1、Designation: D 972 02 (Reapproved 2008)An American National StandardStandard Test Method forEvaporation Loss of Lubricating Greases and Oils1This standard is issued under the fixed designation D 972; the number immediately following the designation indicates the year oforiginal adoption or, in the c
2、ase of revision, 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This tes
3、t method covers the determination of the loss inmass by evaporation of lubricating greases and oils forapplications where evaporation loss is a factor. Evaporationloss data can be obtained at any temperature in the range from100 to 150C (210 to 300F).1.2 The values stated in SI units are to be regar
4、ded asstandard. The values in given in parentheses are for informa-tion only.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 determ
5、ine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2A 240/A 240M Specification for Chromium andChromium-Nickel Stainless Steel Plate, Sheet, and Stripfor Pressure Vessels and for General ApplicationsD 217 Test Methods for Cone Penetration of Lubri
6、catingGreaseD 2595 Test Method for Evaporation Loss of LubricatingGreases Over Wide-Temperature RangeE1 Specification for ASTM Liquid-in-Glass Thermometers3. 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
7、dispersion of the thickener forms atwo-phase system and immobilizes the liquid lubricant bysurface tension and other physical forces. Other ingredients arecommonly D 217 included to impart special properties.3.1.2 thickener, nin lubricating grease, a substance com-posed of finely divided particles d
8、ispersed in a liquid to formthe products 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
9、 that the solid particles are extremely small, uni-formly dispersed, and capable of forming a relatively stable,gel-like structure with the D 217 liquid lubricant.4. Summary of Test Method4.1 The weighed sample of lubricant in an evaporation cellis placed in a bath maintained at the desired test tem
10、perature.Heated air is passed over its surface for 22 h. The evaporationloss is calculated from the loss in mass of the sample.5. Significance and Use5.1 The loss of volatile materials from greases and oils canadversely effect the original performance characteristics of alubricant and therefore coul
11、d be a significant factor in evalu-ating a lubricant for a specific use. Such volatiles can also beconsidered 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 can be run
12、 at any agreed upon temperaturebetween 100 and 150C (210 to 300F).NOTE 1The specified flow of air, 2.58 6 0.02 g/min, (2 L/min atstandard temperature and pressure), assumes dry air. It is not known thatthe original work involved dry air but it has since been shown that this canbe a factor in reprodu
13、cibility and should be addressed. A dew point of lessthan 10C at standard temperature and pressure will be satisfactory.NOTE 2To determine evaporation loss at temperatures above 150C(300F), see Test Methods D 2595.6. Apparatus6.1 Evaporation Cell,(Fig. 1) as described in Annex A1.1This test method i
14、s under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.G0.03 on Physical Tests.Current edition approved May 1, 2008. Published July 2008. Originally approvedin 1948. Last previous edition approved in 2002 as D 97202.2For
15、 referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700
16、, West Conshohocken, PA 19428-2959, United States.6.2 Air Supply System, capable of supplying to the cell therequired flow of air free of entrained particles. A 400-mm(16-in.) length of 25-mm (1-in.) diameter pipe packed withglass wool has been found satisfactory for filtering the air.6.3 Oil Bath,
17、shown in Fig. 1a and described in Annex A1.NOTE 3Other constant-temperature baths may be used if they areequivalent in heat capacity and thermal gradient characteristics to the oilbath.6.4 ThermometersFor tests at 100C (210F) an ASTMThermometer having a range from 95 to 103C (204 to 218F)and conform
18、ing to the requirements for Thermometer 22C86(22F86) as prescribed in Specification E1shall be used. Fortests at temperatures above 100C (210F) an ASTM PrecisionThermometer conforming to the requirements for Thermom-eter 67C86 (67F86) as prescribed in Specification E1 issuitable.6.5 FlowmeterA rotam
19、eter calibrated to deliver air at arate of 2.58 6 0.02 g/min between 15 and 30C (60 and 85F)(2 L/min at standard temperature and pressure). It shall befurnished with a needle valve and mounted as shown in Fig. 1.7. Sampling7.1 Each grease test will require approximately 20 g to fillthe sample cup fo
20、r a single cup for a single run. Therefore, thesample presented for analysis should be large enough to makepossible the selection of a representative portion for testing.Examine the sample for any indication of non-homogenitysuch as oil separation, phase changes, or gross contamination.If any abnorm
21、al conditions are found, obtain a new sample.7.2 Each oil test will require at least 10 g of sample for asingle run. Therefore, sufficient sample should be available toobserve any gross contamination or phase separation. If anyabnormal conditions are found, obtain a new sample.8. Preparation of Appa
22、ratus8.1 Clean and inspect all components and particularly forwear or damage to threads on sample cups and hood assem-blies. Repair or replace if mating is impaired.8.2 Verify unrestricted air flow through tubing on test celland through eduction tube through cover.8.3 Check that the oil bath is fill
23、ed with a sufficient quantityof fluid to allow submersion of the evaporation cell to theproper level as required in 9.2.8.4 Check flowmeter before running any test if there isdoubt of its accuracy.9. Procedure for Greases9.1 Weigh the clean grease-sample cup and hood (Fig. 2)tothe nearest 1 mg. Remo
24、ve the hood and fill the cup withsample, taking care to avoid occlusion of air. Smooth thesurface level with the rim of the cup with a straight-edgedspatula. Remove with a clean cloth any grease which mayremain on the rim or threads of the cup. Thread the hood tightlyonto the cup without disturbing
25、the smoothed grease surface.Weigh the assembly and record the mass of the sample to thenearest 1 mg.9.2 With the cover in place, but without the hood andsample cup attached, allow the evaporation cell to acquire theFIG. 1 Evaporation Test Cell FIG. 1a Assembled ApparatusKey mm in. Key mm in.A 6.4 0.
26、25 D 124/130 5.0 6 0.125B 1830 72 E 3.2 0.125C130.56 0.1 = 25 F 1.3/1.8 0.051/0.072G 73.1 2.875Tolerances: 60.4mm(60.0156 in.) unless otherwise notedD 972 02 (2008)2temperature of the bath (controlled to 60.5C (61F) atwhich the test is to be made by immersing the cell in the bath,as shown in Fig. 2.
27、 Ensure the cell is immersed to thedesignated depth using the support rod adjustment. Allow thecell to remain in the bath at least12 h before beginning the test.During this period, allow clean air to flow through the cell atthe prescribed rate, 2.58 60.02 g/min (2 L/min at standardtemperature and pr
28、essure), as indicated by the rotameter.Remove the cover, thread the weighed hood and sample cupinto place, and replace the cover. Tighten the three cover-tightening screws securely to prevent air leakage under thecover. Pass clean air through the cell at the prescribed rate for22 h 6 5 min.9.3 Remov
29、e the assembled sample cup and hood from thecell. At the end of the 22-h period allow to cool to roomtemperature. Determine the mass of the sample to the nearest 1mg.10. Procedure for Oils10.1 Weigh the clean oil-sample cup and hood (Fig. 2a) tothe nearest 1 mg. Transfer, by means of a pipet, 10.00
30、6 0.05 gof sample to the cup.Assemble the cup and hood, being carefulnot to splash oil on the underside of the hood. Weigh theassembly and record the net sample mass to the nearest 1 mg.10.2 Evaporate the sample as described in 9.2 and 9.3.11. Calculation11.1 Calculate the evaporation loss of the sa
31、mple as follows:Evaporation loss, mass % 5 S 2 W!/S 3 100 (1)where:S = initial mass of sample, g, andW = mass of sample, g, after the test.12. Precision and Bias12.1 The precision of this test method is not known to havebeen obtained in accordance with currently accepted guidelines(in Committee D02
32、research report RR: D02-1007, “Manual onDetermining Precision Data for ASTM Methods on PetroleumProducts and Lubricants”).12.2 The precision of this test method as determined bystatistical examination of interlaboratory results is as follows:12.2.1 RepeatabilityThe difference between two test re-sul
33、ts, obtained by the same operator with the same apparatusFIG. 2 Grease Sample Cup FIG. 2a Oil Sample CupKey mm in. Key mm in.H 66 2.625 O 5.40/5.65 0.213/0.223I 7.62 0.3125 P 1.45/1.70 0.057/0.067J 6.35 0.25 Q 54.64/54.89 2.15/2.16K 1.6 0.0625 R 6.9/7.4 0.27/0.29L 5 0.1875 S 3 0.125M 33 1.3125 T 4 0
34、.16N 40 1.6 U 58.7 2.3Tolerances: 60.4mm(60.0156 in.) unless otherwise notedD 972 02 (2008)3under constant operating conditions on identical test material,would in the long run, in the normal and correct operation ofthe test method, exceed the following value only in one case intwenty:0.025M (2)wher
35、e:M = mean of two values.12.2.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would, inthe long run, in the normal and correct operation of the testmethod, exceed the following val
36、ue only in one case in twenty:0.10M (3)where:M = mean of two values.12.3 BiasThe procedure in this test method for measuringevaporation loss of lubricating greases and oils has no biasbecause the value of loss in mass is defined only in terms ofthis test method.13. Keywords13.1 evaporation; grease;
37、oil; oil bath; rotameter; volatilesANNEX(Mandatory Information)A1. APPARATUSA1.1 Evaporation Cell, with attachments conforming withthe dimensional tolerances as indicated in Fig. 1 and Fig. 1aand capable of being supported upright in the oil bath. Otherstructural details are as follows:A1.1.1 The bo
38、dy and cover of the cell shall be constructedof stainless steel and the air-heating coil of tinned coppertubing.A1.1.2 The sample cups (recommended maximum mass200 g each), hood, eduction tube, and orifice shall be con-structed of 18 % chromium, 8 % nickel alloy steel. A suitablematerial is an alloy
39、 steel conforming to Grade S, Type 304, ofSpecification A 240/A 240M. To facilitate removal and sepa-ration of the cup and hood for inserting the sample andweighing, the sample cup shall be threaded to the hood and thisin turn to the eduction tube of the cover.A1.1.3 The cover of the cell shall be m
40、ade airtight.A1.2 Oil Bath, of sufficient depth to allow submersion of theevaporation cell to the proper level and capable of beingcontrolled at the desired test temperature within 60.5C(61F), with a maximum variation throughout the bath of60.5C (61F). Circulation of the oil heating medium by apump
41、or stirrer is recommended. Sufficient heat capacity shallbe provided to return the bath to the required temperaturewithin 60 min after immersion of the cell. The bath shall beprovided with a temperature well such that the thermometerused can be inserted to its proper immersion depth. The bathshall b
42、e arranged so that there are no wide fluctuations intemperature around the evaporation cell.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determinatio
43、n of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdra
44、wn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your c
45、omments have not received a fair hearing you shouldmake your views known to the ASTM 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 972 02 (2008)4
