ASTM_D_4291_-_04_2013.pdf

Designation:D429104(Reapproved 2013)Standard Test Method forTrace Ethylene Glycol in Used Engine Oil1This standard is issued under the fixed designation D4291;the number immediately following the designation indicates the year 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()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the determination of ethyleneglycol as a contaminant in used engine oil.This test method isdesigned to quantitate ethylene glycol in the range from 5 to200 mass ppm.1.2 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 and health practices and determine the applica-bility of regulatory limitations prior to use.FOR SPECIFIC WARNINGSTATEMENTS,SEESECTION6.NOTE1A qualitative determination of glycol-base antifreeze isprovided in Test Methods D2982.Procedure A is sensitive to about 100ppm.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD2982 Test Methods for Detecting Glycol-Base Antifreezein Used Lubricating OilsD4057 Practice for Manual Sampling of Petroleum andPetroleum Products3.Summary of Test Method3.1 The sample of oil is extracted with water and theanalysis is performed on the water extract.A reproduciblevolume of the extract is injected into a gas chromatographusing on-column injection and the eluting compounds aredetected by a flame ionization detector.The ethylene glycolpeak area is determined and compared with areas obtainedfrom the injection of freshly prepared known standards.4.Significance and Use4.1 Leakage of aqueous engine coolant into the crank caseweakens the ability of the oil to lubricate.If ethylene glycol ispresent,it promotes varnish and deposit formation.This testmethod is designed for early detection to prevent coolant fromaccumulating and seriously damaging the engine.5.Apparatus5.1 GasChromatographAnygaschromatographequipped with the following:5.1.1 Flame Ionization Detector,capable of operating con-tinuously at a temperature equivalent to the maximum columntemperature employed,and connected to the column so as toavoid any cold spots.5.1.2 Sample Inlet System,providing for on-column injec-tion and capable of operating continuously at a temperatureequivalent to the maximum column temperature employed.5.2 RecorderRecording potentiometer with a full-scaleresponse time of 2 s or less may be used.5.3 Columns1.2-m(4-ft)by 6.4-mm(14-in.)copper tubepacked with 5 mass%Carbowax 20-M liquid phase on 30/60mesh Chromosorb T solid support.As an alternative,a fusedsilica capillary column,15 m long with a 0.53mm ID and2.0micron film thickness of a bonded polyethylene glycol canbe used.5.4 IntegratorManual,mechanical,or electronic integra-tion is required to determine the peak area.However,bestprecision and automated operation can be achieved withelectronic integration.5.5 CentrifugeRCF 600 minimum and centrifuge tubeswith stoppers.5.6 SyringeA microsyringe,10 L is needed for sampleintroduction.5.7 Pasteur Pipets.5.8 Vials,2 mL,with crimped septum caps.6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society where1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.04.0L on Gas Chromatography Methods.Current edition approved Oct.1,2013.Published October 2013.Originallyapproved in 1983.Last previous edition approved in 2009 as D4291 04(2009).DOI:10.1520/D4291-04R13.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 such specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water as definedby Type II of Specification D1193.6.3 Air and Hydrogen(WarningThe air supply may befrom a cylinder under high pressure.Hydrogen is an extremelyflammable gas under pressure.)6.4 Calibration MixturesA minimum of three mixtures ofwater and ethylene glycol are prepared to cover the range from5 to 200 mass ppm.Prepare one blend of approximately 2000mass ppm ethylene glycol in water to provide for accurateweighing;then,prepare dilutions of th