1、Designation:D89311 Designation: D893 12Standard 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 year of last revision.
2、 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 determination of penta
3、ne 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 Procedure B covers the dete
4、rmination 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.NOTE 1Results obta
5、ined 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 SI units are to be r
6、egarded 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 health practices and de
7、termine 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 Practice for Automatic
8、 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 asolution of used oil in pe
9、ntane.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 not soluble in pen
10、tane 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 pentane insolubles not
11、 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 Terms Specific to
12、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 under the jurisdicti
13、on of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.06 onAnalysis of Lubricants.Current edition approved Dec. 1, 2011.April 15, 2012. Published JanuaryMay 2012. Originally approved in 1967. Last previous edition approved in 20102011 asD8
14、9305a(2010).D89311. DOI: 10.1520/D0893-112.2For 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 the ASTM website.1This document i
15、s 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 consult prior editions as approp
16、riate. 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 Conshohocken, PA 19428-2959, United Stat
17、es.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 insolubles,a separate sample of
18、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 of used lubricating oil is mixed w
19、ith 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 centrifuged. The precipitate is washed twi
20、cewith 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 resinous matter originating from o
21、il 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 change in pentane insolubles, toluen
22、e 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 equipment failure.6. Apparatus6.1
23、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 tolerances and smallest graduations betwe
24、en 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 give a relative centrifugal force
25、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 122centrifugal force capable of being delivered by the power source
26、 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:Speed, rpm 5 1337 =rcf/d (1)D0893-1
27、2_1where: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 105 6 3C.6.4 Balance, h
28、aving 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, it is intended that a
29、llreagents 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 its use without lesseni
30、ng 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 or swallowed.)7.4 Ethano
31、l, 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. Cannot be made nontox
32、ic.)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. Denatured. Cannotbe made nonto
33、xic.)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 after3Reagent Chemicals, American Chemical Society Specifications,
34、 American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American 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, In
35、c. (USPC), Rockville, MD.TABLE 1 Calibration Tolerances of Cone-Shaped Centrifuge TubeRange, mLSmallest ScaleDivision, 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
36、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 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 oppo
37、site tubes when in rotatingposition.D893 123removal from the lubricating system and the dates of sampling and testing should be noted) to 1 L of n-pentane (WarningMaybe harmful if inhaled or swallowed) and mix.8. Sampling8.1 Obtain a sample using either Practice D4057 or D4177.8.2 If the original co
38、ntainer is of opaque material, or if it is more than three-fourths full, transfer the entire sample to a clearglass bottle having a capacity at least one third greater than the volume of the sample, and transfer all traces of sediment from theoriginal container to the bottle by violent agitation of
39、portions of the sample in the original container. Heat the sample of used oilat 60 6 5C for 30 6 1 min and agitate until all sediment is homogeneously suspended in the oil. After complete suspension ofall sediment, strain the sample or a convenient aliquot through a 150-m (No. 100) sieve to remove l
40、arge contaminating particles.NOTE 2When the sample is clear and transparent and visibly free of sediment, the straining procedure described above 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 6 1 min
41、at 105 6 3C, cool in a desiccator, and weigh to the nearest 1 mg. Weigh 10.06 0.1 g of the prepared sample of used oil into the tube and fill to the 100-mL75-mL mark with pentane (WarningMay beharmful if inhaled or swallowed.). Stopper the tube and shake until the mixture is homogeneous. Do not allo
42、w the mixture to standmore than 3 h.9.1.2 Remove the stopper, and using a wash bottle having a fine jet, wash all insolubles from the stopper into the centrifuge tubewith a minimum of pentane. Balance the weights of each pair of filled centrifuge tubes, place them in the centrifuge on oppositesides
43、of the head, and centrifuge for 20 6 1 min at a rate calculated in accordance with Remove the stopper, and using a washbottle having a fine jet, wash all insolubles from the stopper with pentane into the centrifuge tube and bring the solvent level upto the 100 mL mark. Arrange the tubes symmetricall
44、y about the centrifuge to minimize imbalance. In the event of an odd numberof tubes, using water, fill a dummy tube to the same mass as the sample to balance the odd tube, and centrifuge for 20 6 1 minat a rate calculated in accordance with 6.2, sufficient to produce a relative centrifugal force (rc
45、f) between 600 and 700 at the tipsof the whirling tubes. (See Table 2.) Carefully decant the supernatant liquid without disturbing or dispersing the precipitate, leavingnot more than 3 mL of liquid in the centrifuge tube.NOTE 3Due to safety concerns when handling flammable materials, some laboratori
46、es have found 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 ins
47、olubles adhering to the wire back into the tube with pentane, filling the tube to the 45-mL25-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
48、the centrifuge 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
49、With relatively 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 with 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 al
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