1、Designation: D322 97 (Reapproved 2012)1Standard Test Method forGasoline Diluent in Used Gasoline Engine Oils byDistillation1This standard is issued under the fixed designation D322; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he year 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 U.S. Department of Defense.1NOTEThe IP logo and designation
3、were removed editorially in September 2016.1. Scope1.1 This test method covers determination of the amount ofdilution in crankcase oils of engines when gasoline has beenused as the fuel.NOTE 1There may be cases in dispute, therefore, the user of this testmethod is advised to establish whether this m
4、ethod will be accepted. Theremay be cases where Test Method D3525 results will be set as the refereevalue.1.2 The values stated in acceptable SI units are to beregarded as the standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is the
5、responsibility 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. For specificprecautionary statement, see 6.4, 7.1, and 9.3.2. Referenced Documents2.1 ASTM Standards:2D235 Specification for Mine
6、ral Spirits (Petroleum Spirits)(Hydrocarbon Dry Cleaning Solvent)D3525 Test Method for Gasoline Diluent in Used GasolineEngine Oils by Gas ChromatographyD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4175 Terminology Relating to Petroleum Products, LiquidFuels, and LubricantsD
7、4177 Practice for Automatic Sampling of Petroleum andPetroleum Products2.2 IP Methods for Analyses and Testing, Vol II, Part I33. Terminology3.1 Definitions:3.1.1 fuel diluent, nin used oil analysis, unburnt fuelcomponents that enter the engine crankcase causing dilution ofthe oil.3.1.1.1 Discussion
8、In this test method, the fuel diluentcomponents being determined are from gasoline.3.1.2 used oil, nany oil that has been in a piece ofequipment (for example, an engine, gearbox, transformer, orturbine) whether operated or not. D41753.1.2.1 DiscussionIn this test method, used oil is from agasoline e
9、ngine.4. Summary of Test Method4.1 The sample, mixed with water, is placed in a glass stillprovided with a reflux condenser discharging into a graduatedtrap connected to the still. Heat is applied, and the contents ofthe still are brought to boiling. The diluent in the sample isvaporized with the wa
10、ter and then liquefied in the condenser.The diluent collects at the top of the trap, and the excess waterruns back to the still where it is again vaporized, carrying overan additional quantity of diluent. The boiling is continued untilall the diluent has been boiled out and recovered in the trap.The
11、 volume is recorded.5. Significance and Use5.1 Some fuel dilution of the engine oil may take placeduring normal operation. However, excessive fuel dilution is ofconcern in terms of possible performance problems.6. Apparatus6.1 Flask, round-bottom type (see Fig. 1 and A1.1).6.2 Condenser, Liebig stra
12、ight-tube type (see A1.2).1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.Current edition approved Nov. 1, 2012. Published November 2
13、012. Originallyapproved in 1930. Last previous edition approved in 2007 as D322 97 (2012).DOI: 10.1520/D0322-97R12E01.2For 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 t
14、o the standards Document Summary page onthe ASTM website.3Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.3 Trap, 5 mL, graduat
15、ed in 0.1 mL increments (see Fig. 1and Fig. 2 and A1.3).6.4 HeaterAny suitable gas burner or electric heater maybe used with the glass flask. (WarningHot exposed surface.Avoid contact by wearing protective equipment as required.)7. Reagents and Materials7.1 Ethanol, Denatured , conforming to either
16、Formula No.30 or 3A of the US Bureau of Internal Revenue. (WarningFlammable. Denatured. Cannot be made non-toxic.)7.2 Mineral Spirits (Petroleum Spirits), conforming toSpecification D235.NOTE 2In Annex A1.3, the use of reagent grade heptane may be thepreferred solvent because the use of commerical g
17、rade heptane or mineralspirits can cause complications of container disposal that may not berequired for the disposal of the containers for reagent grade heptane.8. Sampling8.1 Obtain a representative sample using either PracticesD4057 or D4177.9. Procedure9.1 Mix the sample thoroughly, measure 25 m
18、L 6 5mLbymeans of a 25 mL graduated cylinder, and transfer as much aspossible of the contents of the cylinder by pouring it into theflask. Wash the graduated cylinder with successive portions ofhot water until only a negligible amount of oil is left in thecylinder. Add additional water to the flask
19、to make a total ofapproximately 500 mL of water. Fill the trap with cold waterand add 1 mL 6 0.1 mL of denatured ethanol to the water inthe trap.9.2 Assemble the apparatus as shown in Fig. 1, so that thetip of the condenser is directly over the indentation in the trap.9.3 Apply heat to the flask at
20、such a rate that refluxing startswithin 7 min to 10 min after heat is applied, with the water andsample being at 21 C to 38 C prior to application of heat.After boiling and condensation has commenced, adjust the rateof boiling so that condensed distillate is discharged from thecondenser at a rate of
21、 1 to 3 drops per s. (WarningHotexposed surface. Avoid contact by wearing protective equip-ment as required.)NOTE 3Bumping with a tendency to froth over is often experiencedwith dirty oils. The use of boiling stones, steel wool, or about 5 mL ofconcentrated hydrochloric acid (HCl) in the flask is of
22、ten helpful ineliminating this difficulty.9.4 Obtain readings of the amount of diluent at the follow-ing times, taken from the time that refluxing starts: 5 min,15 min, and 30 min, 61 min, and each 15 min, 61 min,following until the test is complete. Completion of the test shallbe determined on the
23、basis of either or both of the followingcriteria:9.4.1 The test is complete when the volume of diluentincreases by not more than 0.1 mL in any 15 min period duringthe course of the test.FIG. 1 Apparatus for Determining Diluent in Gasoline Engine Crankcase OilD322 97 (2012)129.4.2 The test is complet
24、e when the volume of diluentobtained in a given time indicates completion, as follows:Time from Start ofRefluxingTest is Complete if ApparentVolume of Diluent Collected isEqual to or Less Than:5 min no visible diluentA30 min 2.0 mL60 min 4.0 mL90 min 5.0 mLAReport as “no dilution;” otherwise the tes
25、t should be continued at least 30 min.9.5 When the test continues without reaching the limitdefined in 9.4.1, to a point at which any of the conditionsdescribed in 9.4.2 are encountered, the latter shall define thecompletion of the test.9.6 When the test is complete by either of the criteriadefined
26、in 9.4.1 and 9.4.2, turn off the heat. Allow theequipment to stand for at least 30 min to allow the distillate toseparate completely and to cool to approximately room tem-perature. Read the volume of diluent collected in the trap. If thevolume of diluent exceeds the calibrated capacity of the trap,d
27、iscontinue the test and report the results as 20 % plus.10. Calculation10.1 The diluent content of the sample, expressed as volumepercent, is equal to the volume of diluent in millilitresmultiplied by 4.NOTE 4In some cases with samples containing large amounts ofdiluent, equipment limitations do not
28、 permit collection and measurementof the full 5 mL of diluent even when more is present. This conditionexists when the upper limit of the collected diluent is above the zerocalibration mark on the trap. When it occurs, finish the test as prescribedin 9.6, read the maximum volume of diluent collected
29、, calculate thecorresponding percentage x, and report the results as x percent plus.11. Report11.1 Report the result as the Diluent Content, ASTM D322.12. Precision and Bias12.1 The precision of this test method as obtained bystatistical examination of interlaboratory test results is asfollows:12.1.
30、1 RepeatabilityThe difference between successivetest results, obtained by the same operator with the sameapparatus under constant operating conditions of identical testmaterial, would in the long run, in the normal and correctoperation of the test method, exceed the following value onlyin one case i
31、n twenty:0.6 volume% (1)12.1.2 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 following valu
32、e only in one case in twenty:1.4 volume% (2)12.2 BiasThe procedure in this test method has no biasbecause the volume percent of gasoline diluent can only bedefined in terms of this test method.13. Keywords13.1 distillation; engine oils; gasoline distillation; usedAll dimensions are in millimetresFIG
33、. 2 Alternate Closures for Diluent TrapD322 97 (2012)13ANNEX(Mandatory Information)A1. APPARATUSA1.1 Flask, round-bottomed, short-necked, having a nomi-nal capacity of 1 L. Fig. 1 and Fig. 2 show recommendeddesigns and glass connections.A1.2 Condenser , Liebig straight type with a jacket not lesstha
34、n 400 mm long, and with an inner tube having an outsidediameter of 10 mm to 13 mm. Fig. 1 and Fig. 2 showcharacteristic details of suitable condensers.A1.3 Trap, in accordance with the details of constructionshown in Fig. 1 and Fig. 2, and conforming to the followingrequirements: It shall be graduat
35、ed from 0 mL to 5 mL in0.1 mL divisions. It shall be calibrated at four or more pointsby first filling it with water and then adding Stoddard solventor n-heptane from a standard buret having a calibrated capacityat least equal to that of the trap. The Stoddard solvent shouldconform to Specification
36、D235. The n-heptane should conformto the current IP specification (see 2.1). The error of theindicated volume shall not exceed 0.05 mL.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this stand
37、ard are expressly advised 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 andi
38、f not revised, either reapproved 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, wh
39、ich 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 address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
40、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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 97 (2012)14
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