1、Designation: D2273 08 (Reapproved 2016)Standard Test Method forTrace Sediment in Lubricating Oils1This standard is issued under the fixed designation D2273; 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 U.S. Department of Defense.1. Scope1.1 This test method covers the determination of t
3、raceamounts (less than 0.05 % by volume) of sediment in lubricat-ing oils. Since oil-soluble material precipitated by the specifiedsolvent is not intended as part of the measured sediment, thetest method is not applicable in cases where precipitatedoil-soluble components will appreciably contribute
4、to thesediment readings.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.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 st
5、andard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andP
6、etroleum Products3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 trace sediment, nthe number of millilitres of sedi-ment precipitated from 100 mL of oil sample (volume percent)when equal parts of the oil sample and the specified solvent aremixed and centrifuged under the presc
7、ribed conditions.4. Significance and Use4.1 This test measures the trace level amount of sedimentthat is naphtha-insoluble and can be separated by centrifuging.Excessive amounts of sediment in oil could lead to systemmalfunction in critical applications.5. Apparatus5.1 Centrifuge, meeting all the sa
8、fety requirements fornormal use and capable of whirling two or more filledcentrifuge tubes at a speed which can be controlled to give arelative centrifugal force (rcf) between 600 and 700 at the tipof the tubes. The revolving head, trunnion rings, and trunnioncups, including the rubber cushion, shal
9、l be soundly con-structed to withstand the maximum centrifugal force capable ofbeing delivered by the power source. The trunnion cups andcushions shall firmly support the tubes when the centrifuge isin motion. The centrifuge shall be enclosed by a metal shield orcase strong enough to eliminate dange
10、r if any breakage occurs.Calculate the speed of the rotating head as follows:rpm 5 1337 =rcf/d (1)where:rcf = relative centrifugal force, andd = diameter of swing, in millimetres, measured betweentips of opposite tubes when in rotating position.The relationship between the diameter swing, relative c
11、en-trifugal force, and revolutions per minute is given in Table 1.5.2 Centrifuge Tube, cone-shaped, conforming to the di-mensions given in Fig. 1, and made of thoroughly annealedglass. The graduations, numbered as shown in Fig. 1, shall beclear and distinct, and the mouth shall be constructed in a s
12、hapesuitable for closure with a cork. Scale-error tolerances andsmallest graduations between various calibration marks aregiven in Table 2. Calibrated centrifuge tubes shall be purchasedfrom the manufacturer.6. Reagents6.1 Hexanes, reagent grade, minimum purity. (WarningExtremely flammable. Harmful
13、if inhaled. ) See also Note 1.NOTE 1Reagent grade minimum purity hexanes are sometimesreferred to or sold by other names such as precipitation naphtha,1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility
14、 ofSubcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.Current edition approved Oct. 1, 2016. Published November 2016. Originallyapproved in 1964. Last previous edition approved in 2012 as D2273 08 (2012).DOI: 10.1520/D2273-08R16.2For referenced ASTM standards, visit the ASTM website, www
15、.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 States1petrol
16、eum naphtha, petroleum ether, ligroine, petroleum benzin, or indus-trial naphthas.NOTE 2Before use, the hexanes should be free of any extraneousmaterial that might affect the final test readings. For this purpose, it shouldeither be filtered through a membrane filter or centrifuged several timesand
17、decanted just prior to its use.7. Sampling7.1 Refer to Practice D4057 (manual) or D4177 (automatic)for recommended practices for obtaining samples.7.2 The sample shall be thoroughly representative of thematerial in question and the portion used for the test shall bethoroughly representative of the s
18、ample itself. This requiresvigorous agitation of the sample immediately before transfer-ring the sample to the tube. The difficulties in obtainingrepresentative samples for this determination are unusuallygreat; hence, the importance of sampling cannot be toostrongly emphasized.8. Procedure8.1 Measu
19、re 50 mL 6 1 mL of hexanes (see 6.1) into eachof two clean, dry centrifuge tubes at room temperature.(WarningExtremely flammable.) Then fill each tube to the100 mL mark with the oil sample and close tightly with asoftened cork covered with a thin pliable plastic film that isresistant to petroleum pr
20、oducts (not a rubber stopper). Shakesample well to ensure complete mixing, then invert each tubeat least 20 times allowing the liquid to drain thoroughly fromthe tip of the tube at each inversion. If the liquid refuses todrain upon inversion, gently tap the inverted tube against thepalm of the hand
21、to jolt the liquid out of the tip. Place the tubesin a water bath at 32 C to 35 C for 5 min 6 1 min.Momentarily remove the corks to relieve any pressure, andinvert each tube again at least 20 times exactly as before. Thesuccess of this method depends to a large degree upon havinga thoroughly homogen
22、eous mixture which will drain com-pletely as possible from the tip when the tube is inverted.8.2 Balance the two centrifuge tubes or pairs of tubes withtheir respective trunnion cups and place them on opposite sidesof the centrifuge head. Then whirl them for 10 min 6 1 min ata rate sufficient to pro
23、duce a relative centrifuge force (rcf)between 600 and 700 at the tips of the whirling tubes (see 5.1).At the end of the 10 min whirling period, decant the mixturecarefully, allowing the sediment to remain in the tubes.Measure another 50 mL 6 1 mL of the hexanes into each of thetwo tubes, then add th
24、e oil sample until the total volumereaches the 100 mL mark. Then stopper the tubes, repeatedlyinvert, heat, and again invert as described in 8.1. Whirl thetubes in the centrifuge for 10 min 6 1 min as before, repeatingthe 10 min whirling operation until the volume of sediment ineach tube remains con
25、stant for three consecutive readings. Ingeneral, not more than four whirlings will be required for oilshaving low sediment values. Record the final reading forsediment in each tube.9. Calculation9.1 If sediment is present in one or both tubes, as recordedin 8.2, average the final readings for sedime
26、nt in the two tubescontaining the sample to obtain the average volume of sedi-ment per 100 mL sample.10. Report10.1 If no sediment is present in either tube, as determinedand recorded in 8.2, report the sample result as 0.10.2 If the average result determined in 9.1 is 0 % and0.01 %, report the resu
27、lt to the nearest 0.001 %.10.3 If the average result determined in 9.1 is within therange of 0.01 % to 0.05 %, report the result to the nearest0.01 %.11. Precision and Bias11.1 The precision of this test method as determined bystatistical examination of interlaboratory results is as follows:11.1.1 R
28、epeatabilityThe difference between two testresults, obtained by the same operator with the same apparatusunder constant operating conditions on identical test material,TABLE 1 Rotation Speeds for Centrifuges of Various DiametersDiameter of Swing, mmARPM at 600 rcf RPM at 700 rcf483 1490 1610508 1450
29、 1570533 1420 1530559 1390 1500AMeasured in mm between tips of opposite tubes when rotating-position.FIG. 1 Trace Sediment TubeTABLE 2 Trace Sediment Tube Calibration TolerancesRange, mLSmallest ScaleDivision, mLScale Error,max, mL0 to 0.01 0.005 0.001 at 0.010.01 to 0.05 0.01 0.0050.05 to 0.15 0.05
30、 0.010.15 to 0.30 0.05 0.020.30 to 0.50 0.05 0.030.50 to 50 none 1.050 to 100 none 1.0D2273 08 (2016)2would in the long run, in the normal and correct operation ofthe test method, exceed the following values only in one casein twenty:Sediment, percent volume Repeatability0.000 to 0.002 0.0010.003 to
31、 0.005 0.0010.006 to 0.01 0.00211.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would, inthe long run, in the normal and correct operation of the testmethod, exceed the followi
32、ng values only in one case intwenty:Sediment, percent volume Reproducibility0.000 to 0.002 0.0010.003 to 0.005 0.0020.006 to 0.01 0.00311.1.3 BiasTest Method D2273 is empirical and no state-ment of bias can be made.12. Keywords12.1 lubricating oils; trace sedimentASTM International takes no position
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