1、Designation: D322 97 (Reapproved 2016)Standard 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, th
2、e 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.1. Scope1.1 This test method cover
3、s 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. Theremay be cases where Test Method D3525 results wil
4、l 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 this standard to establish appro-priate safety
5、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 Mineral Spirits (Petroleum Spirits)(Hydrocarbon Dry Cleaning Solvent)D3525 Test M
6、ethod 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 LubricantsD4177 Practice for Automatic Sampling of Petroleum andPetroleum Products2.2 IP
7、 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 fuel diluentcomponents being determined are from gas
8、oline.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 engine.4. Summary of Test Method4.1 The sample, mixed with water, is placed in
9、 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 the condenser.The diluent collects at the top of th
10、e 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. Significance and Use5.1 Some fuel dilution of the engi
11、ne 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).1This test method is under the jurisdiction of ASTM
12、 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 Oct. 1, 2016. Published November 2016. Originallyapproved in 1930. Last previous edition approved in 2012 as D3
13、22 97 (2012)1.DOI: 10.1520/D0322-97R16.2For 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 to the standards Document Summary page onthe ASTM website.3Available from Energy
14、 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, graduated in 0.1 mL increments (see Fig. 1and Fig. 2 and A1.3).6.4 HeaterAny suitable
15、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 Formula No.30 or 3A of the US Bureau of Internal Revenue. (WarningFlammable. De
16、natured. 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 grade heptane or mineralspirits can cause complications of container disposal th
17、at 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 mL 6 5mLbymeans of a 25 mL graduated cylinder, and transfer as much aspossible o
18、f 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 to make a total ofapproximately 500 mL of water. Fill the trap with cold watera
19、nd 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 such a rate that refluxing startswithin 7 min to 10 min after heat is applied,
20、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 1 to 3 drops per s. (WarningHotexposed surface. Avoid contact by wearing prote
21、ctive 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 often helpful ineliminating this difficulty.9.4 Obtain readings of the amount of
22、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 basis of either or both of the followingcriteria:9.4.1 The test is complete whe
23、n 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 (2016)29.4.2 The test is complete when the volume of diluentobtained in a given time indicates completion, as fo
24、llows: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 test should be continued at least 30 min.9.5 When the test continues without reachi
25、ng 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 in 9.4.1 and 9.4.2, turn off the heat. Allow theequipment to stand for at least
26、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,discontinue the test and report the results as 20 % plus.10. Calculation10.1 The
27、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 permit collection and measurementof the full 5 mL of diluent even when more is
28、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, calculate thecorresponding percentage x, and report the results as x percent p
29、lus.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:12.1.1 RepeatabilityThe difference between successivetest results, obtained by the sa
30、me 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 in twenty:0.6 volume% (1)12.1.2 ReproducibilityThe difference between two singlea
31、nd 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 value only in one case in twenty:1.4 volume% (2)12.2 BiasThe procedure in this test
32、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. 2 Alternate Closures for Diluent TrapD322 97 (2016)3ANNEX(Mandatory Informatio
33、n)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 lessthan 400 mm long, and with an inner tube having an outsidediameter of 10 mm to 13 mm
34、. 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 graduated from 0 mL to 5 mL in0.1 mL divisions. It shall be calibrated at four or more p
35、ointsby 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 D235. The n-heptane should conformto the current IP specification (see 2.1). The
36、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 standard are expressly advised that determination of the validity of any such patent r
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39、ng 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 m
40、ay 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 (2016)4
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