ASTM_E_1863_-_07.pdf

Designation:E186307Standard Test Method forAnalysis of Acrylonitrile by Gas Chromatography1This standard is issued under the fixed designation E1863;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 the impu-rities in,and the purity of,acrylonitrile by flame ionizationdetector gas chromatography.It is applicable to acrylonitrile inthe range of 99 to 100%purity.1.2 The values stated in SI units are to be regarded asstandard.The values given in parentheses are for informationonly.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 and health practices and determine the applica-bility of regulatory limitations prior to use.Specific hazardstatements are given in Sections 6 and 7.1.4 Review the current MSDS for detailed informationconcerning toxicity,first aid procedures,and safety precau-tions.2.Referenced Documents2.1 ASTM Standards:2E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E1178 Test Methods for Analysis of Acrylonitrile3.Summary of Test Method3.1 In this test method,a representative sample of acrylo-nitrile is introduced in a gas chromatograph equipped with aflame ionization detector and a capillary column where specificimpurities are separated from the acrylonitrile.The chromato-graphic area for each impurity is compared to the area of theinternal standard,toluene or other suitable known,added to thesample.From response factors of these impurities relative tothat of the internal standard and the amount of the standardadded,the concentration of the impurities are calculated.Otherimpurities,such as water,are obtained by use of Test MethodsE1178.The acrylonitrile content is obtained by subtracting thetotal amount of all impurities from 100.0.4.Significance and Use4.1 This test method is designed to obtain acrylonitrilepurity on the basis of impurities normally present in acryloni-trile and may be useful for final product inspection and processcontrol.4.2 This test method will measure the following impurities:acetone,acrolein,acetonitrile,and acetaldehyde.It also willallow calibration of other impurities including benzene,methacrylonitrile,oxazole,propionitrile,cis-crotononitrile,trans-crotononitrile,and others where specific impurity stan-dards are available.5.Apparatus5.1 Capillary Gas ChromatographAny gas chromato-graph equipped with a flame ionization detector and a splitinjection system for use with capillary columns that can beoperated at the conditions given in Table 1.5.2 ColumnThe column,such as Supelcowax 10,4mustgive satisfactory resolution and proper peak shapes for thecomponents listed in Fig.1.5.3 Recorder/IntegratorElectronic integration is recom-mended for this analysis.5.4 Syringe,10 L capacity.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 E15 onIndustrial and Specialty Chemicalsand is the direct responsibility of SubcommitteeE15.02 on Product Standards.Current edition approved April 1,2007.Published May 2007.Originallyapproved in 1997.Last previous edition approved in 2002 as E1863 97(2002).DOI:10.1520/E1863-07.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.4A Supelcowax 10 fused silica capillary column(60 m by 0.32 mm ID by 1 mfilm thickness),has been found to be suitable,but similar polar wax columns fromother vendors may be used after shown to be suitable.*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 such specifications are available.5Other 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 Carrier Gas,helium minimum purity 99.995 mol%.6.3 Hydrogen,high purity.6.4 Air,hydrogen free,high purity.5Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Ana