1、Designation: D7603 10D7603 13Standard 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 revis
2、ion, the 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. Scope Scope*1.1 This test method covers the determination of storage stability characteristics and the compati
3、bility of automotive gearlubricants when blended with reference lubricants. The purpose of the test is to determine if performance-enhancing additivesseparate out under defined conditions.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in
4、this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2.
5、Referenced Documents2.1 ASTM Standards:2D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)D1193 Specification for Reagent WaterD4175 Terminology Relating to Petroleum, Petroleum Products, and LubricantsD5760 Specification for Performance of Manual Transmiss
6、ion Gear LubricantsE542 Practice for Calibration of Laboratory Volumetric ApparatusE1272 Specification for Laboratory Glass Graduated Cylinders2.2 SAE Standards:3J2360 Lubricating Oil, Gear Multipurpose (Metric) Military Use2.3 Federal Test Method Standard:4FED-STD-791/3440.1 Storage Solubility Char
7、acteristics of Universal Gear LubricantsFED-STD-791/3440.2 Compatibility Characteristics of Universal Gear Lubricants3. Terminology3.1 Definitions:3.1.1 calibrate, vto determine the indication or output of a measuring device (for example, thermometer, manometer, engine)with respect to that of a stan
8、dard.3.1.2 candidate oil, nan oil that is intended to have the performance characteristics necessary to satisfy a specification andis to be tested against that specification. D41753.1.3 reference oil, nan oil of known performance characteristics, used as a basis for comparison.3.1.3.1 Discussion1 Th
9、is test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.B0.03D02.B0.01 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 of the Tes
10、t 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 mLof the test oil into a clean, dry beaker (400 mL) and heatin an oven controlled at 120 C 6 1 C for 20 min 6 1 min.8.1.3.3 Remove the beaker from the oven and allow to
11、cool to 25 C 6 3 C. Fill each centrifuge tube with test oil to the markat 100 mL. Stopper the tubes.8.1.4 Storing the Test OilStore the centrifuge tubes for 30 days 6 1 day. Place the tubes in an upright position in a darkenedarea (such as a drawer or cupboard) in a room whose temperature is control
12、led 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 separated fromthe oil. Operate the centrifuge for 30 min 6 1 min at a speed to give a rcf of 407 at the tips of the tubes (see 6.2).8.1.6 After centrifuging, remove the tub
13、es from the centrifuge 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 in the centrifuge tubes, stop the storage stability procedure, recordthat the storage stability test resulted in zero residue, an
14、d report as detailed in 9.1.1.8.1.6.2 If solid or liquid material has separated out, record that the storage stability test resulted in residue, and report as detailedin 9.1.2. If it is desired to quantify the amount of residue, proceed as directed in Appendix X1 and Appendix X2.5 ASTM Test Monitori
15、ng Center, 6555 Penn Ave., Pittsburgh, PA 152064489, www.standards.astmtmc.cmu.edu.6 The sole source of supply of the detergent known to the committee at this time is Alconox, 30 Glenn St., White Plains, NY, . Trademark of Alconox,30 Glenn St., White Plains, NY, . If you are aware of alternative sup
16、pliers, please provide this information to ASTM International Headquarters. Yourcomments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.D7603 1348.2 Compatibility TestingIn general, when a mixture of a test oil and reference oil is store
17、d, residue can originate because ofincompatibility between the test oil and reference oil, or from a storage stability problem associated with the test and referenceoils themselves, or both. In the specific case of the reference oils SSCT Fluid (6-pack), the situation is simplified because they dono
18、t normally produce storage stability residues.NOTE 1In principle, therefore, any residue observed in the compatibility test involving these reference oils arises either from incompatibility betweenthe test oil and the reference oil or from storage stability problems from the test oil alone. In pract
19、ice, however, there is a possibility that the referenceoil(s) alone maymight produce residue during storage. For instance, the reference oil(s) maymight have deteriorated during storage, or have becomecontaminated, or the test maymight have been carried out incorrectly. To cover such eventualities,
20、the procedure requires that in the event a residue isobserved in the compatibility test with a test oil, the reference oil(s) involved are subjected to the storage stability test with a view to eliminating themas the source of residue.8.2.1 If desired, the compatibility testing canmay be carried out
21、 in parallel with the storage stability testing described in 8.1.8.2.2 Perform duplicate tests (that is, use two centrifuge tubes).8.2.3 Screen the Test Oil for Storage StabilitySubject the test oil alone (that is, not in combination with the reference oils) tothe storage stability test as described
22、 in 8.1.8.2.4 Preparation of the Centrifuge Tubes, Graduated Cylinders, 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 to sampling.8.2.5.2 For each reference oil, use separate graduated cylin
23、ders (see 6.7.2) to pour 110 mL 6 1 mL each of the reference oiland the test oil into a clean, dry beaker (400 mL). Use the same graduated cylinder each time the test oil is measured, but a clean,dry, graduated cylinder for each of the reference oils. Heat the beakers containing the reference oil/te
24、st oil mixtures in an oven at120 C 6 1 C for 20 min 6 1 min.8.2.5.3 Remove the beakers from the oven and stir the contents while still hot for 5 min, using a mechanical stirrer operatedat approximately 200 r/min.8.2.5.4 Allow to cool to 25 C 6 3 C. Fill each centrifuge tube with reference oil/test o
25、il mixture to the mark at 100 mL.Stopper the tubes.8.2.6 Store and centrifuge the test oil/reference oil mixtures as directed in 8.1.4 and 8.1.5, respectively.8.2.7 After centrifuging, remove the tubes from the centrifuge and check each tube visually to determine if solid or liquidmaterial has separ
26、ated out.8.2.8 No Residue ObservedIf there is no visual evidence of separated material in the centrifuge tubes, stop the compatibilityprocedure, record that the test oil produced zero residue in the compatibility test, and report as detailed in 9.2.1.8.2.9 Residue ObservedIf solid or liquid material
27、 has separated out from one or more of the reference oil/test oil mixtures,proceed as follows:8.2.9.1 Check the Operational Validity of the TestsThis check is to eliminate operational problems as the source of the residue.Items to check include possible contamination of the test equipment, insuffici
28、ent cleaning of equipment, and inadvertent use of awrong oil in place of a reference oil. Rectify any obvious problems.8.2.9.2 Check the Storage Stability of the Reference Oil(s)For each test oil/reference oil mixture giving a residue, subject thereference oil(s) involved alone (that is, not mixed w
29、ith test oil) to the storage stability test as described in 8.1. This is to checkthat the residue does not arise from any storage stability issues with the reference oil(s) themselves (see Note 1). (There is norequirement to check the reference oils for those test oil/reference oil mixtures not givi
30、ng residues.)If there are no obvious operational problems and if any of the reference oils alone produce residue in the storage stability testrequest the Surveillance Panel responsible for this test method to investigate. Proceed to 8.2.9.3 only after it has been confirmedthat none of the reference
31、oils alone is responsible for producing residues in the storage stability test.8.2.9.3 Repeat the compatibility test, as described in 8.2.4 to 8.2.7, for each test oil/reference oil mixture giving residue.8.2.9.4 No Residue ObservedProceed as described in 8.2.8.8.2.9.5 Residue ObservedRecord that th
32、e test oil produced solid or liquid material in the compatibility test, identify thereference oils involved, and report as detailed in 9.2.2. If it is desired to quantify the amount of residue, proceed as directed inAppendix X1 and Appendix X2.NOTE 2Residues produced in the compatibility test maymig
33、ht arise because of incompatibility between the test oil and reference oil, or from a storagestability problem associated with test oil itself, or both (see 8.2). Without further quantitative testing, as described in Appendix X1 and Appendix X2,it is not possible to identify the source of the residu
34、e in the compatibility test.9. Report9.1 Storage Stability:9.1.1 If the storage stability test resulted in no visual liquid or solid residue, report zero separated residues were observed.9.1.2 If the storage stability test resulted in visual liquid or solid residue, report separated residues were ob
35、served.9.2 Compatibility:9.2.1 If none of the test oil/reference oil mixes resulted in visual solid or liquid residues in the compatibility test, report zeroseparated residues were observed.D7603 1359.2.2 If one or more of the test oil/reference oil mixes resulted in visual solid or liquid residues
36、in the compatibility test, reportthat the test oil resulted in separated residues in the compatibility test and identify the reference oil(s) involved.10. Precision and Bias10.1 No information is presented about either the precision or bias of Test Method D7603 for measuring the storage stabilityand
37、 compatibility of gear oils since the test result is nonquantitative.11. Keywords11.1 compatibility; gear oil; storage stabilityAPPENDIXES(Nonmandatory Information)X1. QUANTIFYING THE AMOUNT OF SOLID OR LIQUID RESIDUESX1.1 The procedures described in this appendix allow the determination of the mass
38、 of solid residues or the volume of liquidresidues in the event such residues are observed at the end of the storage stability and compatibility test storage period of 30 days.X1.2 Observe the nature of any separated material found in 8.1.6.2 and 8.2.9.5.X1.2.1 If the separated material observed in
39、X1.2 is not sufficiently compacted by the centrifuging to permit decanting thesupernatant oil, continue the centrifuging for intervals of 15 min. If after centrifuging for 15 min, the separated material is a solid,proceed as directed in X1.2.2. If after centrifuging for 30 min, the separated materia
40、l is a liquid, or if it has not been 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 and record the volume of the separated liquid at the bottom of each tubeas indicated in Table X1.1 and Fig. X1.1.X1.2.1.2 Calculate and record the average v
41、olume of the separated liquid.X1.2.2 If the separated material is solid, remove the stoppers and decant (and discard) the supernatant oil. Drain the centrifugetubes in an inverted position at 25 C 6 3 C for a period of 2 h. Discard the drained fluid. Wash the solid residue with solventthree times to
42、 assure that it is free of oil. Centrifuge the solid residue between washes, as detailed in 8.1.5, in order to compactthe residue before draining the wash solvent from the tube.X1.2.2.1 To evaporate the solvent, place the centrifuge tubes in an oven controlled at 105 C 6 3 C for 120 6 5min.105 C 6 3
43、 C for 120 min 6 5 min.X1.2.2.2 Remove the centrifuge tubes from the oven and place 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 to the nearest 1 mg. Determine and record the mass of the separatedmaterial in each tube by subtracting the mass of t
44、he empty centrifuge tube.X1.2.2.4 Calculate and record, to the nearest 1 mg, the average mass of the separated material.TABLE X1.1 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 136X2. CAL
45、CULATING THE PERCENT OF ADDITIVE MATERIAL THAT SEPARATES OUTX2.1 This appendix allows the mass or volume of separated residue recorded in Appendix X1 to be converted to the percent ofthe additive material originally contained in the test oil.X2.2 Storage StabilityX2.2.1 If the residue is a solid, ca
46、lculate the mass percent additive precipitated in the test oil, using Eq X2.1:FIG. X1.1 Procedure for Reading Volume of Separated Liquid for the Centrifuge TubeD7603 137Mass percent additive precipitated5100 M/0.9 mt! (X2.1)where:M = average mass (in grams) of separated residue from the two centrifu
47、ge tubes (see X1.2.2.4),mt = mass percent additive in the test oil,7 and0.9 = 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 Eq X2.2:Volume percent liquid additive deposited5100 V/vt
48、 (X2.2)where:V = average volume (in millilitres) of separated liquid residue from the two centrifuge tubes (see X1.2.1.2),vt = volume percent additive in the test oil.7NOTE X2.1Obtain this information from the supplier of the gear oil.X2.3 CompatibilityX2.3.1 If the residues from the test oil/refere
49、nce oil mixes and the test oil alone are solids, calculate the mass percentincompatibility residue for each test oil/reference oil combination using Eq X2.3:Mass percent incompatibility residue5100MX 2MR1MT!#0.950 mr150 mt!(X2.3)where:MX = average mass (in grams) of separated material found in the test oil/reference oil compatibility test (see X1.2.2.4),MR = average mass of separated material in the reference oil alone, grams/50 mL of oil,= 0 for the SSCT Fluid (6-pack) reference oils,MT = average mass of separ
