1、Designation: D 2273 05An American National StandardStandard Test Method forTrace Sediment in Lubricating Oils1This standard is issued under the fixed designation D 2273; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 determin
3、ation of traceamounts (less than 0.05 volume %) of sediment in lubricatingoils. 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 contri
4、bute 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 th
5、is standard 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:2D 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petrole
6、um andPetroleum 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 th
7、e prescribed 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
8、 the safety 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 cushio
9、n, shall 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 eliminat
10、e danger 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, rel
11、ative cen-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
12、 in a shapesuitable for closure with a cork. Scale-error tolerances andsmallest graduations between various calibration marks aregiven in Table 2 and apply to calibrations made with redistilledmercury up to the 0.30-mL mark and distilled water for allremaining marks at 20C.6. Reagents6.1 Hexanes, re
13、agent grade, minimum purity. (WarningExtremely flammable. Harmful if inhaled.) See also Note 1.1This 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 approv
14、ed Nov. 1, 2005. Published November 2005. Originallyapproved in 1964. Last previous edition approved in 2002 as D 227397(2002)e2.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informati
15、on, refer to the standards Document Summary page onthe ASTM website.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.NOTE 1Reagent grade minimum purity hexanes are some
16、times re-ferred to or sold by other names such as precipitation naphtha, petroleumnaphtha, petroleum ether, ligroine, petroleum benzin, or industrial naph-thas.NOTE 2Before use, the hexanes should be free of any extraneousmaterial that might affect the final test readings. For this purpose, it shoul
17、deither be filtered through a membrane filter or centrifuged several timesand decanted just prior to its use.7. Sampling7.1 Refer to Practice D 4057 (manual) or D 4177 (auto-matic) for recommended practices for obtaining samples.7.2 The sample shall be thoroughly representative of thematerial in que
18、stion and the portion used for the test shall bethoroughly representative of the sample 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,
19、 the importance of sampling cannot be toostrongly emphasized.8. Procedure8.1 Measure 50 6 1 mL of hexanes (see 6.1) into each oftwo 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
20、 cork covered with a thin pliable plastic film that isresistant to petroleum products (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 to
21、drain upon inversion, gently tap the inverted tube against thepalm of the hand to jolt the liquid out of the tip. Place the tubesin a water bath at 32 to 35C for 5 6 1 min. Momentarilyremove the corks to relieve any pressure, and invert each tubeagain at least 20 times exactly as before. The success
22、 of thismethod depends to a large degree upon having a thoroughlyhomogeneous mixture which will drain completely as possiblefrom 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 centrifu
23、ge head. Then whirl them for 10 6 1 min at a ratesufficient to produce a relative centrifuge force (rcf) between600 and 700 at the tips of the whirling tubes (see 5.1). At theend of the 10-min whirling period, decant the mixture care-fully, allowing the sediment to remain in the tubes. Measureanothe
24、r 50 6 1 mL of the hexanes into each of the two tubes,then add the oil sample until the total volume reaches the100 mL mark. Then stopper the tubes, repeatedly invert, heat,and again invert as described in 8.1. Whirl the tubes in thecentrifuge for 10 6 1 min as before, repeating the 10-minwhirling o
25、peration until the volume of sediment in each tuberemains constant for three consecutive readings. In general, notmore than four whirlings will be required for oils having lowsediment values. Record the final reading for sediment in eachtube.9. Calculation9.1 If sediment is present in one or both tu
26、bes, as recordedin 8.2, average the final readings for sediment 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 avera
27、ge result determined in 9.1 is 0 and0.01 %, report the result 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 nearest 0.01 %.11. Precision and Bias11.1 The precision of this test method as determined bystatistical exa
28、mination of interlaboratory results is as follows:11.1.1 RepeatabilityThe difference between two test re-sults, obtained by the same operator with the same apparatusTABLE 1 Rotation Speeds for Centrifuges of Various DiametersDiameter of Swing, mmARPM at 600 rcf RPM at 700 rcf483 1490 1610508 1450 15
29、70533 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, mL0to0.01 0.005 60.001 at 0.010.01 to 0.05 0.01 60.0050.05 to 0.15 0.05 60
30、.010.15 to 0.30 0.05 60.020.30 to 0.50 0.05 60.030.50 to 50 none 61.050 to 100 none 61.0D2273052under constant operating 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:Sediment,
31、 percent volume Repeatability0.000 to 0.002 0.0010.003 to 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 an
32、d correct operation of the testmethod, exceed the following 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 D 2273 is empirical and nostatement of bias can be made.12. Keywords12.1 lubricating
33、oils; trace sedimentSUMMARY OF CHANGESSubcommittee D02.06 has identified the location of selected changes to this standard since the last issue(D 227397(2002)e2) that may impact the use of this standard.(1) Removed Test Methods D 86, D 611, and D 1298 from theReferenced Documents and text.(2) Update
34、d 6.1, Note 1, Note 2, 8.2, and 9.1.(3) Corrected 8.1.(4) Deleted former Table 3.(5) Added Section 10, Report.ASTM 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
35、 that determination of the validity 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 rea
36、pproved or withdrawn. Your comments 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 yo
37、u feel that your comments have not 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 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).D2273053
