerAMS 3217/2B, the elastomer is no
longer being made by the original supplier and has been superseded by
3.3 Symbols:
AMS 3217/2C. This material is made by Rubber-Tech (Mr. Forest Back,
3.3.1 Symbols used in the calculation of hardness change
orLeahLark,LLark@DNACO.net,Rubber-Tech,5208WadsworthRoad,
(see Eq 1 in 10.1):
Dayton,Ohio45414,phone937-274-1114)andhasbeenapprovedforuse
by SAE. Limited testing of the new material compared with AMS
∆H = hardness change, Durometer A units,
3217/2B material appears to show no bias but more in-depth evaluation is
H = initial hardness, Durometer A units,
impossible due to lack of the older material. i
H = final hardness, Durometer A units.
f
2.5 ASTM Adjuncts:
3.3.2 Symbols used in the calculation of relative density
ADJD6300 D2PP, Version 4.43, Determination of Preci-
(see Eq 2 in 10.2) and volume change (see Eq 3 in 10.3):
sion and Bias Data for Use inTest Methods for Petroleum
Products
RD = relative density,
∆V = volume change, %,
3. Terminology
M1 = initial mass of coupon in air, g,
3.1 Definitions:
M 2 = initial 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,
therubber-likepropertyofsubstantiallyrecoveringitssizeand
M3 = final mass of coupon in air, g,
shape after removal of a deforming force.
M4 = final mass of coupon and hanger wire in water less
mass of hanger wire partially submerged in water, g.
3.1.2 hardness, n—of an elastomer, the resistance to defor-
mation or indentation.
4. Summary of Test Method
3.1.2.1 Discussion—In this test method the hardness of an
elastomer is measured with a Shore Durometer A (see Test
4.1 A prepared elastomer coupon is measured for initial
Method D2240).
hardness (DurometerA), density or relative density (to ensure
thatthecouponiswithinspecifiedlimits),andvolumebywater
3.1.3 lubricant, n—any material interposed between two
surfacesthatreducesthefrictionorwearbetweenthem. D4175 displacement. The coupon is immersed in test grease or fluid
and aged for 70 h at either 100°C (for chloroprene and similar
3.1.4 lubricating grease, n—a semifluid to solid product of
flex-resistant elastomers) or 150°C (for nitrile and similar
a dispersion of a thickener in a liquid lubricant.
heat-resistant elastomers) or at other conditions as required by
3.1.4.1 Discussion—Thedispersionofthethickenerformsa
the lubricant specification. The resulting changes in hardness
two-phase system and immobilizes the liquid lubricant by
and volume are determined.
surface tension and other physical forces. Other ingredients
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,
which emphasize the evaluation of rubber and rubber-like
Available from Society of Automotive Engineers (SAE), 400 Commonwealth
compounds,Test Method D4289 was developed specifically to
Dr., Warrendale, PA 15096-0001, http://www.sae.org.
evaluatelubricatinggreasesandfluids,especiallythoseusedin
Available from ASTM International Headquarters. Order Adjunct No.
ADJD6300. Originally produced in 2006. automotive applications, although the test method can be
´1
D4289 − 13 (2014)
applied to lubricants used in industrial applications as well. 6.1.1 Before testing with reference elastomers stored for
ExceptingtheShoreDurometerA,thistestmethodrequiresno extended periods (approaching one year or more) or in an
specialized, rubber-testing equipment. Virtually all other adverse environment (high ambient temperatures, solvent
equipment and supplies specified in the procedure are stock vapors, and so forth), the elastomers should be checked for
items in lubricants laboratories. conformance with the requirements in Table A1.1.
5.2 The volume and hardness-change values determined by
NOTE 6—Experience has shown that storage conditions can affect the
shelflifeofthereferenceelastomers.Shelflifecanbeextendedbystoring
this test method do not duplicate similar changes that occur in
elastomersinthedarkinaninertatmosphere(suchasaglassormetal,but
elastomeric seals under actual service conditions. However,
notplastic,container,forexample,vacuumdesiccator,inwhichtheairhas
they can be correlated in many instances. In one such instance,
been replaced by nonreactive gas (such as argon or nitrogen) at refrigera-
thevolume-changevaluesdeterminedbytheantecedentofthis
tor temperatures. Elastomers should not be stored at temperatures lower
test method correlated (r =0.99) with those that occurred
than5°Cbecauseofcrystallinityandsolubilitychangesthatcanaffecttest
performance. Neither should they be stored at reduced pressures or in
during a vehicle test. Because of wide variations in service
permeable containers or wrappers which could allow them to be affected
conditions and differences in grease and elastomer
by the normal atmosphere.
formulations, correlations between the results obtained with
this test method and particular applications should be deter-
7. Apparatus
mined on an individual basis.
7.1 Sample Beaker, heat-resistant glass, Griffin low form,
5.3 When the optional Reference ElastomersAMS 3217/2C
approximately 50 mm in diameter by 70 mm deep (100-mL
(acrylonitrile-butadiene, NBR-L) and AMS 3217/3B
nominal capacity), having volumetric markings.
(chloroprene, CR) are used to evaluate compatibility, the
7.2 Beaker Cover, disposable, aluminum foil weighing
results can be used to judge a service characteristic of
(moisture) dish, with crimped sides and flat, smooth bottom,
lubricants. In this respect, this test method is useful for
about 0.1 mm thick, having bottom inside diameter approxi-
lubricant specifications (for example, Specification D4950).
mately 52 mm and a depth of approximately 14 mm, and a
Similarly, this test method can be used in specifications for
capacity of about 50 mL.
lubricating fluids as well.
7.3 Analytical Balance,havingasensitivityofatleast1mg,
5.4 With specifications requiring elastomers other than Ref-
equipped with a suspension hook and a platform to locate a
erence Elastomers AMS 3217/2C or AMS 3217/3B, coupons
hydrostatic-weighing beaker above the balance pan.
cut from standard sheets (Practice D3182) should be used.
7.4 Hanger Wire, stainless steel, about 0.5-mm diameter
When the preparation of such coupons is not feasible, or the
(No. 25 U.S. Steel Wire Gage or Imperial Wire Gage) of
lubricant specification requires the use of rubber products that
suitable length, having a fish-hook configuration, that is, with
donothaveasuitablesizeorconfigurationforuseinpreparing
a suitably sized eye at one end and a hook configuration
coupons for testing (Practice D3183), this test method can be
(approximately 8-mm gape) at the other.
used as a guide for evaluating compatibility.
7.5 Coupon Suspension Wire, stainless steel, about 0.71 to
NOTE5—Inasmuchastheprecisionvaluesapplyonlytotheelastomers
0.72-mm diameter (No. 22 U.S. Steel Wire Gage or Imperial
specified in Annex A1 of Test Method D4289, when a lubricant specifi-
cationrequiressomeotherelastomer,theuserandsupplierofthelubricant
Wire Gage), configured as shown in Fig. 1, to suspend the
should agree to the values of acceptable precision. Such values may or
coupon below the surface of a fluid sample.
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 7.6 Laboratory Oven, circulating-air type, capable of main-
specification.
taining the test temperature within6 2.5°C and equipped with
one or more grill-type, wire shelves.
5.5 Theresultsofthistestmethodaremostapplicabletothe
useoflubricatinggreasesandfluidsincontactwithelastomeric
7.7 Shore Durometer A, stand-mounted type (see Test
seals, boots, O-rings, and similar products, where the physical
Method D2240).
demands on the elastomer are not extreme.
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D4289 − 13 D4289 − 13 (Reapproved 2014)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
ε NOTE—AMS 3217/3B references were updated editorially in October 2014.
1. Scope*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 Specification AMS 3217/2C (NBR-L) and AMS 3217/3A3217/3B (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 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).
1.3 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.
2. Referenced Documents
2.1 ASTM Standards:
D217 Test Methods for Cone Penetration of Lubricating Grease
D297 Test Methods for Rubber Products—Chemical Analysis
D412 Test Methods for Vulcanized Rubber and Thermoplastic Elastomers—Tension
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 Pieces for Test Purposes from Products
D4175 Terminology Relating to Petroleum, Petroleum Products, and Lubricants
D4950 Classification and Specification for Automotive Service Greases
2.2 Federal Standards:
Federal Test Method Standard 791C, Method 3603.5, Swelling of Synthetic Rubbers
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.G0.01 on Chemical and General Laboratory Tests.
Current edition approved Dec. 1, 2013Oct. 1, 2014. Published February 2014November 2014. Originally approved in 1989. Last previous edition approved in 20082013
as D4289 – 03 (2008).D4289 – 13. DOI: 10.1520/D4289-13.10.1520/D4289-13R14E01.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from Standardization Documents Order Desk, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D4289 − 13 (2014)
2.3 U.S. Air Force Specifications:
USAF-539 Specification Bulletin for Standard Elastomer Stocks
USAF-539 is obsolete, but reproductions have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1165.
´1
D4289 − 13 (2014)
2.4 SAE Standards:
AMS 3217A Standard Elastomer Stocks—Test Slabs
AMS 3217/2C Test Slabs, Acrylonitrile Butadiene (NBR-L)—Low Acrylonitrile, 65–75
AMS 3217/3A3217/3B Test Slabs, Chloroprene (CR)—65–75
NOTE 2—USAF-539 was specified in Test Method D4289–94 and earlier versions. This specification is obsolete and has been replaced by SAE Standard
AMS 3217A. USAF-539 NBR-L was replaced by SAE AMS 3217/2C (NBR-L), which is virtually identical. USAF-539 CR has been replaced by the
similar, but not identical, SAE AMS 3217/3A3217/3B (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 was 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 from ARM-200 to AMS 3021. Reference fluid AMS
3021 better represents current market aviation fluids.
NOTE 4—With respect to elastomer AMS 3217/2B, the elastomer is no longer being made by the original supplier and has been superseded by AMS
3217/2C. This material is made by Rubber-Tech (Mr. Forest Back, or Leah Lark, LLark@DNACO.net, Rubber-Tech, 5208 Wadsworth Road, Dayton,
Ohio 45414, phone 937-274-1114) and has been approved for use by SAE. Limited testing of the new material compared with AMS 3217/2B material
appears to show no bias but more in-depth evaluation is impossible due to lack of the older material.
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—a natural or synthetic polymer having the rubber-like property of substantially recovering its size and shape
after removal of a deforming force.
3.1.2 hardness, n—of an elastomer, the resistance to deformation or indentation.
Available from Society of Automotive Engineers (SAE), 400 Commonwealth Dr., Warrendale, PA 15096-0001, http://www.sae.org.
Available from ASTM International Headquarters. Order Adjunct No. ADJD6300. Originally produced in 2006.
3.1.2.1 Discussion—
In this test method the hardness of an elastomer is measured with a Shore Durometer A (see Test Method D2240).
3.1.3 lubricant, n—any material interposed between two surfaces that reduces the friction or wear between them. D4175
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. D217
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 solid particles be
extremely small, uniformly dispersed, and capable of forming a relatively stable, gel-like structure with the liquid lubricant. D217
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. D3182
3.3 Symbols:
´1
D4289 − 13 (2014)
3.3.1 Symbols used in the calculation of hardness change (see Eq 1 in 10.1):
ΔH = 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,
ΔV = 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,
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 A prepared elastomer coupon is measured for initial hardness (Durometer A), 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 Method 791C ⁄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 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.
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 3217/2C (acrylonitrile-butadiene, NBR-L) and AMS 3217/3A3217/3B
(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 3217/2C or AMS 3217/3A,3217/3B,
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 5—Inasmuch as the precision values apply only to the elastomers specified in Annex A1 of Test Method D4289, when a lubricant specification
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 (Warning—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.)
Verdura, T. M., “Evaluating Compatibility of Greases with Elastomeric Seals,” NLGI Spokesman, Vol 42, 1978, pp. 20–29.
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D4289 − 13 (2014)
6.1.1 Before testing with reference 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 6—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
been replaced by nonreactive gas (such as argon or nitrogen) at refriger
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