ASTM_D_4367_-_02_2012.pdf

Designation:D436702(Reapproved 2012)Standard Test Method forBenzene in Hydrocarbon Solvents by Gas Chromatography1This standard is issued under the fixed designation D4367;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 by gaschromatography of benzene at levels from 0.01 to 1 volume%in hydrocarbon solvents.NOTE1For benzene levels lower than 0.01 volume%,use TestMethod D6229.1.2 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.3 For purposes of determining conformance of an ob-served or a calculated value using this test method to relevantspecifications,test result(s)shall be rounded off“to the nearestunit”in the last right-hand digit used in expressing thespecification limit,in accordance with the rounding-off methodof Practice E29.1.4 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.1.5 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.For specific hazard statements,seeSection 7.2.Referenced Documents2.1 ASTM Standards:2D6229 Test Method for Trace Benzene in HydrocarbonSolvents by Capillary Gas ChromatographyE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE300 Practice for Sampling Industrial Chemicals3.Summary of Test Method3.1 An internal standard,methyl ethyl ketone(MEK),isadded to the material and then introduced into a gas chromato-graph equipped with two columns connected in series.Thespecimen passes first through a column packed with thenonpolar phase,methyl silicone,which separates the compo-nents by boiling point.After octane has eluted,the flowthrough the nonpolar column is reversed,flushing out thecomponents heavier than octane.The octane and lightercomponents then pass through a column with the highly polarphase,1,2,3-tris(2-cyanoethoxy)propane,that separates thearomatic and nonaromatic compounds.The eluted componentsare detected by a conventional detector and recorded on a stripchart.The peak areas are measured and the concentration ofeach component is calculated by reference to the internalstandard.4.Significance and Use4.1 Benzene is classed as a toxic and carcinogenic material.Aknowledge of the concentration of this compound may be anaid in evaluating the possible health hazards to personshandling and using hydrocarbon solvents,but this test methodis not intended to evaluate such hazards.5.Apparatus5.1 ChromatographAny gas chromatographic instrumentthat has a backflush system and flame ionization detector andthat can be operated at the conditions given in Table 1.Thedetector-recorder combination must produce a 4-mm deflectionfor a 1-L specimen containing 0.05 volume%MEK whenoperated at maximum sensitivity.5.2 Columns,one 0.8-m(2.5-ft)length of 3.2-mm(18-in.)outside diameter stainless steel tubing and one 4.6-m(15-ft)length of 3.2-mm(18-in.)outsider diameter stainless steeltubing.5.3 Recorder,Strip ChartPotentiometer with a full-scaledeflection of 1 mV,a full-scale response time of 2 s or less,anda maximum noise level of 60.3%of full scale.5.4 Microsyringe,5-L capacity.5.5 Pipets,measuring 1 and 2 mL,graduated in 0.01 mL;5,10,and 20-mL capacity.5.6 Flasks,volumetric,25 and 100-mL capacity.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents,Plasticizers,and Chemical Intermediates.Current edition approved July 1,2012.Published September 2012.Originallyapproved in 1984.Last previous edition approved in 2007 as D4367 02(2007).DOI:10.1520/D4367-02R12.2For 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 5.7 Vibrator,electric.5.8 Vacuum Source.5.9 Evaporator,vacuum,rotary.5.10 Flask,boiling,round-bottom,short-neck,with 24/40 Tjoint,500-mL capacity.Suitable for use with the evaporator(see 5.9).5.11 Lamp,infrared.5.12 Burets,automatic,with integral reservoir,25-mL ca-pacity.NOTE2Suppliers of stationary phases and supports can be found inResearch Report RR:D01-1038,available from ASTM InternationalHeadquarters.6.Reagents and Materials6.1 Purity of Re