1、Designation: D7603 10Standard Test Method forDetermination of Storage Stability and Compatibility inAutomotive Gear Oils1This standard is issued under the fixed designation D7603; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of storagestability characteristics and the compatibility of automo
3、tivegear lubricants when blended with reference lubricants. Thepurpose of the test is to determine if performance-enhancingadditives separate out under defined conditions.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 T
4、his 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.2. Referenced Docume
5、nts2.1 ASTM Standards:2D235 Specification for Mineral Spirits (Petroleum Spirits)(Hydrocarbon Dry Cleaning Solvent)D1193 Specification for Reagent WaterD4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD5760 Specification for Performance of Manual Transmis-sion Gear Lubricant
6、sE542 Practice for Calibration of Laboratory VolumetricApparatusE1272 Specification for Laboratory Glass Graduated Cylin-ders2.2 SAE Standards:3J2360 Lubricating Oil, Gear Multipurpose (Metric) MilitaryUse2.3 Federal Test Method Standard:4FED-STD-791/3440.1 Storage Solubility Characteristics ofUnive
7、rsal Gear LubricantsFED-STD-791/3440.2 Compatibility Characteristics ofUniversal Gear Lubricants3. Terminology3.1 Definitions:3.1.1 calibrate, vto determine the indication or output ofa measuring device (for example, thermometer, manometer,engine) with respect to that of a standard.3.1.2 candidate o
8、il, nan oil that is intended to have theperformance characteristics necessary to satisfy a specificationand is to be tested against that specification. D41753.1.3 reference oil, nan oil of known performance char-acteristics, used as a basis for comparison.3.1.3.1 DiscussionReference oils are used to
9、 calibratetesting facilities, to compare the performance of other oils, orto evaluate other materials (such as seals) that interact withoils. D41753.1.4 test oil, nany oil subjected to evaluation in anestablished procedure. D41754. Summary of Test Method4.1 Separation of the performance-enhancing ad
10、ditives in atest oil during storage is determined by heating it to 120 C,storing at room temperature for 30 days, and making aqualitative observation as to whether any material has sepa-rated out.4.1.1 An optional, non-mandatory test method is also de-scribed in Appendix X1 and Appendix X2 for quant
11、ifying thepercent of the additive which separated out during storage ofthe test oil.4.2 The compatibility of a test oil is determined by blendingit with different reference oils, heating to 120 C, storing atroom temperature for 30 days, and making a qualitativeobservation as to whether any material
12、has separated out.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.B0.03 on Automotive Gear Lubricants see 8.1.6.2 and 8.2.9.5).Store the tubes in the desiccator until required.8.1.3 Preparation
13、of the Test Oil:8.1.3.1 Thoroughly shake the test oil prior to sampling.8.1.3.2 Using a clean, dry, graduated cylinder (see 6.7.1),pour 220 mL of the test oil into a clean, dry beaker (400 mL)and heat in an oven controlled at 120 C 6 1 C for 20 min 61 min.8.1.3.3 Remove the beaker from the oven and
14、allow to coolto 25 C 6 3 C. Fill each centrifuge tube with test oil to themark at 100 mL. Stopper the tubes.8.1.4 Storing the Test OilStore the centrifuge tubes for 30days 6 1 day. Place the tubes in an upright position in adarkened area (such as a drawer or cupboard) in a room whosetemperature is c
15、ontrolled at 25 C 6 3 C.8.1.5 CentrifugingTransfer the tubes to the centrifuge,taking care not to disturb any material that may have separatedfrom the oil. Operate the centrifuge for 30 min 6 1 min at aspeed to give a rcf of 407 at the tips of the tubes (see 6.2).8.1.6 After centrifuging, remove the
16、 tubes from the centri-fuge and check each tube visually to determine if solid or liquidmaterial has separated out.8.1.6.1 If there is no visual evidence of separated material inthe centrifuge tubes, stop the storage stability procedure, recordthat the storage stability test resulted in zero residue
17、, and reportas detailed in 9.1.1.8.1.6.2 If solid or liquid material has separated out, recordthat the storage stability test resulted in residue, and report asdetailed in 9.1.2. If it is desired to quantify the amount ofresidue, proceed as directed inAppendix X1 andAppendix X2.8.2 Compatibility Tes
18、tingIn general, when a mixture of atest oil and reference oil is stored, residue can originatebecause of incompatibility between the test oil and referenceoil, or from a storage stability problem associated with the testand reference oils themselves, or both. In the specific case ofthe reference oil
19、s SSCT Fluid (6-pack), the situation is simpli-fied because they do not normally produce storage stabilityresidues.NOTE 1In principle, therefore, any residue observed in the compat-ibility test involving these reference oils arises either from incompatibilitybetween the test oil and the reference oi
20、l or from storage stabilityproblems from the test oil alone. In practice, however, there is a possibilitythat the reference oil(s) alone may produce residue during storage. Forinstance, the reference oil(s) may have deteriorated during storage, or havebecome contaminated, or the test may have been c
21、arried out incorrectly.To cover such eventualities, the procedure requires that in the event aresidue is observed in the compatibility test with a test oil, the referenceoil(s) involved are subjected to the storage stability test with a view toeliminating them as the source of residue.8.2.1 If desir
22、ed, the compatibility testing can be carried outin parallel with the storage stability testing described in 8.1.8.2.2 Perform duplicate tests (that is, use two centrifugetubes).8.2.3 Screen the Test Oil for Storage StabilitySubject thetest oil alone (that is, not in combination with the referenceoil
23、s) to the storage stability test as described in 8.1.8.2.4 Preparation of the Centrifuge Tubes, Graduated Cyl-inders, and BeakersProceed as directed in 8.1.2.8.2.5 Preparation of the Test Oil/Reference Oil Mixtures:8.2.5.1 Thoroughly shake the test and reference oils prior tosampling.8.2.5.2 For eac
24、h reference oil, use separate graduated cyl-inders (see 6.7.2) to pour 110 mL 6 1 mL each of the referenceoil and the test oil into a clean, dry beaker (400 mL). Use thesame graduated cylinder each time the test oil is measured, buta clean, dry, graduated cylinder for each of the reference oils.Heat
25、 the beakers containing the reference oil/test oil mixturesin an oven at 120 C 6 1 C for 20 min 6 1 min.8.2.5.3 Remove the beakers from the oven and stir thecontents while still hot for 5 min, using a mechanical stirreroperated at approximately 200 r/min.8.2.5.4 Allow to cool to 25 C 6 3 C. Fill eac
26、h centrifugetube with reference oil/test oil mixture to the mark at 100 mL.Stopper the tubes.8.2.6 Store and centrifuge the test oil/reference oil mixturesas directed in 8.1.4 and 8.1.5, respectively.8.2.7 After centrifuging, remove the tubes from the centri-fuge and check each tube visually to dete
27、rmine if solid or liquidmaterial has separated out.8.2.8 No Residue ObservedIf there is no visual evidenceof separated material in the centrifuge tubes, stop the compat-ibility procedure, record that the test oil produced zero residuein the compatibility test, and report as detailed in 9.2.1.8.2.9 R
28、esidue ObservedIf solid or liquid material hasseparated out from one or more of the reference oil/test oilmixtures, proceed as follows:8.2.9.1 Check the Operational Validity of the TestsThischeck is to eliminate operational problems as the source of theresidue. Items to check include possible contam
29、ination of the6The sole source of supply of the detergent known to the committee at this timeis Alconox, 30 Glenn St., White Plains, NY, . Trademark ofAlconox, 30 Glenn St., White Plains, NY, . If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarter
30、s. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.D7603 104test equipment, insufficient cleaning of equipment, and inad-vertent use of a wrong oil in place of a reference oil. Rectifyany obvious problems.8.2.9.2 Check the Sto
31、rage Stability of the Reference Oil(s)For each test oil/reference oil mixture giving a residue, subjectthe reference oil(s) involved alone (that is, not mixed with testoil) to the storage stability test as described in 8.1. This is tocheck that the residue does not arise from any storage stabilityis
32、sues with the reference oil(s) themselves (see Note 1). (Thereis no requirement to check the reference oils for those testoil/reference oil mixtures not giving residues.)If there are no obvious operational problems and if any of thereference oils alone produce residue in the storage stability testre
33、quest the Surveillance Panel responsible for this test methodto investigate. Proceed to 8.2.9.3 only after it has beenconfirmed that none of the reference oils alone is responsiblefor producing residues in the storage stability test.8.2.9.3 Repeat the compatibility test, as described in 8.2.4to 8.2.
34、7, for each test oil/reference oil mixture giving residue.8.2.9.4 No Residue ObservedProceed as described in8.2.8.8.2.9.5 Residue ObservedRecord that the test oil pro-duced solid or liquid material in the compatibility test, identifythe reference oils involved, and report as detailed in 9.2.2.Ifitis
35、 desired to quantify the amount of residue, proceed asdirected in Appendix X1 and Appendix X2.NOTE 2Residues produced in the compatibility test may arise becauseof incompatibility between the test oil and reference oil, or from a storagestability problem associated with test oil itself, or both (see
36、 8.2). Withoutfurther quantitative testing, as described in Appendix X1 and AppendixX2, it is not possible to identify the source of the residue in thecompatibility test.9. Report9.1 Storage Stability:9.1.1 If the storage stability test resulted in no visual liquidor solid residue, report zero separ
37、ated residues were observed.9.1.2 If the storage stability test resulted in visual liquid orsolid residue, report separated residues were observed.9.2 Compatibility:9.2.1 If none of the test oil/reference oil mixes resulted invisual solid or liquid residues in the compatibility test, reportzero sepa
38、rated residues were observed.9.2.2 If one or more of the test oil/reference oil mixesresulted in visual solid or liquid residues in the compatibilitytest, report that the test oil resulted in separated residues in thecompatibility test and identify the reference oil(s) involved.10. Precision and Bia
39、s10.1 No information is presented about either the precisionor bias of Test Method D7603 for measuring the storagestability and compatibility of gear oils since the test result isnonquantitative.11. Keywords11.1 compatibility; gear oil; storage stabilityAPPENDIXES(Nonmandatory Information)X1. QUANTI
40、FYING THE AMOUNT OF SOLID OR LIQUID RESIDUESX1.1 The procedures described in this appendix allow thedetermination of the mass of solid residues or the volume ofliquid residues in the event such residues are observed at theend of the storage stability and compatibility test storage periodof 30 days.X
41、1.2 Observe the nature of any separated material found in8.1.6.2 and 8.2.9.5.X1.2.1 If the separated material observed in X1.2 is notsufficiently compacted by the centrifuging to permit decantingthe supernatant oil, continue the centrifuging for intervals of15 min. If after centrifuging for 15 min,
42、the separated materialis a solid, proceed as directed in X1.2.2. If after centrifugingfor 30 min, the separated material is a liquid, or if it has notbeen compacted, proceed as directed in X1.2.1.1 and X1.2.1.2.X1.2.1.1 Remove the tubes from the centrifuge. Read andrecord the volume of the separated
43、 liquid at the bottom of eachtube as indicated in Table X1.1 and Fig. X1.1.X1.2.1.2 Calculate and record the average volume of theseparated liquid.X1.2.2 If the separated material is solid, remove the stop-pers and decant (and discard) the supernatant oil. Drain thecentrifuge tubes in an inverted po
44、sition at 25 C 6 3 C for aperiod of 2 h. Discard the drained fluid. Wash the solid residuewith solvent three times to assure that it is free of oil.Centrifuge the solid residue between washes, as detailed in8.1.5, in order to compact the residue before draining the washsolvent from the tube.X1.2.2.1
45、 To evaporate the solvent, place the centrifugetubes in an oven controlled at 105 C 6 3 C for 120 6 5 min.X1.2.2.2 Remove the centrifuge tubes from the oven andplace them in a desiccator to cool to 25 C 6 3 C.X1.2.2.3 Measure the mass of each tube and its contents tothe nearest 1 mg. Determine and r
46、ecord the mass of theseparated material in each tube by subtracting the mass of theempty centrifuge tube.X1.2.2.4 Calculate and record, to the nearest 1 mg, theaverage mass of the separated material.D7603 105FIG. X1.1 Procedure for Reading Volume of Separated Liquid for the Centrifuge TubeTABLE X1.1
47、 Procedure for Reading Volume for the Cone-ShapedCentrifuge TubeVolume of Separated Liquid, mL Read to Nearest, mL0.0 to 0.2 0.0250.2 to 1.0 0.05 1.0 0.10D7603 106X2. CALCULATING THE PERCENT OF ADDITIVE MATERIAL THAT SEPARATES OUTX2.1 This appendix allows the mass or volume of separatedresidue recor
48、ded inAppendix X1 to be converted to the percentof the additive material originally contained in the test oil.X2.2 Storage StabilityX2.2.1 If the residue is a solid, calculate the mass percentadditive precipitated in the test oil, using Eq X2.1:Mass percent additive precipitated 5 100 M/0.9 mt! (X2.
49、1)where:M = average mass (in grams) of separated residue from thetwo centrifuge tubes (see X1.2.2.4),mt= mass percent additive in the test oil,7and0.9 = assumed specific gravity of the test oil.X2.2.2 If the residue is a liquid (see X1.2.1.1 and X1.2.1.2),calculate the volume percent liquid additive deposited using EqX2.2:Volume percent liquid additive deposited 5 100 V/vt(X2.2)where:V = average volume (in millilitres) of separated liquidresidue from the two centrifuge tubes (see X1.2.1.2),vt= volume percent additive i
