1、Designation: D 322 97 (Reapproved 2007)Designation: 23/2000An American National StandardStandard Test Method forGasoline Diluent in Used Gasoline Engine Oils byDistillation1This standard is issued under the fixed designation D 322; the number immediately following the designation indicates the year
2、oforiginal adoption or, in the case of revision, the year of last 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 Departmen
3、t of Defense.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 method will be accepted. Therem
4、ay be cases where Test Method D 3525 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 theresponsibility of the user of
5、 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:2D 235 Specification for Mineral Spirits (Petroleum Spiri
6、ts)(Hydrocarbon Dry Cleaning Solvent)D 3525 Test Method for Gasoline Diluent in Used GasolineEngine Oils by Gas ChromatographyD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD 4177 Practice for Automatic
7、 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 DiscussionIn this test method, the fu
8、el 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. D 41753.1.2.1 DiscussionIn this test method, used oil is from agasoline engine.4. Summary of Test M
9、ethod4.1 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 water and then liquefied in
10、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 volume is recorded.5. Sig
11、nificance 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 straight-tube type (see A1.2).
12、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.This test method was adopted as a joint ASTM-IP standard in 1964. In the IP, thismethod is under the jurisdiction of
13、the Standardization Committee.Current edition approved May 1, 2007. Published June 2007. Originally approvedin 1930. Last previous edition approved in 2002 as D 322 97 (2002)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. F
14、or Annual Book of ASTMStandards volume information, refer to 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consho
15、hocken, PA 19428-2959, United States.6.3 Trap, 5 mL, graduated 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
16、 and Materials7.1 Ethanol, Denatured , conforming to either 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 D 235.NOTE 2In Annex A1.3, the use of reagent grade heptan
17、e may be thepreferred solvent because the use of commerical grade 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 PracticesD 4057 or
18、 D 4177.9. Procedure9.1 Mix the sample thoroughly, measure 25 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 oi
19、l is left in thecylinder. Add additional water to the flask to make a total ofapproximately 500 mL of water. Fill the trap with cold waterand add 1 6 0.1 mL of denatured ethanol to the water in thetrap.9.2 Assemble the apparatus as shown in Fig. 1, so that thetip of the condenser is directly over th
20、e indentation in the trap.9.3 Apply heat to the flask at such a rate that refluxing startswithin 7 to 10 min after heat is applied, with the water andsample being at 21 to 38C prior to application of heat. Afterboiling and condensation has commenced, adjust the rate ofboiling so that condensed disti
21、llate is discharged from thecondenser at a rate of 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 ofconce
22、ntrated hydrochloric acid (HCl) in the flask is often 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, 15, and30 min, 6 1 min, and each 15 min, 6 1 min, following untilthe test is complete. Compl
23、etion of the test shall be determinedon the basis of either or both of the following criteria: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
24、 OilD 322 97 (2007)29.4.2 The test is complete when the volume of diluentobtained in a given time indicates completion, as follows:Time from Start of Re-fluxingTest 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.
25、0 mLAReport as “no dilution;” otherwise the test 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 tes
26、t is complete by either of the criteriadefined 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 diluen
27、t exceeds the calibrated capacity of the trap,discontinue 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
28、amounts ofdiluent, equipment limitations do not 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.
29、6, read the maximum volume of diluent collected, calculate thecorresponding percentage x, and report the results as x percent plus.11. Report11.1 Report the result as the Diluent Content, ASTMD322IP23.12. Precision and Bias12.1 The precision of this test method as obtained bystatistical examination
30、of interlaboratory test results is asfollows:12.1.1 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 me
31、thod, exceed the following value onlyin one case in 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 ope
32、ration of the testmethod, exceed the following value 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 di
33、stillation; usedAll dimensions are in millimetresFIG. 2 Alternate Closures for Diluent TrapD 322 97 (2007)3ANNEX(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 Conden
34、ser, Liebig straight type with a jacket not lessthan 400 mm long, and with an inner tube having an outsidediameter of 10 to 13 mm. Fig. 1 and Fig. 2 show characteristicdetails of suitable condensers.A1.3 Trap, in accordance with the details of constructionshown in Fig. 1 and Fig. 2, and conforming t
35、o the followingrequirements: It shall be graduated from 0 to 5 mL in 0.1-mLdivisions. It shall be calibrated at four or more points by firstfilling it with water and then adding Stoddard solvent orn-heptane from a standard buret having a calibrated capacity atleast equal to that of the trap. The Sto
36、ddard solvent shouldconform to Specification D 235. 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
37、mentionedin this standard. Users of this standard 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 commit
38、tee and must be reviewed every five years andif 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 mee
39、ting of theresponsible technical committee, which 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,
40、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).D 322 97 (2007)4
