1、Designation:E186318Standard 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 i
2、n 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 the impu-rities in,and the purity of,acrylonitrile by flame ionizationdetector gas chromatography.It i
3、s 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 therespon
4、sibility 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.Specific hazard statements are given in Sections 6 and 7.1.4 Review the current MSDS for detailed informationconcerning to
5、xicity,first aid procedures,and safety precau-tions.1.5 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 b
6、y the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.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Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E1178 Test Methods for Analysis of Acrylonitril
7、e(With-drawn 2016)33.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 fo
8、r 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
9、,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
10、 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,
11、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
12、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.1This test method is under the jurisdiction of ASTM Commit
13、tee D20 on Plasticsand is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materi-als.Current edition approved Oct.1,2018.Published October 2018.Originallyapproved in 1997.Last previous edition approved in 2007 as E1863 07,which waswithdrawn January 2016 and reinstated in October 20
14、18.DOI:10.1520/E1863-18.2For 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 histori
15、cal 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.Copyright ASTM International,100 Barr Harbor Drive,PO
16、 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 6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is
