1、Designation: D972 02 (Reapproved 2008)D972 16Standard Test Method forEvaporation Loss of Lubricating Greases and Oils1This standard is issued under the fixed designation D972; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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 U.S. Department of Defense.1. Scope Scope*1.1 This test method cov
3、ers the determination of the loss in mass by evaporation of lubricating greases and oils for applicationswhere evaporation loss is a factor. Evaporation loss data can be obtained at any temperature in the range from 100100 C to 150C(210150 C (210 F to 300F).300 F).1.2 The values stated in SI units a
4、re to be regarded as standard. The values in given in parentheses are for information only.1.2.1 ExceptionThe values given in parentheses are for information only.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
5、 user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2A240/A240M Specification for Chromium and Chromium-Nickel Stainless Steel Plate, Sheet, and Strip for Pressure
6、Vessels andfor General ApplicationsD217 Test Methods for Cone Penetration of Lubricating GreaseD2595 Test Method for Evaporation Loss of Lubricating Greases Over Wide-Temperature RangeE1E2251 Specification for ASTM Liquid-in-Glass ThermometersLiquid-in-Glass ASTM Thermometers with Low-HazardPrecisio
7、n Liquids3. Terminology3.1 Definitions:3.1.1 lubricating grease, na semi-fluid to solid product of a thickener in a liquid lubricant.3.1.1.1 DiscussionThe dispersion of the thickener forms a two-phase system and immobilizes the liquid lubricant by surface tension and otherphysical forces. Other ingr
8、edients are commonly D217 included to impart special properties.3.1.2 thickener, nin lubricating grease, a substance composed of finely divided particles dispersed in a liquid to form theproducts structure.3.1.2.1 DiscussionThickeners can be fibers (such as various metallic soaps) or plates or spher
9、es (such as certain non-soap thickeners), which areinsoluble or, at most, only very slightly soluble in the liquid lubricant. The general requirements are that the solid particles areextremely small, uniformly dispersed, and capable of forming a relatively stable, gel-like structure with the D217 li
10、quid lubricant.1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.G0.03 on Physical Tests.Current edition approved May 1, 2008April 1, 2016. Published July 2008May 2016. O
11、riginally approved in 1948. Last previous edition approved in 20022008 asD972D972 02 (2008).02. DOI: 10.1520/D0972-02R08.10.1520/D0972-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume i
12、nformation, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequatel
13、y depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM Inter
14、national, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Summary of Test Method4.1 The weighed sample of lubricant in an evaporation cell is placed in a bath maintained at the desired test temperature. Heatedair is passed over its surface for 22 h. 22 h. The e
15、vaporation loss is calculated from the loss in mass of the sample.5. Significance and Use5.1 The loss of volatile materials from greases and oils can adversely effect the original performance characteristics of alubricant and therefore could be a significant factor in evaluating a lubricant for a sp
16、ecific use. Such volatiles can also be consideredcontaminants in the environment in which the lubricant is to be used. Correlation between results from this test method and serviceperformance has not been established.5.2 The test can be run at any agreed upon temperature between 100100 C and 150C (2
17、10150 C (210 F to 300F).300 F).NOTE 1The specified flow of air, 2.582.58 g min 6 0.020.02 g g/min,min, (2 L (2 L/min min at standard temperature and pressure), assumes dryair. It is not known that the original work involved dry air but it has since been shown that this can be a factor in reproducibi
18、lity and should be addressed.A dew point of less than 10C10 C at standard temperature and pressure will be satisfactory.NOTE 2To determine evaporation loss at temperatures above 150C (300F),150 C (300 F), see Test Methods D2595.6. Apparatus6.1 Evaporation Cell, (Fig. 1) as described in Annex A1.6.2
19、Air Supply System, capable of supplying to the cell the required flow of air free of entrained particles. A 400-mm(16-in.)400 mm (16 in.) length of 25-mm (1-in.)25 mm (1 in.) diameter pipe packed with glass wool has been found satisfactoryfor filtering the air.6.3 Oil Bath, shown in Fig. 1a and desc
20、ribed in Annex A1.NOTE 3Other constant-temperature baths may be used if they are equivalent in heat capacity and thermal gradient characteristics to the oil bath.6.4 ThermometersFor tests at 100C (210F)100 C (210 F) an ASTM Thermometer having a range from 9595 C to 103C(204103 C (204 F to 218F)218 F
21、) and conforming to the requirements for Thermometer 22C86 (22F86)S22C (S22F) asprescribed in Specification E1E2251 shall be used. For tests at temperatures above 100C (210F)100 C (210 F), an ASTMPrecision Thermometer conforming to the requirements for Thermometer 67C86 (67F86)S67C (S67F) as prescri
22、bed inSpecification E1E2251 is suitable.FIG. 1 Evaporation Test Cell FIG. 1a Assembled ApparatusKey mm in. Key mm in.A 6.4 0.25 D 124/130 5.0 0.125B 1830 72 E 3.2 0.125C 13 0.5 0.1 = 25 F 1.3/1.8 0.051/0.072G 73.1 2.875Tolerances: 0.4 mm (0.0156 in.) unless otherwise notedD972 1626.5 FlowmeterArotam
23、eter calibrated to deliver air at a rate of 2.582.58 gmin 6 0.020.02 g g/min min between 1515 C and30C (60 and 85F) (230 C (60 F and 85 F) (2 L L/min min at standard temperature and pressure). It shall be furnished witha needle valve and mounted as shown in Fig. 1.7. Sampling7.1 Each grease test wil
24、l require approximately 20 g 20 g to fill the sample cup for a single cup for a single run. Therefore, thesample presented for analysis should be large enough to make possible the selection of a representative portion for testing. Examinethe sample for any indication of non-homogenity such as oil se
25、paration, phase changes, or gross contamination. If any abnormalconditions are found, obtain a new sample.7.2 Each oil test will require at least 10 g 10 g of sample for a single run. Therefore, sufficient sample should be available toobserve any gross contamination or phase separation. If any abnor
26、mal conditions are found, obtain a new sample.8. Preparation of Apparatus8.1 Clean and inspect all components and particularly for wear or damage to threads on sample cups and hood assemblies.Repair or replace if mating is impaired.8.2 Verify unrestricted air flow through tubing on test cell and thr
27、ough eduction tube through cover.8.3 Check that the oil bath is filled with a sufficient quantity of fluid to allow submersion of the evaporation cell to the properlevel as required in 9.2.8.4 Check flowmeter before running any test if there is doubt of its accuracy.9. Procedure for Greases9.1 Weigh
28、 the clean grease-sample cup and hood (Fig. 2) to the nearest 1 mg. Remove the hood and fill the cup with sample,taking care to avoid occlusion of air. Smooth the surface level with the rim of the cup with a straight-edged spatula. Remove witha clean cloth any grease which may remain on the rim or t
29、hreads of the cup. Thread the hood tightly onto the cup without disturbingthe smoothed grease surface. Weigh the assembly and record the mass of the sample to the nearest 1 mg. 1 mg.9.2 With the cover in place, but without the hood and sample cup attached, allow the evaporation cell to acquire the t
30、emperatureof the bath (controlled to 60.5C (61F)60.5 C (61 F) at which the test is to be made by immersing the cell in the bath, asshown in Fig. 2. Ensure the cell is immersed to the designated depth using the support rod adjustment. Allow the cell to remainin the bath at least 12 h h before beginni
31、ng the test. During this period, allow clean air to flow through the cell at the prescribedrate, 2.582.58 g 60.02min 60.02 g g/minmin (2 L (2 L/min min at standard temperature and pressure), as indicated by therotameter. Remove the cover, thread the weighed hood and sample cup into place, and replac
32、e the cover. Tighten the threecover-tightening screws securely to prevent air leakage under the cover. Pass clean air through the cell at the prescribed rate for22 h 6 5 min.22 h 6 5 min.9.3 Remove the assembled sample cup and hood from the cell. At the end of the 22-h22 h period allow to cool to ro
33、omtemperature. Determine the mass of the sample to the nearest 1 mg.1 mg.10. Procedure for Oils10.1 Weigh the clean oil-sample cup and hood (Fig. 2a) to the nearest 1 mg. 1 mg. Transfer, by means of a pipet, 10.0010.00 g6 0.05 g of sample to the cup. Assemble the cup and hood, being careful not to s
34、plash oil on the underside of the hood. Weighthe assembly 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 sample as follows:Evaporation loss,mass%5S 2W!/S# 3100 (1)where:S = initial mas
35、s 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 have been obtained in accordance with currently accepted guidelines (inCommittee D02 research report RR:D02-1007, “Manual on Determining Precision Data for ASTM Metho
36、ds on PetroleumProducts and Lubricants”).12.2 The precision of this test method as determined by statistical examination of interlaboratory results is as follows:D972 16312.2.1 RepeatabilityThe difference between two test results, obtained by the same operator with the same apparatus underconstant o
37、perating conditions on identical test material, would in the long run, in the normal and correct operation of the testmethod, exceed the following value only in one case in twenty:0.025M (2)where:M = mean of two values.12.2.2 ReproducibilityThe difference between two single and independent results o
38、btained by different operators working indifferent laboratories on identical test material would, in the long run, in the normal and correct operation of the test method,exceed the following value only in one case in twenty:0.10M (3)where:M = mean of two values.12.3 BiasThe procedure in this test me
39、thod for measuring evaporation loss of lubricating greases and oils has no bias becausethe value of loss in mass is defined only in terms of this test method.13. Keywords13.1 evaporation; grease; oil; oil bath; rotameter; volatilesFIG. 2 Grease Sample Cup FIG. 2a Oil Sample CupKey mm in. Key mm in.H
40、 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 0.16N 40 1.6 U 58.7 2.3Tolerances: 0.4 mm (0.0156 in.) unless otherwise notedD972 164ANNEX(Mandatory Information)A1. APPARATUSA
41、1.1 Evaporation Cell,with attachments conforming with the dimensional tolerances as indicated in Fig. 1 and Fig. 1a and capableof being supported upright in the oil bath. Other structural details are as follows:A1.1.1 The body and cover of the cell shall be constructed of stainless steel and the air
42、-heating coil of tinned copper tubing.A1.1.2 The sample cups (recommended maximum mass 200 g each), hood, eduction tube, and orifice shall be constructed of 18 %chromium, 8 % nickel alloy steel. A suitable material is an alloy steel conforming to Grade S, Type 304, of SpecificationA240/A240M. To fac
43、ilitate removal and separation of the cup and hood for inserting the sample and weighing, the sample cup shallbe threaded to the hood and this in turn to the eduction 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 the
44、evaporation cell to the proper level and capable of being controlledat the desired test temperature within 60.5C (61F),60.5 C (61 F), with a maximum variation throughout the bath of 60.5C(61F).60.5 C (61 F). Circulation of the oil heating medium by a pump or stirrer is recommended. Sufficient heat c
45、apacity shallbe provided to return the bath to the required temperature within 60 min 60 min after immersion of the cell. The bath shall beprovided with a temperature well such that the thermometer used can be inserted to its proper immersion depth. The bath shall bearranged so that there are no wid
46、e fluctuations in temperature around the evaporation cell.SUMMARY OF CHANGESSubcommittee D02.G0 has identified the location of selected changes to this standard since the last issue(D972 02 (2008) that may impact the use of this standard. (Approved April 1, 2016.)(1) Revised Referenced Documents and
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