ASTM_D_4291_-_21.pdf

Designation:D429121Standard 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.Scope*1.1 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 from5 mass ppm to 200 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific warning statements,see Section 7.NOTE1A qualitative determination of glycol-base antifreeze isprovided in Test Methods D2982.Procedure A is sensitive to about100 ppm.1.3 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.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 ProductsD4175 Terminology Relating to Petroleum Products,LiquidFuels,and LubricantsE355 Practice for Gas Chromatography Terms and Relation-shipsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid Chromatography3.Terminology3.1 Definitions:3.1.1 This test method makes reference to common gaschromatographic procedures,terms,and relationships.Detaileddefinitions of these can be found in Practices E355 and E594,and Terminology D4175.4.Summary of Test Method4.1 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.5.Significance and Use5.1 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.6.Apparatus6.1 GasChromatographAnygaschromatographequipped with the following:6.1.1 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.6.1.2 Sample Inlet System,providing for on-column injec-tion and capable of operating continuously at a temperatureequivalent to the maximum column temperature employed.6.2 RecorderRecording potentiometer with a full-scaleresponse time of 2 s or less may be used.6.3 Columns1.2 m by 6.4 mm(4 ft by14in.)copper tubepacked with 5%by mass Carbowax 20-M liquid phase on30/60 mesh Chromosorb T solid support.As an alternative,afused silica capillary column,15 m long with a 0.53 mm IDand 2.0 micron film thickness of a bonded polyethylene glycolcan be used.6.4 IntegratorManual,mechanical,or electronic integra-tion is required to determine the peak area.However,best1This 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 Dec.1,2021.Published December 2021.Originallyapproved in 1983.Last previous edition approved in 2017 as D4291 04(2017).DOI:10.1520/D4291-21.2For 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.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1?precision and automated operation can be achieved withelectronic integration.6.5 CentrifugeRCF 600 minimum and centrifu