ASTM_D_2593_-_93_2014.pdf

Designation:D259393(Reapproved 2014)Standard Test Method forButadiene Purity and Hydrocarbon Impurities by GasChromatography1This standard is issued under the fixed designation D2593;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.Scope1.1 This test method covers the determination of butadiene-1,3 purity and impurities such as propane,propylene,isobutane,n-butane,butene-1,isobutylene,propadiene,trans-butene-2,cis-butene-2,butadiene-1,2,pentadiene-1,4,and,methyl,dimethyl,ethyl,and vinyl acetylene in polymerizationgrade butadiene by gas chromatography.Impurities includingbutadiene dimer,carbonyls,inhibitor,and residue are measuredby appropriate ASTM procedures and the results used tonormalize the component distribution obtained by chromatog-raphy.NOTE1Other impurities present in commercial butadiene must becalibrated and analyzed.Other impurities were not tested in the coopera-tive work on this test method.NOTE2This test method can be used to check for pentadiene-1,4 andother C5s instead of Test Method D1088.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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.For specificwarning statements,see 6.1 and 9.3.2.Referenced Documents2.1 ASTM Standards:2D1088 Method of Test for Boiling Point Range ofPolymerization-Grade Butadiene(Withdrawn 1983)32.2 Energy Institute Standards:4IP 194 Analysis of Butadiene-1,3 Polymerization Grade3.Summary of Test Method3.1 A representative sample is introduced into a gas-liquidpartition column.The butadiene and other components areseparated as they are transported through the column by aninert carrier gas.Their presence in the effluent is measured bya detector and recorded as a chromatogram.The chromatogramof the sample is interpreted by applying component attenuationand detector response factors to the peak areas or peak heightsand the relative concentration determined by relating indi-vidual peak response to total peak response.Impurities includ-ing butadiene dimer,carbonyls,inhibitor,and residue aremeasured by appropriate ASTM procedures and the resultsused to normalize the distribution obtained by gas chromatog-raphy.4.Significance and Use4.1 The trace hydrocarbon compounds listed can have aneffect in the commercial use of butadiene.This test method issuitable for use in process quality control and in settingspecifications.5.Apparatus5.1 ChromatographAny chromatograph having either athermal-conductivity or flame ionization detector can be usedprovided the system has sufficient sensitivity and stability toobtain a recorder deflection of at least 2 mm at signal-to-noiseratio of at least 5:1 for 0.01 weight%of impurity.5.2 ColumnAny column can be used that is capable ofresolving the components listed in 1.1 with the exception ofbutene-1 and isobutylene,which can be eluted together.Thecomponents should be resolved into distinct peaks such that theratio A/B will not be less than 0.5 where A is the depth of thevalley on either side of peak B and B is the height above thebaseline of the smaller of any two adjacent peaks.In the casewhere the small component peak is adjacent to a large one,it1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.D0.04 on C4 Hydrocarbons.This test method was adopted as a joint ASTM-IP Standard,IP 194,in 1972.Current edition approved May 1,2014.Published July 2014.Originally approvedin 1967.Last previous edition approved in 2009 as D259393(2009).DOI:10.1520/D2593-93R14.2For 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.4Obsolete.Contact Energy Institute,61 New Cavendish St.,London,WIG 7AR,U.K.,http:/www.energyinst.org.uk.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 can be necessary to construct a baseline of the small peaktangent to the curve as shown in Fig.1.5.2.1 A description of columns that meet the requirementsof this test method is tabulated in the Appendix.Persons usingother column materials must establish that the column givesresults that meet the precision requirements of Section 11.5.3 Sample Inlet SystemMeans shall be pr