1、Designation: D6184 16Standard 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3、 leakage from lubricating grease (commonly known as thecone bleed test) uses the same equipment as the obsolete, withdrawn Federal Test Method (FTM)791C Method 321.3, Oil Separation from Lubricating Grease (Static Technique). Despite the lack ofa precision statement, Method 321.3 was used for many y
4、ears in specifications to evaluate thetendencies of base fluid separation from military and industrial greases. Test Method D6184supersedes the FTM method by overcoming deficiencies of Method 321.3. It includes the proceduresand precision determinations resultant from a cooperative study conducted b
5、y participating membersof Subcommittee D02.G0 of Committee D02.1. Scope*1.1 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 100 C for30 h unless other conditions are required by the gre
6、ase speci-fication.1.2 This test method 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 re
7、garded asstandard. The term 60 mesh was originally described in thenow withdrawn E437 standard.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 responsibil
8、ityof the user of this standard to 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 Lubricating
9、Grease During StorageE437 Specification for Industrial Wire Cloth and Screens(Square Opening Series) (Discontinued 2000) Replacedby E 2016 (Withdrawn 2000)32.2 Government Standard (Withdrawn):Federal Test Method (FTM) 791C 321.3, Oil Separationfrom Lubricating Greases (Static Technique)WithdrawnNove
10、mber 200743. Terminology3.1 Definitions:3.1.1 lubricating grease, na semifluid to solid product ofa dispersion of a thickener in a liquid lubricant.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
11、Subcommittee D02.G0.03 on Physical TestsCurrent edition approved Sept. 1, 2016. Published September 2016. Originallyapproved in 1997. Last previous edition approved in 2014 as D6184 14. DOI:10.1520/D6184-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer
12、 Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from Standardization Documents Order Desk, Bldg. 4 Section
13、D, 700Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1.1 DiscussionThe dispersion of the thickener forms atwo
14、-phase system and immobilizes the liquid lubricant bysurface 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,
15、nin a lubricating grease, a substancecomposed 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 m
16、ost, only veryslightly soluble in the 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
17、 in a cone-shaped, wire-cloth sieve, 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 C 6 0.5 C for 30 h 60.25 h. The separated oil is weighed and
18、reported as apercentage of the mass of the 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 inten
19、ded to predict oilseparation tendencies of grease under dynamic service condi-tions.5.2 This test method is used for specifications and qualitycontrol.6. Apparatus6.1 Test ApparatusThe assembled apparatus consists of acone-shaped sieve constructed of 60 mesh, corrosion-resistantwire cloth, a 200 mL
20、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. 60 medium-heavy mesh asdefined in Table 2 of Specification E
21、437 and shall be fabricatedto the dimensions and requirements shown in Fig. 1.NOTE 1Sieves of stapled or wire-bound construction, instead ofsilver-soldered construction, have been used in the past. Such sieves donot conform to this test method.6.2 Oven, capable of maintaining the specified temperatu
22、re,100 C 6 0.5 C.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 abnormal conditions are found, obtain anew sample.7.2 The
23、sample submitted for analysis should be minimallysufficient for duplicate testing.7.3 Although the mass of the test grease is determined, thesieve is filled by volume rather than mass. Each test willrequire a quantity sufficient to fill the sieve to approximatelyNOTE 1Dimensions are provided in mill
24、imetres (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) approximately (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 162the same level as indicat
25、ed 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 g to12 g.8. Preparation of Apparatus8.1 Carefully clean the sieve, beaker, and cover, by wipingwith a suitable solvent. Allow the sieve to air dry.
26、 See Note 2.NOTE 2Use 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 irregularities such as tears, dents, creases, orenlarged or d
27、iminished openings.9. Procedure9.1 Preheat the oven to test temperature. Unless otherwisespecified, the test shall be conducted at standard conditions of100 C 6 0.5 C for 30 h 6 0.25 h.9.2 Weigh the beaker to within 0.01 g, Wi.9.3 Tare the assembled apparatus consisting of the sieve,cover, and beake
28、r 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. Smooth and shape the top of the grease intoa slight
29、ly 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 and temperature.9.7 Remove the apparatus from the
30、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 completion of the test, clean the apparatus(Section 8) in
31、 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 after heating, andG = mass of the grease tested.11.
32、 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 in a cooperative program conducted in accordancewit
33、h 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 obtained in accordance withADJ6300 (D2PP software).
34、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 apparatusunder constant specified operating cond
35、itions 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.12.3.2 ReproducibilityThe difference between two sing
36、leand 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:reproducibility, % oil separation 5 1.517 3 M!0.5(3)whereM =
37、 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 grease; oil bleed;oil separation5Supporting data
38、 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 PercentagesOil Separation, % Repeatability Reproducibility1 1
39、.15 1.515 2.57 3.3910 3.64 4.7920 5.15 6.78D6184 163SUMMARY OF CHANGESSubcommittee D02.G0 has identified the location of selected changes to this standard since the last issue(D6184 14) that may impact the use of this standard. (Approved Sept. 1, 2016.)(1) Revised the Introduction.(2) Updated subsec
40、tion 2.2.(3) Deleted former Note 1.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 risk
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