1、Designation: D 4289 03An American National StandardStandard Test Method forElastomer Compatibility of Lubricating Greases and Fluids1This standard is issued under the fixed designation D 4289; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript 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 *1.1 This test me
3、thod evaluates the compatibility of lubricat-ing greases and fluids with coupons cut from standard elas-tomer sheets (Practice D 3182) or, optionally, from SAESpecification AMS 3217/2B (NBR-L) and AMS 3217/3A (CR)sheets. Compatibility is evaluated by determining the changesin volume and Durometer A
4、hardness that occur when elas-tomer coupons are totally immersed in a lubricant sample for70 h at either 100 or 150C or as required by the lubricantspecification.1.1.1 Some lubricant specifications may require differenttest conditions, such as longer durations or lower or highertemperatures. In such
5、 instances, the repeatability and reproduc-ibility values stated in Section 12 do not apply, and the user andsupplier should agree on acceptable limits of precision.NOTE 1The scope of this test method now includes the evaluation ofthe elastomer compatibility of both lubricating fluids and greases. T
6、estingof fluids was not included in Test Method D 428995 and earlier versions.1.2 This test method can also be used as a guide to evaluatethe compatibility of greases with rubber products not instandard sheet form (Practice D 3183).1.3 The values stated in SI and Durometer A units shall beregarded a
7、s the standard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.
8、For specific warningstatements, see 8.4-8.6.2. Referenced Documents2.1 ASTM Standards:D 217 Test Methods for Cone Penetration of LubricatingGrease2D 297 Test Methods for Rubber ProductsChemicalAnalysis3D 412 Test Methods for Vulcanized Rubber and Thermo-plastic ElastomersTension3D 471 Test Method fo
9、r Rubber PropertyEffect of Liq-uids3D 1193 Specification for Reagent Water4D 2240 Test Method for Rubber PropertyDurometerHardness3D 3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulcanized Sheets3D 3183 Practice for RubberPreparati
10、on of Pieces for TestPurposes from Products3D 4175 Terminology Relating to Petroleum, PetroleumProducts, and Lubricants5D 4950 Classification of and Specification for AutomotiveService Greases52.2 Federal Standard:Federal Test Method Standard 791C, Method 3603.5,Swelling of Synthetic Rubbers62.3 U.S
11、. Air Force Specification:539 Specification Bulletin for Standard Elastomer Stocks72.4 SAE Standards:AMS 3217A Standard Elastomer StocksTest Slabs8AMS 3217/2B Test Slabs, Acrylonitrile Butadiene (NBR-L)Low Acrylonitrile, 65758AMS 3217/3A Test Slabs, Chloroprene (CR)65758NOTE 2USAF Specification Bull
12、etin 539 was specified in TestMethod D 4289 94 and earlier versions. This specification is obsoleteand has been replaced by SAE Standard AMS 3217A. USAF-539 NBR-Lhas been replaced by SAE AMS 3217/2B (NBR-L), which is virtuallyidentical. USAF-539 CR has been replaced by the similar, but not1This test
13、 method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.G0 on Lubricating Grease.Current edition approved May 10, 2003. Published June 2003. Originallyapproved in 1989. Last previous edition approved in 1997 as D
14、 428997.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 09.01.4Annual Book of ASTM Standards, Vol 11.01.5Annual Book of ASTM Standards, Vol 05.02.6Available from Standardization Documents Order Desk, Bldg. 4, Section D,700 Robbins Ave., Philadelphia, PA 19111-5094, Attn
15、: NPODS.7USAF Specification Bulletin 539 is obsolete, but reproductions are available byrequesting RR: D02-1165 from ASTM Headquarters.8Available from Society of Automotive Engineers, 400 Commonwealth Drive,Warrendale, PA 15096.1*A Summary of Changes section appears at the end of this standard.Copyr
16、ight ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.identical, SAE AMS 3217/3A (CR). Elastomer sheets prepared to thislatter specification are not known or expected to provide test resultsidentical with those of the USAF Specification 539 coun
17、terpart.NOTE 3With respect to elastomer AMS 3217/2A, the elastomerspecification has been superseded by AMS 3217/2B. Per SAE, theelastomers are identical, however, the synthetic lubricant immersion fluidused to reference the elastomer has been exchanged from ARM-200 toAMS 3021. Reference fluid AMS 30
18、21 better represents current marketaviation fluids.3. Terminology3.1 Definitions:3.1.1 elastomer, na natural or synthetic polymer havingthe rubber-like property of substantially recovering its size andshape after removal of a deforming force.3.1.2 hardness, nof an elastomer, the resistance to defor-
19、mation or indentation.3.1.2.1 DiscussionIn this test method the hardness of anelastomer is measured with a Shore Durometer A (see TestMethod D 2240).3.1.3 lubricant, nany material interposed between twosurfaces that reduces the friction or wear between them.D 41753.1.4 lubricating grease, na semiflu
20、id to solid product ofa dispersion of a thickener in a liquid lubricant.3.1.4.1 DiscussionThe dispersion of the thickener forms atwo-phase system and immobilizes the liquid lubricant bysurface tension and other physical forces. Other ingredientsimparting special properties are often included. D 2173
21、.1.5 relative density, nthe ratio of the density of amaterial at temperature, t1, to the density of water at a referencetemperature, t2.3.1.5.1 DiscussionIn this test method relative density isdetermined with the temperature of the elastomer and waterbeing equal and within the range from 20 to 25C,
22、and thetemperature correction for the density of water is not applied.The term, relative density, replaces the synonymous, depre-cated term, specific gravity, used in some earlier editions of thistest method.3.1.6 thickener, nin a lubricating grease, a substancecomposed of finely divided particles d
23、ispersed in a liquidlubricant to form the products structure.3.1.6.1 DiscussionThe thickener can be fibers (such asvarious metallic soaps) or plates or spheres (such as certainnon-soap thickeners) which are insoluble or, at most, only veryslightly soluble in the liquid lubricant. The general require
24、-ments are that the solid particles be extremely small, uniformlydispersed, and capable of forming a relatively stable, gel-likestructure with the liquid lubricant. D 2173.2 Definitions of Terms Specific to This Standard:3.2.1 coupon, na test piece of specified dimensions cutfrom standard elastomer
25、sheets. D 31823.3 Symbols:3.3.1 Symbols used in the calculation of hardness change(see Eq 1 in 10.1):DH = hardness change, Durometer A units,Hi= initial hardness, Durometer A units,Hf= final hardness, Durometer A units.3.3.2 Symbols used in the calculation of relative density(see Eq 2 in 10.2) and v
26、olume change (see Eq 3 in 10.3):RD = relative density,DV = volume change, %,M1 = initial mass of coupon in air, g,M2 = initial mass of coupon and hanger wire in water lessmass of hanger wire partially submerged in water, g,M3 = final mass of coupon in air, g,M4 = final mass of coupon and hanger wire
27、 in water lessmass of hanger wire partially submerged in water, g.4. Summary of Test Method4.1 A prepared elastomer coupon is measured for initialhardness (Durometer A), density or relative density (to ensurethat the coupon is within specified limits), and volume by waterdisplacement. The coupon is
28、immersed in test grease or fluidand aged for 70 h at either 100C (for chloroprene and similarflex-resistant elastomers) or 150C (for nitrile and similarheat-resistant elastomers) or at other conditions as required bythe lubricant specification. The resulting changes in hardnessand volume are determi
29、ned.5. Significance and Use5.1 Measurement of the changes in the volume and hardnessof an elastomer that occur from immersion in a lubricatinggrease or fluid provides a means for evaluating relativecompatibility. Much of this test method was derived fromprocedures described in Test Method D 471 and
30、Federal TestMethod 791C/3603.5. In contrast to these two test methods,which emphasize the evaluation of rubber and rubber-likecompounds, Test Method D 4289 was developed specifically toevaluate lubricating greases and fluids, especially those used inautomotive applications, although the test method
31、can beapplied to lubricants used in industrial applications as well.Excepting the Shore Durometer A, this test method requires nospecialized, rubber-testing equipment. Virtually all otherequipment and supplies specified in the procedure are stockitems in lubricants laboratories.5.2 The volume and ha
32、rdness-change values determined bythis test method do not duplicate similar changes that occur inelastomeric 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 thistest method correlat
33、ed (r2= 0.99) with those that occurredduring a vehicle test.9Because of wide variations in serviceconditions and differences in grease and elastomer formula-tions, correlations between the results obtained with this testmethod and particular applications should be determined on anindividual basis.5.
34、3 When the optional Reference Elastomers AMS 3217/2B(acrylonitrile-butadiene, NBR-L) and AMS 3217/3A (chloro-prene, CR) are used to evaluate compatibility, the results can beused to judge a service characteristic of lubricants. In thisrespect, this test method is useful for lubricant specifications9
35、Verdura, T. M., “Evaluating Compatibility of Greases with Elastomeric Seals,”NLGI Spokesman, Vol 42, 1978, pp. 2029.D4289032(for example, Specification D 4950). Similarly, this test methodcan be used in specifications for lubricating fluids as well.5.4 With specifications requiring elastomers other
36、than Ref-erence Elastomers AMS 3217/2B or AMS 3217/3A, couponscut from standard sheets (Practice D 3182) should be used.When the preparation of such coupons is not feasible, or thelubricant specification requires the use of rubber products thatdo not have a suitable size or configuration for use in
37、preparingcoupons for testing (Practice D 3183), this test method can beused as a guide for evaluating compatibility.NOTE 4Inasmuch as the precision values apply only to the elastomersspecified in Annex A1 of Test Method D 4289, when a lubricantspecification requires some other elastomer, the user an
38、d supplier of thelubricant should agree to the values of acceptable precision. Such valuesmay or may not be the same as those of Test Method D 4289. It isrecommended that the agreed upon precision values be stated in the userslubricant specification.5.5 The results of this test method are most appli
39、cable to theuse of lubricating greases and fluids in contact with elastomericseals, boots, O-rings, and similar products, where the physicaldemands on the elastomer are not extreme. In critical applica-tions where the lubricant will be in contact with rubber partssubject to severe flexing, extreme t
40、emperatures, or similarstresses, other rubber properties, such as tensile strength andelongation, should also be evaluated as they may be moreindicative of the true compatibility characteristics.6. Interferences6.1 (WarningAlthough greases and elastomers typicallyhave long shelf lives, there is pote
41、ntial for change in time.Therefore, in order to ensure acceptable precision in this testmethod, neither test greases nor test elastomers should be morethan approximately one year old.)6.1.1 Before testing with reference elastomers stored forextended periods (approaching one year or more) or in anadv
42、erse environment (high ambient temperatures, solvent va-pors, and so forth), the elastomers should be checked forconformance with the requirements in Table A1.1.NOTE 5Experience has shown that storage conditions can affect theshelf life of the reference elastomers. Shelf life can be extended by stor
43、ingelastomers in the dark in an inert atmosphere (such as a glass or metal, butnot plastic, container, for example, vacuum desiccator, in which the air hasbeen replaced by nonreactive gas (such as argon or nitrogen) at refrigera-tor temperatures. Elastomers should not be stored at temperatures lower
44、than 5C because of crystallinity and solubility changes that can affect testperformance. Neither should they be stored at reduced pressures or inpermeable containers or wrappers which could allow them to be affectedby the normal atmosphere.7. Apparatus7.1 Sample Beaker, heat-resistant glass, Griffin
45、 low form,approximately 50 mm in diameter by 70 mm deep (100-mLnominal capacity), having volumetric markings.7.2 Beaker Cover, disposable, aluminum foil weighing(moisture) dish, with crimped sides and flat, smooth bottom,about 0.1 mm thick, having bottom inside diameter approxi-mately 52 mm and a de
46、pth of approximately 14 mm, and acapacity of about 50 mL.7.3 Analytical Balance, having a sensitivity of at least 1 mg,equipped with a suspension hook and a platform to locate ahydrostatic-weighing beaker above the balance pan.7.4 Hanger Wire, stainless steel, about 0.5-mm diameter(No. 25 U.S. Steel
47、 Wire Gage or Imperial Wire Gage) ofsuitable length, having a fish-hook configuration, that is, witha suitably sized eye at one end and a hook configuration(approximately 8-mm gape) at the other.7.5 Coupon Suspension Wire, stainless steel, about 0.71 to0.72-mm diameter (No. 22 U.S. Steel Wire Gage o
48、r ImperialWire Gage), configured as shown in Fig. 1, to suspend thecoupon below the surface of a fluid sample.7.6 Laboratory Oven, circulating-air type, capable of main-taining the test temperature within6 2.5C and equipped withone or more grill-type, wire shelves.7.7 Shore Durometer A, stand-mounte
49、d type (see TestMethod D 2240).7.8 Coupon Cutting Die, optional, as shown in Fig. 2(recommended).8. Reagents and Materials8.1 Purity of ReagentsIt is intended that reagent gradechemicals be used in all tests. Unless otherwise indicated, allreagents shall conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Society,FIG. 1 Coupon Suspension Wire for Fluid SamplesFIG. 2 Coupon Cutting Die (Optional)D4289033where such specifications are available.10Other grades may beused, provided it is first ascertained that
