1、Designation:D89305a (Reapproved 2010) Designation: D893 11Standard Test Method forInsolubles in Used Lubricating Oils1This standard is issued under the fixed designation D893; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r of last revision. 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 Department of Defense.1. Scope*1.1 This test method covers the det
3、ermination of pentane and toluene insolubles in used lubricating oils.1.2 Procedure A covers the determination of insolubles without the use of coagulant in the pentane. It provides an indicationof the materials that can readily be separated from the oil-solvent mixtures by centrifuging.1.3 Procedur
4、e B covers the determination of insolubles in oils containing detergents and employs a coagulant for both thepentane and toluene insolubles. In addition to the materials separated by using Procedure A, this coagulation procedure separatessome finely divided materials that may be suspended in the oil
5、.NOTE 1Results obtained by Procedures A and B should not be compared since they usually give different values. The same procedure should beemployed when comparing values obtained periodically on an oil in use or when comparing results determined by two or more laboratories.1.4 The values stated in S
6、I units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and heal
7、th practices and determine the applicability of regulatorylimitations prior to use. For specific warning statements, see Section 7 and 9.1.1.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Pra
8、ctice for Automatic Sampling of Petroleum and Petroleum Products3. Terminology3.1 Definitions:3.1.1 coagulate, vto cause to become viscous or thickened into a coherent mass.3.1.2 coagulated pentane insolubles, nin used oil analysis, separated matter that results when a coagulant is added to asolutio
9、n of used oil in pentane.3.1.2.1 DiscussionThe addition of a coagulant will aid in separating finely divided materials that may have been held insuspension because of the dispersant characteristics of the oil.3.1.3 coagulated toluene insolubles, nin used oil analysis, coagulated and separated matter
10、 not soluble in pentane or toluene.3.1.4 pentane insolubles, nin used oil analysis, separated matter resulting when a used oil is mixed with pentane.3.1.4.1 DiscussionIn this test method, the separation is effected by centrifugation.3.1.5 toluene insolubles, nin used oil analysis, the portion of pen
11、tane insolubles not soluble in toluene.3.1.6 used oil, nany oil that has been in a piece of equipment (for example, an engine, gearbox, transformer, or turbine),whether operated or not.3.1.6.1 DiscussionIn this test method, the oil can be any oil that has been used for lubrication.3.2 Definitions of
12、 Terms Specific to This Standard:3.2.1 insoluble resins, nin used oil analysis, separated matter soluble in toluene but not pentane.3.2.1.1 DiscussionInsoluble resins can be calculated for either Procedure A or B by subtracting the toluene insolubles fromthe pentane insolubles.1This test method is u
13、nder the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.06 onAnalysis of Lubricants.Current edition approved MayDec. 1, 2010.2011. Published June 2010.January 2012. Originally approved in 1967. Last previous edition approv
14、ed in 20052010 asD89305a(2010). DOI: 10.1520/D0893-05AR10. 10.1520/D0893-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on
15、the ASTM website.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users
16、 consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoh
17、ocken, PA 19428-2959, United States.4. Summary of Test Method4.1 Procedure AA representative sample of used lubricating oil is mixed with pentane and centrifuged. The oil solution isdecanted and the precipitate washed twice with pentane, dried, and weighed to give the pentane insolubles. For toluene
18、 insolubles,a separate sample of the oil is mixed with pentane and then centrifuged. The precipitate is washed twice with pentane, once withtoluene-alcohol solution, and once with toluene. The insoluble material is then dried and weighed to give the insolubles.4.2 Procedure BArepresentative sample o
19、f used lubricating oil is mixed with pentane-coagulant solution and centrifuged. Theprecipitate is washed twice with pentane, dried, and weighed to give coagulated pentane insolubles. For coagulated tolueneinsolubles a separate sample of the oil is mixed with pentane-coagulant solution and centrifug
20、ed. The precipitate is washed twicewith pentane, once with toluene-alcohol solution, and once with toluene. The insoluble material is then dried and weighed to givecoagulated toluene insolubles.5. Significance and Use5.1 Pentane insolubles can include oil-insoluble materials and some oil-insoluble r
21、esinous matter originating from oil oradditive degradation, or both.5.2 Toluene insoluble materials can come from (1) external contamination, (2 ) fuel carbon and highly carbonized materialsfrom degradation of fuel, oil, and additives, or (3) engine wear and corrosion materials.5.3 A significant cha
22、nge in pentane insolubles, toluene insolubles (with or without coagulant), and insoluble resins indicates achange in oil which could lead to lubrication system problems.5.4 Insolubles measured can also assist in evaluating the performance characteristics of a used oil or in determining the causeof e
23、quipment failure.6. Apparatus6.1 Centrifuge Tube, cone-shaped, conforming to the dimensions given in Fig. 1, and made of thoroughly annealed glass. Thegraduations, numbered as shown in Fig. 1, shall be clear and distinct and the mouth constricted in shape for closure with a cork.Scale error toleranc
24、es and smallest graduations between various calibration marks are given in Table 1 and apply to calibrationsmade with air-free water at 20C.6.2 Centrifuge, meeting all safety requirements for normal use and capable of whirling two or more filled centrifuge tubes ata speed that can be controlled to g
25、ive a relative centrifugal force (rcf) between 600 and 700 at the tips of the tubes. The revolvinghead, trunnion rings, and trunnion cups, including the rubber cushion, shall be soundly constructed to withstand the maximumFIG. 1 ASTM Cone-Shaped Centrifuge TubeD893 112centrifugal force capable of be
26、ing delivered by the power source. The trunnion cups and cushions shall firmly support the tubeswhen the centrifuge is in motion. The centrifuge shall be enclosed by a metal shield or case strong enough to eliminate danger ifany breakage occurs. Calculate the speed of the rotating head as follows:Sp
27、eed, rpm 5 1337 =rcf/d (1)where:rcf = relative centrifugal force, andd = diameter swing, mm, measured between tips of opposite tubes when in rotating position.Table 2 shows the relationship between the diameter of swing, ref and rpm.6.3 Oven, explosion-proof, capable of maintaining a temperature of
28、105 6 3C.6.4 Balance, having a sensitivity of 0.5 mg for weighing the 100-mL beaker and centrifuge tube, and a balance having asensitivity of 0.1 g for weighing the oil sample.7. Reagents and Solvents7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated
29、, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.3Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit
30、its use without lessening the accuracy of the determination.7.2 Purity of WaterUnless otherwise indicated references to water shall be understood to mean water in accordance withSpecification D1193, Type IV.7.3 nbutyl diethanolamine (2,21 (butylimino) diethanol). (Warning May be harmful if inhaled o
31、r swallowed.)7.4 Ethanol, denaturedconforming to either Formula 30 or 3A of the U.S. Bureau of Internal Revenue. (WarningFlammable. Denatured. Cannot be made nontoxic.)7.5 Pentane(Warning Extremely flammable. Vapors may cause flash fires.)7.6 Propan2ol (isopropyl alcohol)(WarningFlammable. Denatured
32、. Cannot be made nontoxic.)7.7 Toluene(Warning Flammable. Vapor harmful.)7.8 Toluene-Alcohol Solution, wash solvent, made by mixing 1 volume of toluene (7.7) with 1 volume of denatured ethanolconforming to either Formula No. 30 or 3A of the U.S. Bureau of Internal Revenue. (WarningFlammable. Denatur
33、ed. Cannotbe made nontoxic.)7.9 Pentane-Coagulant Solution Add 50 mL of n-butyl diethanolamine (WarningFlammable) and 50 mL of isopropylalcohol (2-propanol) (WarningAs used oil may change appreciably in storage, samples should be tested as soon as possible afterremoval from the lubricating system an
34、d the dates of sampling and testing should be noted) to 1 L of n-pentane (WarningMaybe harmful if inhaled or swallowed) and mix.3Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe America
35、n Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.TABLE 1 Calibration Tolerances of Cone-Shaped Centrifuge TubeRange, mLSmallest ScaleDi
36、vision, mLMaximum ScaleError, mL0to0.1 0.05 60.02Over 0.1 to 0.3 0.05 60.03Over 0.3 to 0.5 0.05 60.05Over 0.5 to 1.0 0.1 60.05Over 1.0 to 2.0 0.1 60.10Over 2.0 to 3.0 0.2 60.10Over 3.0 to 5.0 0.5 60.20Over 5.0 to 10.0 1.0 60.50Over 10 to 25 5.0 61.0Over 25 to 100 25.0 61.0TABLE 2 Rotation Speeds for
37、 Centrifuges of Various Diametersof SwingDiameter of Swing, mmArpm at 600 rcf rpm at 700 rcf483 1490 1610508 1450 1570533 1420 1530559 1390 1500AMeasured in millimetres between tips of opposite tubes when in rotatingposition.D893 1138. Sampling8.1 Obtain a sample using either Practice D4057 or D4177
38、.8.2Heat the sample of used oil to 60 6 5C in the original container and agitate until all sediment is homogeneously suspendedin the oil. 8.2 If the original container is of opaque material, or if it is more than three-fourths full, transfer the entire sample toa clear glass bottle having a capacity
39、 at least one third greater than the volume of the sample, and transfer all traces of sedimentfrom the original container to the bottle by violent agitation of portions of the sample in the original container. Heat the sampleof used oil at 60 6 5C for 30 6 1 min and agitate until all sediment is hom
40、ogeneously suspended in the oil. After completesuspension of all sediment, strain the sample or a convenient aliquot through a 150-m (No. 100) sieve to remove largecontaminating particles.NOTE 2When the sample is clear and transparent and visibly free of sediment, the straining procedure described a
41、bove can be omitted.9. Procedure A for Pentane and Toluene Insolubles Without Coagulant9.1 Pentane Insolubles:9.1.1 Dry a clean centrifuge tube for 30 min at 105 6 3C, cool in a desiccator, and weigh to the nearest 1 mg. Weigh 10.0 60.1 g of the prepared sample of used oil into the tube and fill to
42、the 100-mL mark with pentane (WarningMay be harmful ifinhaled or swallowed.). Stopper the tube and shake until the mixture is homogeneous. Do not allow the mixture to stand more than3h.9.1.2 Remove the stopper, and using a wash bottle having a fine jet, wash all insolubles from the stopper into the
43、centrifuge tubewith a minimum of pentane. Balance the weights of each pair of filled centrifuge tubes, place them in the centrifuge on oppositesides of the head, and centrifuge for 20 6 1 min at a rate calculated in accordance with 6.2, sufficient to produce a relativecentrifugal force (rcf) between
44、 600 and 700 at the tips of the whirling tubes. (See Table 2.) Carefully decant the supernatant liquidwithout disturbing or dispersing the precipitate, leaving not more than 3 mL of liquid in the centrifuge tube.NOTE 3Due to safety concerns when handling flammable materials, some laboratories have f
45、ound it suitable to use refrigerated or explosion-proofcentrifuges or hermetically sealed centrifuge cups with screw caps and seals.9.1.3 Add 10 6 1 mL of pentane to the tube. Dislodge and break up all of the insolubles from the bottom of the tube by meansof a clean stiff wire. Wash all insolubles a
46、dhering to the wire back into the tube with pentane, filling the tube to the 50-mL45-mLmark. Stopper the tube and shake until the mixture is homogeneous. Remove and wash the stopper with pentane, filling the tubeto the 50 mL mark. Centrifuge for 20 6 1 min. Pour the supernatant liquid from the centr
47、ifuge tube, using care to avoid disturbingthe cake of insolubles in the bottom of the tube.9.1.4 Repeat the entire operation described in 9.1.3.9.1.5 Dry the centrifuge tube containing the washed precipitate for 30 6 1 min at 105 6 3C, cool in desiccator, and weighto the nearest 1 mg.9.1.6 With rela
48、tively heavy precipitates there can be some spattering if the tube is placed directly from the centrifuge into theoven. In such cases, the precipitate may be partially dried by weathering at room or slightly higher temperatures before beingplaced in the oven.9.2 Toluene Insolubles:9.2.1 Starting wit
49、h a fresh sample of used oil, precipitate and centrifuge the pentane insolubles as described in 9.1.1-9.1.4, butdo not dry the insolubles in the centrifuge tube.9.2.2 Add 10 6 1 mL of toluene-alcohol solution. Break up and dislodge all of the insolubles from the bottom of the centrifugetube by means of a clean, stiff wire. Wash any insolubles adhering to the wire back into the tube with toluene-alcohol solution,using a sufficient amount of this solvent to fill the tube to the 50-mL45-mL mark. Stopper the tube and shake until the mixturei
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