1、Designation: D 1404/D 1404M 99 (Reapproved 2003)An American National StandardStandard Test Method forEstimation of Deleterious Particles in Lubricating Grease1This standard is issued under the fixed designation D 1404/D 1404M; the number immediately following the designation indicates theyear of ori
2、ginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure for the detectionand esti
3、mation of deleterious particles in 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
4、 intopetrolatum or grease known to be free of deleterious particles.1.3 The values stated in either inch-pound units or SI unitsare to be regarded separately as standard. Within the text, theSI units are shown in brackets. The values stated in eachsystem shall be used independently of the other. Com
5、biningvalues from the two systems could result in nonconformancewith the standard.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 d
6、etermine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 235 Specification for Mineral Spirits (Petroleum Spirits)(Hydrocarbon Dry Cleaning Solvent)D 785 Test Method for Rockwell Hardness of Plastics andElectrical Insulating MaterialsD 4175 Term
7、inology Relating to Petroleum, PetroleumProducts, and Lubricants3. Terminology3.1 DefinitionsSee Terminology D 4175.3.1.1 lubricant, nany material interposed between twosurfaces that reduces the friction or wear between them.3.1.2 lubricating grease, na semi-fluid to solid product ofa dispersion of
8、a thickener in a liquid lubricant.3.1.2.1 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.3.1.3 thickener, nin lubricating grease, a
9、 substance com-posed of finely-divided particles dispersed in a liquid lubricantto form the products structure.3.1.3.1 DiscussionThe solid thickener can be fibers (suchas various metallic soaps) or plates or spheres (such as certainnon-soap thickeners), which are insoluble or, at the most, onlyvery
10、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.3.2 Definitions of Terms Specific to This Standard:3.2.1 deleterious particle
11、s, 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 and parallel in metal holders.
12、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 relative number of such solid
13、 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 abrasive to plastic will notne
14、cessarily be abrasive to steel or other bearing materials.Some correlation was obtained in that the contaminant used inSample 3 (see 10.1.1) had a greater wear rate in a laboratoryball bearing abrasive wear test than the contaminant in Sample2.1This test method is under the jurisdiction of ASTM Comm
15、ittee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.G0 on Lubricating Grease.Current edition approved Nov. 1, 2003. Published November 2003. Originallyapproved in 1956. Last previous edition approved in 1999 as D 140499.2For referenced ASTM standards, vi
16、sit 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-
17、2959, United States.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 possible division could be:1 . . less than 10 scratches2 . . 10 to 40 scratches3 . . more than 40 scratches5.2 An ad
18、vantage 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 is shown in Figs. 1 and 2. Asillustrated in Fig. 2, the plastic test plates,31, are rigidly heldin a parallel po
19、sition in square recesses in parts 2 and 7. Theholder, 7, is part of the cap assembly, 7 to 11, which can beremoved as a unit from the body, 3, by removing four capscrews. The lower plate holder, 2, can slide along the axis ofthe main housing, but it is restricted from turning by keys3Suitable, comm
20、ercial acrylic plastic, produced in uniform, highly polishedsheets, is available as Plexiglas and Lucite, manufactured respectively by Rohm andHaas Co. (Independence Mall, Philadelphia, PA) and E. I. du Pont de Nemours andCo. (Wilmington, DE). Sized test plates are available from Koehler Instrument
21、Co.,Inc., 1595 Sycamore Ave., Bohemia, NY 11716.(a) Assembled View(b) Unassembled ViewFIG. 1 Apparatus for Determining Deleterious Particles in Lubricating GreaseD 1404/D 1404M 99 (2003)2spaced 180 apart. Pressure is applied to the plastic plates, 13,through the holder, 2, by means of the coil sprin
22、g, 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 linear amount of springcompression, which in turn, is a measure of the pressureapplied to the two plastic plates. The u
23、pper 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 holder, the wing nut is loosened, andthe handle, 11, is turned. A leather washer, 10, between holder,7, and cap, 8, is used to
24、 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 permitted if it can hold the two plastic test plates parallelto each other; apply and measure a minimum pressure of 200 psi 1.
25、38MPa on the plastic plates; and provide for 30 relative rotation of the twoplates.6.2 Plastic Test Plates4acrylic plastic test plates (two pertest), 1 6 0.050 in. square by18 6 0.025 in. 25.4 6 1.3 mmsquare by 3.2 6 0.64 mm uniformly thick, having a RockwellM hardness of 94 6 10 (Test Method D 785)
26、, and havinghighly polished surfaces protected on both sides with protec-tive paper.NOTE 3Whether dimensioned in inches or millimetres, the plastic testplates should be fabricated to match the square recesses in holders 2 and7.7. Reagents and Materials7.1 Stoddard solvent conforming to Specification
27、 D 235.(WarningFlammable. Vapor harmful.)NOTE 4Other naphthas or pure paraffinic hydrocarbons, such asn-heptane, can be substituted providing they are suitable volatile and donot soften or otherwise attack acrylic plastic.8. Procedure8.1 Use a fine, smoothing file to break sharp edges of oneface of
28、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 tension from the spring anddisassemble the apparatus from the top, Fig. 1b. Snap a testplate into each of the square rece
29、sses 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 solidmaterial, to preclude uneven loading of the plastic plates.8.3 Remove the protective paper from the test plates. Thee
30、xposed 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, orcompressed-gas (ionizing-type recommended) dust remover.8.4 Place a pea-sized (about 0.25 g), representative sampleof the test
31、 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. Turnthe loading screw to apply a pressure of 200 psi 1.38 MPa asindicated by the pointer and scale and the apparatus maker
32、sspring calibration.NOTE 6The scale indicates linear displacement and does not directlyindicate pressure. The apparatus should be supplied with a calibration toconvert the scale reading to pressure. (Consult the manufacturer if thiscalibration information is missing.) One equipment maker reported th
33、efollowing 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 pressure applied to the plates determines the thickness ofthe grease layer between them. A pressure of 200 psi 1.38 M
34、Pa 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 locking wing nut,14, on the cap assembly and turn handle, 11, once as far as itwill go (about 30).8.6 Release the spring
35、pressure and disassemble the appa-ratus. Carefully remove the plastic plates from their holders.8.7 Mark the plates for identification and remove the pro-tective paper from the back faces. Wash the test grease from theplates with filtered Stoddard solvent (WarningFlammable.Vapor harmful) and blow dr
36、y 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.4The apparatus shown in Figs. 1 and 2 is available from Falex
37、 Corp., 1020Airpark Dr., Sugar Grove, IL 605549585 and from Koehler Instrument Co., Inc.,1595 Sycamore Ave., Bohemia, L.I., NY 11716.1 plastic test plates2 lower plate holder3 body4 spring5 spring follower plate6 loading screw7 upper plate holder8 cap9 threaded pin10 leather washer11 handle12 indica
38、tor pin13 key14 wing nutFIG. 2 Cross-section View of ApparatusD 1404/D 1404M 99 (2003)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 Bias51
39、0.1 PrecisionThe precision of this test method was notdetermined with any currently acceptable guidelines of eitherASTM or Committee D02.10.1.1 A series of cooperative tests were run on three greasesamples, two of which were artificially contaminated. Theresults from six different laboratories were:
40、SampleAverage No.of ScratchesStandardDeviation14624183 113 2710.2 BiasThe procedure in Test Method D 1404 has nobias because the value of the estimation of deleterious particlesin lubricating grease can be defined only in terms of a testmethod.11. Keywords11.1 abrasive particles; cleanliness; contam
41、ination; deleteri-ous particles; lubricating grease; particles; scratch testASTM 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 validit
42、y of any such patent rights, and the riskof infringement of such rights, are entirely 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 comment
43、s are invited either for revision of this standard or for additional standardsand 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
44、 received a fair hearing you shouldmake your views known to the ASTM Committee on 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 copi
45、es) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).5There 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 ofScratchingD 1404/D 1404M 99 (2003)4
