1、Designation: D 972 02An 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 case of revision, t
2、he 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. Scope1.1 This test method covers t
3、he 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 either SI units or inch-pound unitsshall
4、be regarded separately as standard. The values stated ineach system may not be exact equivalents of the other;therefore each system must be used independently of the other,without combining values in any way.1.3 This standard does not purport to address all of thesafety concerns, if any, associated
5、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 Documents2.1 ASTM Standards:A 240/A240M Specification for Chromium and Chromium-Nickel Stainl
6、ess Steel Plate, Sheet, and Strip for PressureVessels and for General Applications2D 217 Test Methods for Cone Penetration of LubricatingGrease3D 2595 Test Methods for Evaporation Loss of LubricatingGreases Over Wide Temperature Range3E1 Specification for ASTM Thermometers33. Terminology3.1 Definiti
7、ons:3.1.1 lubricating grease, na semi-fluid to solid product ofa thickener in a liquid lubricant.3.1.1.1 DiscussionThe dispersion of the thickner forms atwo-phase system and immobilizes the liquid lubricant bysurface tension and other physical forces. Other ingredients arecommonly D 217 included to
8、impart special properties.3.1.2 thickener, nin lubricating grease, a substance com-posed of finely - divided particles dispersed 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 thicke
9、ners), which are insoluble or, at most, only veryslightly soluble in the liquid lubricant. The general require-ments are 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 Tes
10、t Method4.1 The weighed sample of lubricant in an evaporation cellis placed in a bath maintained at the desired test temperature.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 mater
11、ials from greases and oils canadversely effect the original performance characteristics of alubricant and therefore could 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. C
12、orrelation between results from thistest method and service performance has not been established.5.2 The test can be run at any agreed upon temperaturebetween 100 and 150C (210 to 300F).NOTE 1The specified flow of air, 2.58 60.02 g/min, (2L/min atstandard temperature and pressure), assumes dry air.
13、It is not known thatthe original work involved dry air but it has since been shown that this canbe a factor in reproducibility 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
14、(300F), see Test Methods D 2595.6. Apparatus6.1 Evaporation Cell,(Fig. 1) as described in Annex A1.6.2 Air Supply System, capable of supplying to the cell therequired flow of air free of entrained particles. A400 mm(16-in.) length of 25-mm (1-in.) diameter pipe packed withglass wool has been found s
15、atisfactory for filtering the air.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.G on Lubricating Grease.Current edition approved April 10, 2002. Published May 2002. Originallypublished as D 97
16、2 48 T. Last previous edition D 972 97.2Annual Book of ASTM Standards, Vol 01.03.3Annual Book of ASTM Standards, Vol 14.03.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3 Oil Bath, shown in Fig. 1a and described in Annex A1.NOTE
17、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 conforming to the requirements for Thermometer 22C86(22
18、F86) 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 rotameter calibrated to deliver air at arate of 2.58
19、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 for a single cup for a single run. Therefore, thes
20、ample 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 abnormal conditions are found, obtain a new sample.7.2
21、 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 Apparatus8.1 Clean and inspect all components and pa
22、rticularly 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 filled with a sufficient quantityof fluid to allow s
23、ubmersion 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. Remove the hood and fill the cup withsample, taking
24、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 the smoothed grease surface.Weigh the assembly a
25、nd 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 thetemperature of the bath (controlled to 60.5C (61F) atFIG. 1 Evaporation Test Cell FIG. 1a Assembled ApparatusKey mm in. Key mm in.A 6
26、.4 0.25 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:6 0.4mm (60.0156 in.) unless otherwise notedD972022which the test is to be made by immersing the cell in the bath,as shown in Fig. 2. Ensure the cell is immersed to thedesignated depth usin
27、g 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 pressure), as indicated by the rotameter.Remove the cover,
28、 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 Remove the assembled sample cup and hood from thecell. At the
29、 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, 10.006 0.05g of sample to the cup. Assemble the cup and hood,
30、beingcareful not to splash oil on the underside of the hood. Weighthe assembly and record the net sample mass to the nearest 1mg.10.2 Evaporate the sample as described in 9.2 and 9.3.11. Calculation11.1 Calculate the evaporation loss of the sample as follows:Evaporation loss, mass % 5 S 2 W!/S 3 100
31、 (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 research report RR: D02-1007, “Manual onDetermining Preci
32、sion 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:FIG. 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
33、 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 0.16N 40 1.6 U 58.7 2.3Tolerances:6 0.4mm (60.0156 in.) unless otherwise notedD97202312.2.1 RepeatabilityThe difference between two test re-sults, obtained by the same opera
34、tor with the same apparatusunder 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)where:M = mean of two values12.2.2 ReproducibilityThe difference betw
35、een 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 value only in one case in twenty:0.10M (3)where:M = mean of two value
36、s12.3 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; oil; oil bath; rotameter; volatilesANNEX(Mandatory Information)A1.
37、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 body and cover of the cell shall be constructedof stainless steel and
38、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 steel conforming to Grade S, Type 304, ofSpecificationA 240. To fac
39、ilitate removal and separation of thecup and hood for inserting the sample and weighing, thesample cup shall be threaded to the hood and this in turn to theeduction tube of the cover.A1.1.3 The cover of the cell shall be made airtight.A1.2 Oil Bath of sufficient depth to allow submersion of theevapo
40、ration 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 or stirrer is recommended. Sufficient heat capacity shallbe provided to return
41、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 be arranged so that there are no wide fluctuations intemperature around the evap
42、oration 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 determination of the validity of any such patent rights, and the riskof infringement of suc
43、h 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 withdrawn. Your comments are invited either for revision of this standard or for addit
44、ional 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 comments have not received a fair hearing you shouldmake your views known to the
45、 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).D972024
