ASTM_D_4424_-_09_2014.pdf

Designation:D442409(Reapproved 2014)Standard Test Method forButylene Analysis by Gas Chromatography1This standard is issued under the fixed designation D4424;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 gas chromatographic analy-sis of commercial butylenes,butylene concentrates,andbutane-butylene mixtures.1.2 This test method does not cover high-purity butene-1 orhigh-purity isobutene streams,or both.However,it is possiblethat one or more columns listed in Appendix X3 may becapable of the separation necessary for high-purity analyses.1.3 This test method is designed to cover the componentslisted below at about 0.05%or greater.It is not intended fortrace hydrocarbon analysis.Components to be determined are:propane,propylene,isobutane,n-butane,butene-1,isobutene,trans-butene-2,cis-butene-2,1,3-butadiene,isopentane,n-pentane.1.4 The values stated in SI units are to be regarded as thestandard.The values stated in inch-pound units are for infor-mation only.1.5 This standard does not purport to address all of thesafety concerns associated with its use.It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.For specific warning statements,see5.3.1.2.Referenced Documents2.1 ASTM Standards:2E260 Practice for Packed Column Gas Chromatography3.Summary of Test Method3.1 The sample is separated in a gas chromatograph systemusing a packed chromatographic column with either helium orhydrogen as the carrier gas.The separated components of thesample are detected by either a thermal conductivity detector orby a flame ionization detector.Calibration data are obtained byusing either relative response factors or by using a standardcalibration blend.4.Significance and Use4.1 This test method could be used to determine butylenestream composition for custody transfer payments.It is alsocapable of providing data necessary to evaluate processingrequirements in an operating plant.5.Apparatus5.1 ChromatographAny chromatographic instrumenthaving either a thermal conductivity or flame ionizationdetector with an overall sensitivity sufficient to detect at least0.05%of each of the components listed in 1.3.5.2 DetectorEither a thermal conductivity or flame ion-ization detector may be used.5.3 Sample ValveEither a constant-volume gas samplingvalve or a liquid sampling valve may be used.If a gas samplingvalve is used,greater care must be taken to ensure that thevaporized butylenes that are injected into the chromatographare a true representation of the sample.5.3.1 If the liquid sample valve is used,the sample cylindermust be pressured up to at least 1100 kPa(160 psig)with aninert gas,such as nitrogen or helium.(WarningCompressedgas under high pressure.Gas reduces oxygen available forbreathing.)Also a valve must be installed in the purge linedownstream of the liquid sample valve to ensure the butylenessample in the sampling valve is entirely in the liquid phaseprior to injection into the column.(WarningExtremelyflammable liquefied gas under pressure.Vapor reduces oxygenavailable for breathing.)5.4 ColumnAny chromatographic column may be used,providing the components listed in the scope can be separatedsufficiently for the accurate determination of component con-centration.Resolution between peaks must afford a resolutionsuch that the depth of the valleys between peaks are no lessthan 50%of the peak height of the lesser component.A list ofsatisfactory columns is given in Appendix X3.5.5 RecorderA recorder with a full-scale response of 2 sor less and a maximum rate of noise of 60.3%of full scale.1This 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.Current edition approved May 1,2014.Published July 2014.Originally approvedin 1984.Last previous edition approved in 2009 as D4424 09.DOI:10.1520/D4424-09R14.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Preparation of Apparatus6.1 Set up the chromatograph in accordance with the manu-facturers recommendations.Install the analytical column andadjust the carrier gas flow and column temperature so that thecomponents will elute within the time desired for the analysis.7.Calibration7.1 A standard blend containing the components to beanalyzed may be either made or purchased fro