1、Designation: D 2595 96 (Reapproved 2002)e1An American National StandardStandard Test Method forEvaporation Loss of Lubricating Greases Over Wide-Temperature Range1This standard is issued under the fixed designation D 2595; the number immediately following the designation indicates the year oforigina
2、l adoption or, in the case of 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 Defe
3、nse.e1NOTEWarning notes were placed in the text editorially in May 2002.1. Scope1.1 This test method covers the determination of evapora-tion loss of lubricating greases at temperatures between 93 and316C (200 and 600F). This test method is intended toaugment Test Method D 972, which is limited to 1
4、49C(300F).1.2 The values stated in SI units are to be regarded as thestandard.1.3 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 deter
5、mine the applica-bility of regulatory limitations prior to use. For specific safetyinformation, see 5.2.2. Referenced Documents2.1 ASTM Standards:A 240 Specification for Heat-Resisting Chromium andChromium-Nickel Stainless Steel Plate, Sheet, and Stripfor Pressure Vessels2D 217 Test Methods for Cone
6、 Penetration of LubricatingGrease3D 972 Test Method for Evaporation Loss of LubricatingGreases and Oils3E1 Specification for ASTM Thermometers43. Terminology3.1 Definitions:3.1.1 lubricating grease, na semi-fluid to solid product ofa thickener in a liquid lubricant.3.1.1.1 DiscussionThe dispersion o
7、f the thickener forms atwo-phase system and immobilizes the liquid lubricant bysurface tension and other physical forces. Other ingredients arecommonly included to impart special properties. D 2173.1.2 thickener, na substance composed of finely-dividedparticles dispersed in a liquid to form the prod
8、ucts structure.3.1.2.1 DiscussionThickeners can be fibers (such as vari-ous 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-ments are that the solid particles are extrem
9、ely small, uni-formly dispersed, and capable of forming a relatively stable,gel-like structure with the liquid lubricant. D 2174. Summary of Test Method4.1 A weighed sample of grease in an evaporation cell isplaced in a heating device maintained at the desired testtemperature. Heated air is passed o
10、ver the grease surface for 226 0.1 h. The loss in weight of the sample due to evaporationis determined.5. Significance and Use5.1 The loss of volatile materials from greases and oils canadversely affect the original performance characteristics of alubricant and, therefore, could be a significant fac
11、tor inevaluating a lubricant for a specific use. Such volatiles can alsobe considered contaminants in the environment in which thelubricant is to be used. Correlation between results from thistest method and service performance has not been established.5.2 The test method can be used at any specifie
12、d tempera-ture between 93 and 316C (200 and 600F) that may beagreed upon by the user of the method. (WarningThis testmethod should not be used at temperatures which exceed theflash point of the base oil of the grease.)NOTE 1The specified flow of air, 2.58 6 0.02 g/min, (2 L/min atstandard temperatur
13、e and pressure), assumes dry air. It is not known thatthe original work involved dry air but it has since been shown that this can1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.0G on Lubricatin
14、g Grease.Current edition approved June 10, 1996. Published August 1996. Originallypublished as D 2595 67. Last previous edition D 2595 90.2Annual Book of ASTM Standards, Vol 01.03.3Annual Book of ASTM Standards, Vol 05.01.4Annual Book of ASTM Standards, Vol 14.03.1Copyright ASTM International, 100 B
15、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.be a factor in reproducibility and should be addressed. Air with a dewpoint of less than 10C at standard temperature and pressure will besatisfactory.6. Apparatus56.1 Evaporation Cell Assembly (Fig. 1) consisting of thefo
16、llowing items:6.1.1 Sample Cup, A.6.1.2 Hood, B.6.1.3 Cover and Eduction Tube, CThese items (5.1.1 to5.1.3) shall be constructed from a stainless steel conforming toType 304 of Specification A 240. Design dimensions anddimensional tolerances shall be as shown in Fig. 2 and Fig. 3.6.1.4 GasketShall b
17、e of a heat-resistant (315C (600F)material. A gasket cut from 3.2 mm (18-in.) TFE-fluorocarbonsheet has been found to work successfully.6.1.5 Thermocouple Tube and SupportsThe tube shall beof stainless steel having an outside diameter of 3.186 0.025mm (0.125 6 0.001 in.) and fitted with stainless st
18、eel centeringdevices as shown in Fig. 1.6.2 Air Supply SystemShall consist of a calibrated flow-meter, filtering device, and accessory valves capable of deliv-ering and maintaining a flow of dust-free air at the rate of 2.586 0.02 g/min between 15.6 and 29.4C (60 and 85F) (2 L/minat standard tempera
19、ture and pressure).6.3 Heating Device5An aluminum block heater similar tothat shown in Fig. 4 has been found to be satisfactory. It ismore fully described in the Appendix.6.4 ThermometersASTM thermometers graduated in ei-ther Fahrenheit or Celsius degrees and having a range from 5to 400C (20 to 760F
20、) and conforming to the requirements forThermometers 3C or 3F respectively as described in Specifi-cation E1.7. Sampling7.1 Each test will require approximately 20 g to fill thesample cup for a single run. Therefore, the sample presentedfor analysis should be large enough to make possible theselecti
21、on of a representative portion for testing. Examine thesample for any indication of non-homogeneity such as oilseparation, phase changes, or gross contamination. If anyabnormal conditions are found, obtain a new sample.8. Preparation of Apparatus8.1 Clean thoroughly all parts of the evaporation cell
22、assembly.8.2 With Fig. 1 as reference, connect the cover-eductiontube (C) to the hood (B). Adjust thermocouple tube so that thebottom of the tube is flush with face of hood as shown. Insert5A suitable apparatus is available from Koehler Instrument Co., 1595 SycamoreAve., Bohemia, L.I., NY 11716 and
23、Stanhope Seta, Ltd., Park Close, EnglefieldGreen, Egham, Surrey TW20 OXD, England.FIG. 1 Thermocouple Arrangement SECTION OF GREASE SAMPLE CUPALL DIMENSIONS 6.0156 in. (60.4 mm) UNLESS OTHERWISE SPECI-FIEDFIG. 2 Evaporation Test CellFIG. 3 Assembled Test Cell in Aluminum Block HeaterD 2595 96 (2002)
24、e12thermocouple in tube and adjust so that tip is flush with bottomedge of tube. Fasten the thermocouple securely in this positionby compressing the top edge of the tube. Remove the tube-thermocouple assembly and disconnect the hood from thecover-eduction tube.8.3 Clean thoroughly all parts of the e
25、vaporation cellassembly.8.4 Place the cover-eduction tube (C) thermocouple assem-bly and gasket in the heating device as shown by Fig. 4. Fastenthe cover securely in position.8.5 Adjust the temperature of the heating device to maintainthe test temperature and control within 61.0C (62F). Usethe therm
26、ometer for this observation.8.6 Regulate air flow through the assembly to 2.58 6 0.02g/min (2 litres/min at standard temperature and pressure).8.7 By regulating the air preheater, adjust the exit airtemperature to the specified test temperature within 61.1C(62F). Use the thermocouple plus a temperat
27、ure indicator orrecorder for this measurement.8.8 Maintain the temperatures of the heating device and exitair and the air flow rate for at least 0.5 h prior to test.9. Procedure9.1 Weigh the clean grease sample cup and hood to thenearest 0.01 g. Remove the hood and fill the cup with the testgrease t
28、aking care to avoid occlusion of air. Smooth the surfacelevel with the rim of the cup with a straight edge spatula.Remove with a clean cloth any grease which may remain onthe rim or threads of the cup. Thread the hood tightly onto thecup without disturbing the smoothed grease surface. Weigh theassem
29、bly and record the net mass of the grease sample to thenearest 0.01 g.9.2 Remove the cover, eduction tube, and thermocoupleassembly from the heating device. Thread the weighed andassembled sample cup and hood into the eduction tube. Installthe complete assembly in the heating device. Fasten the cove
30、rsecurely in position. If necessary, readjust the temperature andair flow to the levels required.9.3 Maintain the air flow rate at 2.58 6 0.02 g/min (2L/min) and the exit air temperature at the required testtemperature within 61.1C (62F) for 22 6 0.1 h. The exit airtemperature shall be the specified
31、 test temperature.9.4 At the end of the 22-h period, remove the assembledsample cup and hood from the cell and allow to cool to roomtemperature. Determine the net mass of the sample to thenearest 1 mg.10. Calculation10.1 Calculate the evaporation loss of the sample as fol-lows:Mass % evaporation los
32、s 5 S 2 W!/S 3 100 (1)where:S = initial mass of sample, g, andW = mass of sample after test, g.11. Precision and Bias11.1 The precision of this test method is not known to havebeen obtained in accordance with currently accepted guidelines(see the Committee D02 Research Report RR:D2-1007,“Manual on D
33、etermining Precision Data for ASTM Methodson Petroleum Products and Lubricants”).611.1.1 RepeatabilityThe difference between two test re-sults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialwould, in the long run, in the normal and
34、correct operation ofthe test, exceed the following value only in one case in twenty:10 % of the mean value11.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical materials would, in thelong run, ex
35、ceed the following value only in one case intwenty:15 % of the mean value11.2 BiasBias cannot be determined in this test methodbecause the value of the evaporation loss can be defined onlyin terms of the test method.12. Keywords12.1 evaporation; grease; high temperature; test cell; vola-tiles6Annual
36、 Book of ASTM Standards, Vol 05.03.FIG. 4 Aluminum Block HeaterD 2595 96 (2002)e13APPENDIX(Nonmandatory Information)X1. ALUMINUM BLOCK HEATERX1.1 The aluminum block heater found to be satisfactoryconsists of an aluminum block approximately 254 mm (10 in.)wide, 356 mm (14 in.) long, and 203 mm (8 in.
37、) deep. It iscompletely and adequately insulated on all sides. It is heated bytwo 650-W cartridge-type heaters and a 500-W ring-typeheater under each of the two cells as shown in Fig. 2. Thesewere sufficient for the two-cell block but if additional evapo-ration spaces are included, additional or lar
38、ger heaters will berequired. The heaters should be of sufficient size so that theblock will return to the desired test temperature within 60 minafter insertion of the test samples. It shall be equipped withsufficient heaters and control instruments to maintain thedesired test temperature within 1.1C
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42、Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 2595 96 (2002)e14