1、Designation: D 566 02 (Reapproved 2009)Designation: 132/96British Standard 2877Standard Test Method forDropping Point of Lubricating Grease1This standard is issued under the fixed designation D 566; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se 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 test
3、 method covers the determination of the drop-ping point of lubricating grease.1.2 This test method is not recommended for use at bathtemperatures above 288C. For higher temperatures TestMethod D 2265 should be used.1.3 The values stated in SI units are to be regarded asstandard. No other units of me
4、asurement are included in thisstandard.1.4 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 determine the applica-bility of regulatory l
5、imitations prior to use. For specific hazardstatements, see 6.4 and 8.1.2. Referenced Documents2.1 ASTM Standards:2D 217 Test Methods for Cone Penetration of LubricatingGreaseD 235 Specification for Mineral Spirits (Petroleum Spirits)(Hydrocarbon Dry Cleaning Solvent)D 2265 Test Method for Dropping
6、Point of LubricatingGrease 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 dispersion of the thickner forms atwo-phase sys
7、tem and immobilizes the liquid lubricant bysurface tension and other physical forces. Other ingredients arecommonly included to impart special properties. D 2173.1.2 thickener, nin lubricating grease, a substance com-posed of finely-divided particles dispersed in a liquid to formthe products structu
8、re.3.1.2.1 DiscussionThickeners can be fibers (such as vari-ous metallic soaps) or plates or spheres (such as certainnon-soaps thickeners), which are insoluble or, at most, onlyvery slightly soluble in the liquid lubricant. The generalrequirements are that the solid particles are extremely small,uni
9、formly dispersed and capable of forming a relatively stable,gel-like structure with the liquid lubricant. D 2173.2 Definitions of Terms Specific to This Standard:3.2.1 dropping point, na numerical value assigned to agrease composition representing the temperature at which thefirst drop of material f
10、alls from the test cup; that temperaturebeing the average of the thermometer readings of the sampleand bath.3.2.1.1 DiscussionIn the normal and proper operation ofthis test method the temperature of the interior of the greasetest cup and the temperature of the oil bath are monitoredsimultaneously as
11、 the bath is heated. When the first drop ofmaterial falls from the cup, the temperature of the grease testcup and the bath temperature are averaged and recorded as theresult of the test.4. Summary of Test Method4.1 A sample of lubricating grease contained in a cupsuspended in a test tube is heated i
12、n an oil bath at a prescribedrate. The temperature at which material falls from the hole inthe bottom of the cup is averaged with the temperature of theoil bath and recorded as the dropping point of the grease.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and
13、 Lubricants and is the direct responsibility of SubcommitteeD02.G0.03 on Physical Tests.Current edition approved April 15, 2009. Published July 2009. Originallyapproved in 1940. Last previous edition approved in 2002 as D 56602.In the IP, this test method is under the jurisdiction of the Standardiza
14、tionCommittee. This test method was adopted as a joint ASTM-IP standard in 1964.This test method has been adopted for use by government agencies to replaceMethod 1421 of Federal Test Method Standard No. 791b.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custome
15、r 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, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 In general,
16、 the dropping point is the temperature atwhich the grease passes from a semisolid to a liquid state underthe conditions of test. This change in state is typical of greasescontaining as thickeners soaps of conventional types. Greasescontaining as thickeners materials other than conventionalsoaps can,
17、 without change in state, separate oil. This testmethod is useful to assist in identifying the grease as to typeand for establishing and maintaining bench marks for qualitycontrol. The results are considered to have only limitedsignificance with respect to service performance as droppingpoint is a s
18、tatic test.NOTE 1Cooperative testing indicates that in general, dropping pointsby Test Method D 5663and Test Method D 2265 are in agreement. Incases where results differ, there is no known significance. However,agreement between producer and consumer as to the test method used isadvisable.6. Apparat
19、us6.1 Grease CupA chromium-plated brass cup conformingto the dimensions shown in Fig. 1.6.2 Test TubeA test tube of heat-resistant glass,4with rim,100 to 103 mm in length and 11.1 to 12.7 mm in insidediameter provided with three indentations about 19 mm fromthe bottom, equally spaced on the circumfe
20、rence. The depth ofthese indentations shall be such as to support the grease cup atabout the point shown in Fig. 2.6.3 Thermometers, two, having ranges as shown below andconforming to the requirements prescribed in SpecificationE1:Thermometer NumberTemperature Range ASTM IP5 to + 300C 2C 62C6.4 Acce
21、ssoriesA stirred oil bath consisting of a 400-mLbeaker, a ring stand and ring for support of the oil bath, clampsfor thermometers, two corks as illustrated in Fig. 2, a polishedmetal rod 1.2 to 1.6 mm in diameter and 150 to 152 mm inlength (Fig. 3), a cup plug gage and thermometer depth gage,both sh
22、own in Fig. 1.(WarningThe fluid for the oil bathmust have a flash point in excess of the maximum temperatureat which the bath is to be used5and allowance must be madefor thermal expansion to prevent overflow. Heating is prefer-ably done by an immersed electrical-resistance heater regulatedby voltage
23、 control. An open flame must not be used as theheating source.) (WarningWhen a hot plate is used, caremust be taken to avoid spilling oil on the hot surface.)7. Sampling7.1 When ready to test, examine the sample for any indica-tion of non-homogeneity such as oil separation, phase changes,or gross co
24、ntamination. When any abnormal conditions arenoted, obtain a new sample.8. Preparation of Apparatus8.1 Thoroughly clean the cup and test tube with mineralspirits conforming to Specification D 235. (WarningFlammable. Vapor harmful.)8.2 Use only cups that are clean and free from any residuefrom previo
25、us runs. When the interior plating of the cup showsindications of wear, discard.8.3 When new cups are to be used, check their dimensionsby using the cup plug gage (Fig. 1). To check the bottomopening a 2.72-mm rod should fit easily while a 2.82-mm rodshould not.6If the hole is undersized, ream to co
26、rrect size. Iftoo large, discard.3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D02-1164.4Borosilicate glass has been found satisfactory for this purpose.5Dow Corning 710 Fluid has been found satisfactory when bath temperature
27、s ashigh as 288C are required. Dow Corning is a registered trademark of the DowCorning Corp., Midland, MI 48686.6These are commonly available as a764-in. drill and a No. 34 drill, respectively.NOTE 1Dimensions in millimetres.FIG. 1 Plug Gage, Depth Gage, and Grease CupD 566 02 (2009)28.4 Test tube s
28、hall be clean and free of residues. Inspect thetube for evidence of chipping or cracking, particularly thepoints of indentation. Replace when necessary.8.5 Inspect both cork ring guide and upper cork for charringor distortions in shape. Total clearance between the cork ringguide and the inside wall
29、of the test tube is 1.5 mm. Wheneither cork is abnormal, replace.8.6 Inspect the bulb end of the thermometer to be used in thetest tube. Clean if there is any residue build-up.9. Procedure9.1 Fill a test cup with sample by pressing the largeropening into the grease to be tested until the cup is fill
30、ed.Remove excess grease with a spatula. Gently press the cup,held in a vertical position with the smaller opening at thebottom, down over the metal rod until the latter protrudes about25 mm. Press the rod against the cup in such a manner that therod makes contact at both upper and lower peripheries
31、of thecup. Maintain this contact, rotating the cup on the rod along theindex finger to give a spiral-like motion down the rod toremove a conical section of the grease which adheres along therod.As the cup approaches the end of the rod, carefully slip therod out of the cup so that a smooth film, free
32、 of air bubbles andof reproducible thickness, remains inside the cup. See Fig. 4.9.2 Place the corks on the thermometer to be used in the testtube as shown in Fig. 2. With the thermometer depth gage inposition in the test tube, adjust the position of the upper cork onthe thermometer so that the ther
33、mometer bulb bottoms snuglyin the depth gage. Observe the relative position of the top edgeof the upper cork to the thermometer stem as well as therelative position of the top edge of the test tube to the cork.Care must be taken to be certain that the thermometer isinserted to the same depth when th
34、e apparatus is reassembledwith the grease cup in position.9.3 Replace the depth gage with the grease cup as shown inFig. 2 so that the thermometer is inserted to the previouslygaged depth. When properly inserted, the bulb of the thermom-eter does not touch either the grease sample or the cup.9.4 Sus
35、pend the test tube in the oil bath to a depthcorresponding to the 76 mm immersion mark on the thermom-eter. This should leave the test tube rim at least 6 mm above theoil level.9.5 Suspend the second thermometer in the oil bath so thatits bulb is at approximately the same level as the bulb of thetes
36、t tube thermometer.9.6 Stir the oil bath and heat at a rate of 4 to 7C/min untilthe bath reaches a temperature of approximately 17C belowthe expected dropping point of the grease. At this point reducethe rate of heating so that the temperature difference betweenthe test tube and the oil bath is main
37、tained between 1 and 2C.This condition is established when the oil bath is heated at arate of about 1 to 1.5C/min. As the temperature increases,material will gradually protrude through the orifice of theNOTE 1Dimensions in millimetres.FIG. 2 Assembled ApparatusNOTE 1Dimensions in millimetres.FIG. 3
38、Polished Metal RodD 566 02 (2009)3grease cup. When a drop of material falls, note the tempera-tures on the two thermometers and record their average to thenearest degree as the dropping point of the grease.NOTE 2Certain greases form a drop with a tailing thread uponmelting, which can break off or wh
39、ich can hold until the drop reaches thebottom of the test tube; in any case, the observed dropping point is thetemperature when the drop reaches the bottom of the test tube.NOTE 3The dropping points of some greases, particularly thosecontaining simple aluminum soaps, are known to decrease upon aging
40、, thechange being much greater than the deviation permitted in results obtainedby different laboratories. Therefore, comparative tests between laborato-ries should be made within a period of six days.9.7 Two determinations can be made simultaneously in thesame bath, provided both samples have approx
41、imately thesame dropping points.10. Report10.1 Report the result to the nearest degree as the ASTM-IPdropping point, ASTM D566.11. Precision and Bias711.1 PrecisionThe precision of this test method as deter-mined by statistical examination of interlaboratory results is asfollows:11.1.1 Repeatability
42、The 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 correct operation ofthe test method, exceed the following value only in one case intwenty:Repeatabilit
43、y 5 7C(1)11.1.2 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 value in only one c
44、ase in twenty:Reproducibility 5 13C(2)NOTE 4Although the cooperative data does show that precisionvaried considerably with dropping point range, a statistical analysis of thecomposite of the cooperative data was used to generate the precisionstatement. This test data is given in the article “Report
45、ofASTM TechnicalCommittee G on Dropping Point Methods for Lubricating Grease” by P.R. McCarthy appearing in the NLGI Spokesman, Vol 31, 1967, page 76.11.1.3 BiasThere is no bias in this test method becausethe value of the dropping point can be defined only in terms ofthe test method.12. Keywords12.1
46、 dropping point; grease; lubricating grease7There is no research report on file because this test method was developed priorto the development of Research Report guidelines. The statistical method used todetermine precision is unknown.FIG. 4 Procedure to Fill CupD 566 02 (2009)4ASTM International ta
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