ASTM_D_3606_-_10.pdf

Designation:D360610Standard Test Method forDetermination of Benzene and Toluene in Finished Motorand Aviation Gasoline by Gas Chromatography1This standard is issued under the fixed designation D3606;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 benzeneand toluene in finished motor and aviation gasolines by gaschromatography.1.2 Benzene can be determined between the levels of 0.1and 5 volume%and toluene can be determined between thelevels of 2 and 20 volume%.1.3 The precision for this test method was determined usingconventional gasoline as well as gasolines containing oxygen-ates(ethers such as methyl tert-butyl ether,ethyl tert-butylether and tert-amyl methyl ether).1.4 Methanol may cause interference.Appendix X1 pro-vides an option for modifying the test method for analyzingsamples containing ethanol.1.5 The values stated in SI units are to be regarded asstandard.The values given in parentheses are for informationonly.1.6 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.2.Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsE694 Specification for Laboratory Glass Volumetric Appa-ratusE969 Specification for Glass Volumetric(Transfer)PipetsE1044 Specification for Glass Serological Pipets(GeneralPurpose and Kahn)E1293 Specification for Glass Measuring Pipets3.Summary of Test Method3.1 An internal standard,methyl ethyl ketone(MEK),isadded to the sample which is then introduced into a gaschromatograph equipped with two columns connected inseries.The sample passes first through a column packed with anonpolar phase such as dimethylpolysiloxane(8.1.1)whichseparates the components according to boiling point.Afteroctane has eluted,the flow through the nonpolar column isreversed,flushing out the components heavier than octane.Theoctane and lighter components then pass through a columnpacked with a highly polar phase such as 1,2,3-tris(2-cyanoethoxy)propane(8.1.2)which separates the aromatic andnonaromatic compounds.The eluted components are detectedby a thermal conductivity detector.The detector response isrecorded,the peak areas are measured,and the concentration ofeach component is calculated with reference to the internalstandard.4.Significance and Use4.1 Benzene is classed as a toxic material.A knowledge ofthe concentration of this compound can be an aid in evaluatingthe possible health hazard to persons handling and using thegasoline.This test method is not intended to evaluate suchhazards.5.Apparatus5.1 ChromatographAny chromatographic instrument thathas a backflush system and thermal conductivity detector,andthat can be operated at the conditions given in Table 1,can beemployed.Two backflush systems are shown.Fig.1 is apressure system and Fig.2 is a switching valve system.Eitherone can be used.5.2 Columns:5.2.1 Column AOne 0.8 m(2.5 ft)by 3.2 mm(18in.)outside diameter stainless steel column packed with 10 mass%dimethylpolysiloxane(for example,OV-101)on ChromosorbW,60 to 80 mesh.5.2.2 Column BOne 4.6 m(15 ft)by 3.2 mm outsidediameter stainless steel column packed with 20 mass%TCEPon Chromosorb P,80 to 100 mesh.1This 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.1,2010.Published November 2010.Originallyapproved in 1977.Last previous edition approved in 2007 as D360607.DOI:10.1520/D3606-10.2For 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 States1 5.3 Recordera strip chart recorder.An electronic integrat-ing device or a computer capable of graphical presentation ofthe chromatogram.The electronic integrating device or com-puter must be capable of measuring 0.1 volume%MEK withsatisfactory signal-to-noise.If a strip chart recorder is to beused,a 0 to 1 mV range recording potentiometer with aresponse time of 2 s or less and a maximum noise level of 60.3%of full scale is recommended.The detector strip chartrecorder combination must produce a 4 mm deflection for a 2L sample containing 0.1 volume%MEK when operated atmaxim