1、Designation: D6184 14Standard Test Method forOil Separation from Lubricating Grease (Conical SieveMethod)1This standard is issued under the fixed designation D6184; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r
2、evision. 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.INTRODUCTIONThe conical sieve method for measuring
3、 leakage from lubricating grease (commonly known as thecone bleed test) uses the same equipment as the now obsolete and withdrawn Federal Test Method(FTM) 791C Method 321.3, Oil Separation from Lubricating Grease (Static Technique). Despite thelack of a precision statement, Method 321.3 had been use
4、d for many years in military and industrialgrease specifications to determine fluid separation tendencies from greases. Test Method D6184overcomes the deficiencies of Method 321.3. It reflects the procedures and precision determinationsused in a cooperative study in Subcommittee D02.G0 of Committee
5、D02 and supersedes the FTMmethod.1. Scope1.1 This test method covers the determination of the ten-dency of lubricating grease to separate oil at an elevatedtemperature. This test method shall be conducted at 100C for30 h unless other conditions are required by the greasespecification.1.2 This test m
6、ethod is suitable for use with most allgreases, but the test precision was established using greaseshaving a worked penetration (Test Methods D217) greater than220 (NLGI No. 3 grade) and less than 340 (NLGI No. 1 grade).1.3 The values stated in SI units are to be regarded asstandard. The term 60 mes
7、h was originally described in thenow withdrawn E437 standard. It is used to describe the wiremesh because there is no exact metric equivalent.1.4 This standard does not purport to address all the safetyconcerns, if any, associated with its use. It is the responsibilityof the user of this standard to
8、 establish appropriate safetypractices and determine the applicability of regulatory limita-tions prior to use.2. Referenced Documents2.1 ASTM Standards:2D217 Test Methods for Cone Penetration of LubricatingGreaseD1742 Test Method for Oil Separation from LubricatingGrease During StorageE437 Specific
9、ation for Industrial Wire Cloth and Screens(Square Opening Series) (Discontinued 2000) Replacedby E 2016 (Withdrawn 2000)32.2 Withdrawn Government Standard:Federal Test Method (FTM) 791C Method 321.3, OilSeparation from Lubricating Greases (Static Method)Withdrawn 200743. Terminology3.1 Definitions:
10、3.1.1 lubricating grease, na semifluid to solid product ofa dispersion of a thickener in a liquid lubricant.3.1.1.1 DiscussionThe dispersion of the thickener forms atwo-phase system and immobilizes the liquid lubricant by1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum P
11、roducts, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.G0.03 on Physical TestsCurrent edition approved Dec. 1, 2014. Published February 2015. Originallyapproved in 1997. Last previous edition approved in 2005 as D6184 98 (2005),which was withdrawn in July 2014 and
12、reinstated in December 2014. DOI:10.1520/D6184-14.2For 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.3The last a
13、pproved version of this historical standard is referenced onwww.astm.org.4Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29
14、59. United States1surface tension and other physical forces. Other ingredientsimparting special properties are often included. D2173.1.2 oil separation, nthe appearance of a liquid fractionfrom an otherwise homogeneous lubricating composition.D17423.1.3 thickener, nin a lubricating grease, a substan
15、cecomposed of finely divided particles dispersed in a liquidlubricant to form the products structure.3.1.3.1 DiscussionThe thickener can be fibers (such asvarious metallic soaps) or plates or spheres (such as certainnon-soap thickeners) which are insoluble or, at most, only veryslightly soluble in t
16、he liquid lubricant. The general require-ments are that the solid particles be extremely small, uniformlydispersed, and capable of forming a relatively stable, gel-likestructure with the liquid lubricant D2174. Summary of Test Method4.1 The weighed sample is placed in a cone-shaped, wire-cloth sieve
17、, suspended in a beaker, then heated under staticconditions for the specified time and temperature. Unlessotherwise required by the grease specification, the sample istested at standard conditions of 100 6 0.5C for 30 6 0.25 h.The separated oil is weighed and reported as a percentage ofthe mass of t
18、he starting test sample.5. Significance and Use5.1 When lubricating grease separates oil, the residualmaterial may change in consistency, which can affect theability of the product to function as designed. Test resultsobtained with this procedure are not intended to predict oilseparation tendencies
19、of grease under dynamic service condi-tions.5.2 This test method is used for specifications and qualitycontrol.NOTE 1No data have been developed to compare results between thistest method and Test Method D1742.6. Apparatus6.1 Test ApparatusThe assembled apparatus consists of acone-shaped sieve const
20、ructed of 60-mesh, corrosion-resistantwire cloth, a 200-mL tall-form beaker without spout, and aclosely fitting cover with a hook in the center. Constructiondetails and dimensions are shown in Fig. 1.6.1.1 The conical sieve shall be fabricated of stainless steel,monel, or nickel wire cloth, of No. 6
21、0 medium-heavy mesh asdefined in Table 2 of Specification E437 and shall be fabricatedto the dimensions and requirements shown in Fig. 1.NOTE 2Sieves of stapled or wire-bound construction, instead ofsilver-soldered construction, have been used in the past. Such sieves donot conform to this test meth
22、od.6.2 Oven, capable of maintaining the specified temperature,100 6 0.5C.6.3 Balance, having a minimum capacity of 250 g and asensitivity of at least 0.01 g.7. Sampling7.1 Examine the sample for any indication of non-homogeneity such as oil separation, phase changes, or grosscontamination. If any ab
23、normal conditions are found, obtain anew sample.7.2 The sample submitted for analysis should be minimallysufficient for duplicate testing.NOTE 1Dimensions are provided in millimetres (with in./lb. units in parentheses) as follows:A 38.1 0.3 (1.50 0.01) radiusB 27.0 0.3 (1.06 0.01) heightC 70 (2.8) a
24、pproximately (to fit beaker)D 9.7 3.3 (0.38 0.13) lengthE 100 (4) approximatelyF 36 (1.4) approximatelyFIG. 1 Cone Fabrication and Test SetupD6184 1427.3 Although the mass of the test grease is determined, thesieve is filled by volume rather than mass. Each test willrequire a quantity sufficient to
25、fill the sieve to approximatelythe same level as indicated in Fig. 1 (about 10 mL). Approxi-mately the same volume shall be used for each test regardlessof the grease density; the mass will range from about 8 to 12 g.8. Preparation of Apparatus8.1 Carefully clean the sieve, beaker, and cover, by wip
26、ingwith a suitable solvent. Allow the sieve to air dry. See Note 3.NOTE 3Use of an ultrasonic solvent bath has been found helpful incleaning the sieve.8.2 Inspect the sieve to make certain that it is clean and freeof deposits that could affect the passage of oil. It shall be freeof any screen irregu
27、larities such as tears, dents, creases, orenlarged or diminished openings.9. Procedure9.1 Preheat the oven to test temperature. Unless otherwisespecified, the test shall be conducted at standard conditions of100 6 0.5C for 30 6 0.25 h.9.2 Weigh the beaker to within 0.01 g, Wi.9.3 Tare the assembled
28、apparatus consisting of the sieve,cover, and beaker as shown in Fig. 1 to the nearest 0.01 g.9.4 With a suitable spatula, fill the cone sieve with sufficientgrease to approximate the level shown in Fig. 1, being carefulto avoid inclusion of air. Exercise care not to force greasethrough the screen. S
29、mooth and shape the top of the grease intoa slightly convex surface to prevent trapping free oil.9.5 Assemble the entire apparatus as shown in Fig. 1, andweigh to the nearest 0.01 g. Calculate the mass of the grease bydifference, G.9.6 Place the assembled apparatus in the oven for thespecified time
30、and temperature.9.7 Remove the apparatus from the oven and cool to roomtemperature. Remove the cone from the beaker, tapping itgently against the inside of the beaker to take off any oiladhering to its tip. Weigh the beaker containing the collectedoil to the nearest 0.01 g, Wf.9.8 Soon after complet
31、ion of the test, clean the apparatus(Section 8) in preparation for subsequent testing.10. Calculation10.1 Calculate the oil separation as the percentage separatedfrom the original sample as follows:oil separation, % 5Wf2 WiG3100 (1)where:Wi= mass of the beaker before heating,Wf= mass of the beaker a
32、fter heating, andG = mass of the grease tested.11. Report11.1 Report the following information:11.1.1 Grease identity,11.1.2 Test date,11.1.3 Test temperature and duration, and11.1.4 Oil separation, nearest 0.1 %.12. Precision and Bias12.1 PrecisionEight cooperators tested eight greases forleakage i
33、n a cooperative program conducted in accordancewith the design-of-experiments described in RR:D02-1007.5All tests were run in duplicate. The total range of results werefrom 0.1 to 23.7 % leakage (see Table 1).12.2 The precision of the percent oil separation as deter-mined by this test method was obt
34、ained in accordance withADJ6300 (D2PP software).612.3 The repeatability and reproducibility of the test methodas determined by statistical examination of the interlaboratoryresults are as follows:12.3.1 RepeatabilityThe difference between two testresults, obtained by the same operator with the same
35、apparatusunder constant specified operating conditions on identical testmaterial would, in the long run, in the normal and correctoperation of the test method, exceed the following values onlyin 1 case in 20:repeatability, % oil separation 5 1.151 3 M!0.5(2)where:M = mean of two determinations.12.3.
36、2 ReproducibilityThe difference between two singleand independent results by two different operators working indifferent laboratories on identical test material would, in thelong run, in the normal and correct operation of the testmethod, exceed the following values only in 1 case in 20:reproducibil
37、ity, % oil separation 5 1.517 3 M!0.5(3)whereM = mean of two determinations.12.4 BiasThe procedure for measuring the oil separationfrom lubricating grease has no bias because the value of the oilloss is defined only in terms of this test method.13. Keywords13.1 cone-bleed test; leakage; lubricating
38、grease; oil bleed;oil separation5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1007.6Available from ASTM International Headquarters. Order Adjunct No.ADJ6300.TABLE 1 Precision Values for Several Oil Separation PercentagesOi
39、l Separation, % Repeatability Reproducibility1 1.15 1.515 2.57 3.3910 3.64 4.7920 5.15 6.78D6184 143ASTM 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 dete
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