1、Designation: D1404/D1404M 99 (Reapproved 2014)Standard Test Method forEstimation of Deleterious Particles in Lubricating Grease1This standard is issued under the fixed designation D1404/D1404M; the number immediately following the designation indicates theyear of original adoption or, in the case of
2、 revision, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure for the detectionand estimation of deleterious particles in
3、 lubricating grease.1.2 This test method is applicable to all lubricating greases.It can also be used to test other semi-solid or viscous materials.Grease fillers, such as graphite and molybdenum disulfide, canbe tested for abrasive contaminants by first mixing them intopetrolatum or grease known to
4、 be free of deleterious particles.1.3 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems
5、may result in non-conformancewith the standard. Within the text, the SI units are shown inbrackets.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 healt
6、h practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D235 Specification for Mineral Spirits (Petroleum Spirits)(Hydrocarbon Dry Cleaning Solvent)D785 Test Method for Rockwell Hardness of Plastics andElectrical Insulating Mater
7、ialsD4175 Terminology Relating to Petroleum, PetroleumProducts, and Lubricants3. Terminology3.1 DefinitionsSee Terminology D4175.3.2 Definitions:3.2.1 lubricant, nany material interposed between twosurfaces that reduces the friction or wear between them.3.2.2 lubricating grease, na semi-fluid to sol
8、id product ofa dispersion of a thickener in a liquid lubricant.3.2.2.1 DiscussionThe dispersion of the thickener forms atwo-phase system and immobilizes the liquid lubricant bysurface tension and other physical forces. Other ingredients arecommonly included to impart special properties.3.2.3 thicken
9、er, nin lubricating grease, a substance com-posed of finely-divided particles dispersed in a liquid lubricantto form the products structure.3.2.3.1 DiscussionThe solid thickener can be fibers (suchas various metallic soaps) or plates or spheres (such as certainnon-soap thickeners), which are insolub
10、le or, at the most, onlyvery slightly soluble in the liquid lubricant. The generalrequirements are that the solid particles be extremely small,uniformly dispersed, and capable of forming a relatively stable,gel-like structure with the liquid lubricant.3.3 Definitions of Terms Specific to This Standa
11、rd:3.3.1 deleterious particles, nin lubricating grease, minutebits of solid material present as a contaminant and abrasive toacrylic plastic.4. Summary of Test Method4.1 A small portion of the lubricating grease sample isplaced between two clean, highly polished acrylic-plasticplates held rigidly an
12、d parallel in metal holders. A pressure of200 psi 1.38 MPa is applied, and one plate is rotated 30relative to the other. Particles harder than the plastic andexceeding in size the distance between the plates will imbed inthe plates and cause characteristic, arc-shaped scratches in theplates.4.2 The
13、relative number of such solid particles can beestimated by counting the total number of arc-shaped scratcheson the two plates.5. Significance and Use5.1 The significance of the number of scratches as far ascorrelation with field performance is concerned has not beenestablished. A particle which is a
14、brasive to plastic will notnecessarily be abrasive to steel or other bearing materials.Some correlation was obtained in that the contaminant used in1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
15、Subcommittee D02.G0.01 on Chemical and General Laboratory Tests.Current edition approved Oct. 1, 2014. Published November 2014. Originallyapproved in 1956. Last previous edition approved in 2008 as D1404/D1404M 99(2008). DOI: 10.1520/D1404_D1404M-99R14.2For referenced ASTM standards, visit the ASTM
16、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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United S
17、tates1Sample 3 (see 10.1.1) had a greater wear rate in a laboratoryball bearing abrasive wear test than the contaminant in Sample2.NOTE 1The number of scratches obtained cannot be used to draw finedifferences between greases, but rather, to group them into two or threegeneral classes. One such possi
18、ble division could be:1 . . less than 10 scratches2 . . 10 to 40 scratches3 . . more than 40 scratches5.2 An advantage of this test method is that each test takesonly a few minutes to run.5.3 This test method is used for quality control and speci-fication purpose.6. Apparatus6.1 The test apparatus i
19、s shown in Figs. 1 and 2.Asillustrated in Fig. 2, the plastic test plates (commercial acrylic(a) Assembled View(b) Unassembled ViewFIG. 1 Apparatus for Determining Deleterious Particles in Lubricating GreaseD1404/D1404M 99 (2014)2plastic, produced in uniform, highly polished sheets),3,41, arerigidly
20、 held in a parallel position in square recesses in parts 2and 7. The holder, 7, is part of the cap assembly, 7 to 11, whichcan be removed as a unit from the body, 3, by removing fourcap screws. The lower plate holder, 2, can slide along the axisof the main housing, but it is restricted from turning
21、by keysspaced 180 apart. Pressure is applied to the plastic plates, 13,through the holder, 2, by means of the coil spring, 4, springfollower plate, 5, and loading screw, 6. The large loading screwalso serves as a base for the apparatus. The indicator pin, 12,onthe spring follower plate, 5, shows the
22、 linear amount of springcompression, which in turn, is a measure of the pressureapplied to the two plastic plates. The upper holder, 7 , is keptfrom rotating by the threaded pin, 9, which projects through amilled slot in cap, 8, and ends with a locking wing nut, 14.Torotate the upper plate and holde
23、r, the wing nut is loosened, andthe handle, 11, is turned. Aleather washer, 10 , between holder,7, and cap, 8, is used to facilitate turning.NOTE 2Although 6.1 describes an apparatus of specific design, anyother device that provides the essential operating conditions can be used.Such device is permi
24、tted if it can hold the two plastic test plates parallelto each other; apply and measure a minimum pressure of 200 psi 1.38MPa on the plastic plates; and provide for 30 relative rotation of the twoplates.6.2 Plastic Test Plates4,5acrylic plastic test plates (twoper test), 1 6 0.050 in. square by18 6
25、 0.025 in. 25.4 6 1.3mm square by 3.2 6 0.64 mm uniformly thick, having aRockwell M hardness of 94 6 10 (Test Method D785), andhaving highly polished surfaces protected on both sides withprotective paper.NOTE 3Whether dimensioned in inches or millimetres, the plastic testplates should be fabricated
26、to match the square recesses in holders 2 and7.7. Reagents and Materials7.1 Stoddard solvent conforming to Specification D235.(WarningFlammable. Vapor harmful.)NOTE 4Other naphthas or pure paraffinic hydrocarbons, such asn-heptane, can be substituted providing they are suitable volatile and donot so
27、ften or otherwise attack acrylic plastic.8. Procedure8.1 Use a fine, smoothing file to break sharp edges of oneface of each test plate. (A sharp edge could scratch the face ofthe opposite plate.) Remove plastic filings and dust. Do notremove protective paper at this time.8.2 Completely remove the te
28、nsion from the spring anddisassemble the apparatus from the top, Fig. 1b. Snap a testplate into each of the square recesses of holders 2 and 7 (Fig.2); locate the plates such that the surfaces with the filed edgesare opposite each other.NOTE 5The square recesses should be clean, that is, free of sol
29、idmaterial, to preclude uneven loading of the plastic plates.8.3 Remove the protective paper from the test plates. Theexposed polished surfaces must be free of scratches and dust.Remove any incidental dust with a soft brush (beware of staticcharges attracting more dust), damp chamois skin, orcompres
30、sed-gas (ionizing-type recommended) dust remover.8.4 Place a pea-sized (about 0.25 g), representative sampleof the test grease on the face of the lower test plate. Bolt on thecap assembly, making sure the threaded pin, 9, is against onestop. Use the locking wing nut, 14, to retain this position. Tur
31、nthe loading screw to apply a pressure of 200 psi 1.38 MPa asindicated by the pointer and scale and the apparatus makersspring calibration.NOTE 6The scale indicates linear displacement and does not directlyindicate pressure. The apparatus should be supplied with a calibration toconvert the scale rea
32、ding to pressure. (Consult the manufacturer if thiscalibration information is missing.) One equipment maker reported thefollowing calibration:Scale reading of 29 5 200 psi 1.38 mPA#,65%. (1)Equipment made at other times or by other manufacturers can vary andcan have different calibrations.NOTE 7The
33、pressure applied to the plates determines the thickness ofthe grease layer between them. A pressure of 200 psi 1.38 MPa gave athinner layer than 100 psi 0.69 MPa, but increasing the pressure from200 to 500 psi 1.38 to 3.45 MPa caused very little change.8.5 With this pressure applied, loosen the lock
34、ing wing nut,14, on the cap assembly and turn handle, 11, once as far as itwill go (about 30).8.6 Release the spring pressure and disassemble the appa-ratus. Carefully remove the plastic plates from their holders.3The sole source of supply of sized test plates known to the committee at thistime is K
35、oehler Instrument Company, Inc., 1595 Sycamore Ave., Bohemia, NY11716.4If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may at
36、tend.5The apparatus shown in Figs. 1 and 2 is available from Falex Corp., 1020Airpark Dr., Sugar Grove, IL 605549585, and from Koehler Instrument Company,Inc., 1595 Sycamore Ave., Bohemia, New York 11716.1 plastic test plates2 lower plate holder3 body4 spring5 spring follower plate6 loading screw7 u
37、pper plate holder8 cap9 threaded pin10 leather washer11 handle12 indicator pin13 key14 wing nutFIG. 2 Cross-section View of ApparatusD1404/D1404M 99 (2014)38.7 Mark the plates for identification and remove the pro-tective paper from the back faces. Wash the test grease from theplates with filtered S
38、toddard solvent (WarningFlammable.Vapor harmful) and blow dry with filtered air. Handle the testplates very carefully to avoid accidental scratches.8.8 Count and record the total number of arc-shapedscratches on the two plastic test plates. See Fig. 3 for examplesof different degrees of scratching.9
39、. Report9.1 Report the following information:9.1.1 Date,9.1.2 Grease identity,9.1.3 Test pressure to the nearest 10 psi 0.07 MPa, and9.1.4 Total number of scratches on the two test plates.10. Precision and Bias610.1 PrecisionThe precision of this test method was notdetermined with any currently acce
40、ptable guidelines of eitherASTM or Committee D02.10.1.1 Aseries of cooperative tests were run on three greasesamples, two of which were artificially contaminated. Theresults from six different laboratories were:Sample Average No.of ScratchesStandardDeviation14624183 113 2710.2 BiasThe procedure in T
41、est Method D1404/D1404Mhas no bias because the value of the estimation of deleteriousparticles in lubricating grease can be defined only in terms ofa test method.11. Keywords11.1 abrasive particles; cleanliness; contamination; deleteri-ous particles; lubricating grease; particles; scratch testASTM I
42、nternational 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 such rights, are entir
43、ely 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 additional standardsand
44、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 ASTM Committee on
45、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
46、610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ is no research report on file because this test method was developedbefore research report guidelines were instituted and data are no longer available.FIG. 3 Plastic Test Plates Showing Different Degrees of Scratch-ingD1404/D1404M 99 (2014)4
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