1、Designation: D 4055 04An American National StandardStandard Test Method forPentane Insolubles by Membrane Filtration1This standard is issued under the fixed designation D 4055; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of pentaneinsolubles for particles exceeding 0.8 m in new and usedlu
3、bricating oils.NOTE 1Pentane insolubles with particle sizes less than 0.8 m may bestudied with appropriate size membrane filters. Particle sizes above orbelow 0.8 m can be studied. The precision of this test method has beendetermined only at 0.8 m.1.2 The values stated in SI units are to be regarded
4、 as thestandard.1.3 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 limitations prior to use
5、. For specificwarning statements, see 7.1, 8.2.1, and Annex A1.2. Referenced Documents2.1 ASTM Standards:2D 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD 4177 Practice for Automatic Sampling of Petrole
6、um andPetroleum Products3. Terminology3.1 Definitions:3.1.1 pentane insolubles, in used oil analysis, nseparatedmatter resulting when a used oil is dissolved in pentane.3.1.1.1 DiscussionIn this method, the separation is ef-fected by filtration through a membrane.3.1.2 used oil, nany oil that has be
7、en in a piece ofequipment (for example, an engine, gearbox, transformer, orturbine) whether operated or not. D 41754. Summary of Test Method4.1 A sample of new or used lubricating oil is mixed withpentane in a volumetric flask. The oil solution is filteredthrough an 0.8-m membrane filter. The flask,
8、 funnel, and filterare washed with additional pentane to effect a completetransfer of particulates onto the filter. The filter and itsparticulates are dried and weighed to give the pentane in-solubles.5. Significance and Use5.1 Pentane insolubles above 0.8 m in size may lead toincreased wear. This i
9、ncreased wear can lead to prematureequipment failure in critical applications.6. Apparatus6.1 In the development of this test method, it was noted thatvariations, particularly with respect to glassware and filtermedia, can affect the test result significantly.6.2 When the user of this test method us
10、es an alternatemembrane filter, it is incumbent upon them to establish that thealternate filter will give equal results.6.3 Precision data were established using the apparatuslisted and a 0.8 m filter pore size.6.4 Membrane Filter.36.5 Borosilicate Filter Holder.46.6 Borosilicate Filtering Flask.56.
11、7 Forceps6(plain flat tips, not serrated),6.8 Wash Bottle7equipped with 0.8-m membranes.6.9 Analytical Balance, capable of weighing with an accu-racy of 60.1 mg.6.10 Vacuum Source, capable of maintaining a vacuum of255 6 50 mm Hg.6.11 Oven, capable of maintaining 90 6 5C.6.12 Oven Thermometer, ASTM
12、Thermometer 1C.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.06 on Analysis of Lubricants.Current edition approved May 1, 2004. Published June 2004. Originallyapproved in 1992. Last previous e
13、dition approved in 2002 as D 405502.2For 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.3Millipore AAWP04700, ava
14、ilable from Millipore Corp, Bedford MA, 01273,has been found to be satisfactory; also an equivalent may be used.4Millipore XX1004700, available from Millipore Corp, Bedford MA, 01273,has been found to be satisfactory; also an equivalent may be used.5Millipore XX1004705, available from Millipore Corp
15、, Bedford MA, 01273,has been found to be satisfactory; also an equivalent may be used.6Millipore XX6200006, available from Millipore Corp, Bedford MA, 01273,has been found to be satisfactory; also an equivalent may be used.7Millipore XX6602500, available from Millipore Corp, Bedford MA, 01273,has be
16、en found to be satisfactory; also an equivalent may be used.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.13 Aluminum Foil Weighing Dish, about 60 mm in diam-eter.
17、6.14 Desiccator, with calcium chloride.6.15 Mechanical Paint Shaker, three-dimensional.86.16 Volumetric Flask, 100-mL with ground-glass or TFE-fluorocarbon stopper.6.17 Ionizing Unit9, insert under or next to balance pan.7. Reagent7.1 Pentane, reagent grade or better. (WarningExtremelyflammable. Vap
18、ors can cause flash fire. See A1.1.)8. Procedure8.1 Using either Practice D 4057 (manual sampling) orPractice D 4177 (automatic sampling), obtain a representativesample of the material to be tested.8.1.1 Preparation of Sample and Materials:8.1.2 Warm the oil in the original container, if possible, t
19、o60 6 5C. Shake for a minimum of 30 min on the mechanicalshaker to resuspend the insolubles uniformly.NOTE 2Deviation from this sample preparation will normally result inpoor precision. Correct sample size is particularly important.8.1.3 Weigh1gofarepresentative sample of the oil into a100-mL volume
20、tric flask to the nearest 0.01 g.8.1.3.1 Certain oils may require smaller size samples toprevent plugging the membrane. When the 100 mL of themixture has not passed through the membrane after 2 min,discard the test and repeat with a smaller sample size (610 %)in the order listed:0.80 0.33 0.13 0.050
21、.64 0.26 0.11 0.040.51 0.21 0.09 0.030.41 0.17 0.07 0.028.1.4 Filter pentane through an 0.8-m filter.8.2 Preparation of Membrane:8.2.1 Wash the membrane with 100 mL of filtered pentane(WarningSee 7.1) and place the membrane right side up(8.2.1.1) into individual aluminum weighing dish.8.2.1.1 Import
22、antThe top side of the membrane as re-moved from the manufacturers container shall be similarlyorientated for the duration of the procedure. If the filter isreversed, the results are invalid.8.2.2 Place the dish into the oven and dry for a minimum of30 min at 90 6 5C. At the end of the drying period
23、, removethe dish from the oven and cool for a minimum of 30 min in adesiccator containing calcium chloride or some other materialthat will assure an atmosphere free of moisture and hydrocar-bon vapors.8.2.3 When the membranes have reached equilibrium(about 30 min), weigh the membrane to the nearest
24、0.1 mg.8.2.4 Store the aluminum dish in the desiccator until readyfor use.8.3 Filtration:8.3.1 Remove the membrane filter from the weighing dishwith the flat forceps and center in the filtering apparatus.Assemble the funnel and clamp.8.3.2 Fill the volumetric flask containing the sample to the100-mL
25、 mark with filtered pentane. Stopper and shake well.Immediately filter the mixture using a vacuum of 255 6 50 mmHg (see 8.1.3.1). Rinse the flask and stopper twice with smallamounts of filtered pentane, pouring the washings down thesides of the filter funnel. Rinse the walls of the filter funnelwith
26、 a gentle stream of pentane dispensed from the wash bottle.8.3.3 Carefully, remove the clamp and funnel. Wash anyadhering insolubles from the funnel onto the membrane, usingthe wash bottle with pentane. Wash the membrane gently,particularly the edges, with pentane from the wash bottle. Ifany sample
27、fails to remain on the membrane, the test must berepeated.8.3.4 Release the vacuum and carefully remove the mem-brane with the forceps. Place in the same aluminum weighingdish originally used and dry in the oven and cool in thedesiccator as in 8.2.2. Weigh the membrane to the nearest 0.1mg.NOTE 3The
28、 use of a semimicro balance for particulates weighing lessthan 0.0010 g is strongly recommended.9. Calculation9.1 Calculate the pentane insolubles content of the oil bymembrane filtration as follows:Pentane insolubles, % 5 100M22 M1!/S (1)where:S = mass of sample, g,M1= initial mass of membrane, g,
29、andM2= final mass of membrane and insolubles, g.10. Report10.1 Report the percentages of pentane insolubles by mem-brane filtration as:pentane insolubles (0.8 m) percent weight10.2 Some new oil chemistry will require determination ofa baseline value for the new oil (that is, the blank determinationm
30、ay not be zero).11. Precision and Bias1011.1 The precision of this test method as determined bystatistical examination of interlaboratory results is as follows:11.1.1 RepeatabilityThe difference between two test re-sults, obtained by the same operator with the same apparatusunder constant operating
31、conditions on identical test material,would in the long run, in the normal and correct operation ofthe test method, exceed the following values only in one casein twenty:0.177 X2/3(2)where:8Red Devil 5400 or an equivalent is preferred.9Staticmaster 24500 has been found to be satisfactory; also an eq
32、uivalent may beused.10Supporting data have been filed at ASTM International and may be obtainedby requesting Research Report RR: D021209.D4055042X = average of two results.11.1.2 ReproducibilityThe interlaboratory precision (re-producibility) of this test is very poor, and this method ofmeasuring pe
33、ntane insolubles is unsuitable for the purpose ofcomparison of interlaboratory results. Additional cooperativestudies to improve the precision are planned.0.759 X2/3(3)where:X = average of two results.11.2 BiasA statement of bias is not applicable since astandard reference material for this property
34、 is not available.12. Keywords12.1 lubricating oils; membrane filtration; pentaneinsolublesANNEX(Mandatory Information)A1. WARNING STATEMENTSA1.1 PentaneWarningExtremely flammable liquid!Vapors may cause flash fire.Keep away from heat, sparks, and open flame.Keep container closed.Use with adequate v
35、entilation.Avoid buildup of vapors and eliminate all sources ofignition, especially nonexplosion-proof electrical devices andheaters.Avoid prolonged breathing of vapor or spray mist.Avoid prolonged or repeated skin contact.SUMMARY OF CHANGESSubcommittee D02.06 has identified the location of selected
36、 changes to this standard since the last issue(D 405502) that may impact the use of this standard.(1) Rewrote Eq 2 for calculating repeatability in 11.1.1 tocorrect a publication error.(2) Rewrote Eq 3 for calculating reproducibility in 11.1.2 tocorrect a publication error.ASTM International takes n
37、o 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 entirely their own respon
38、sibility.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 should be addressed
39、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 Standards, at the ad
40、dress 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 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D4055043
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