1、Designation:D530392(Reapproved 2012)Standard Test Method forTrace Carbonyl Sulfide in Propylene by GasChromatography1This standard is issued under the fixed designation D5303;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year o
2、f 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 traces ofcarbonyl sulfide(COS)in propylene.It is applicable to COSconcentrat
3、ions from 0.5 to 4.0 mg/kg(parts per million bymass).See Note 1.NOTE1The lower limit of this test method is believed to be below 0.1mg/kg,depending on sample size and sensitivity of the instrumentationbeing used.However,the cooperative testing program was conducted inthe 0.5 to 4.0 range due to limi
4、tations in preparing commercial testmixtures.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 th
5、e user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.Specific hazardsstatements are given in Section 8.2.Referenced Documents2.1 ASTM Standards:2D3609 Practice for Calibration Techniques Using Perme-atio
6、n TubesD4468 Test Method for Total Sulfur in Gaseous Fuels byHydrogenolysis and Rateometric ColorimetryE840 Practice for Using Flame Photometric Detectors in GasChromatography3.Summary of Test Method3.1 A procedure is given for removing a sample from thesample cylinder,separating COS from propylene,
7、detectingCOS,calibrating the detector,quantitating COS content in thesample,and assaying the gas standard.General comments andrecommended techniques are given.3.2 Arelatively large volume of sample is injected into a gaschromatograph having a single packed column,operated iso-thermally at 10 to 50C,
8、that separates COS from propylene.COS is detected with a flame photometric detector.3.3 Calibration data,based on peak areas,are obtained usinga known gas standard blend of COS in the range expected forthe sample.The COS peak area in the sample is measured andthe concentration of COS calculated.3.4
9、The COS gas standard blend is assayed prior to use forcalibration.4.Significance and Use4.1 In processes producing propylene,COS usually remainswith the C3hydrocarbons and must be removed,since it affectsproduct quality.COS acts as a poison to commercial polym-erization catalysts,resulting in deacti
10、vation and costly processdowntime.4.2 Accurate gas chromatographic determination of traceCOS in propylene involves unique analytical problems becauseof the chemical nature of COS and idiosyncracies of trace levelanalyses.These problems result from the reactive and absorp-tive nature of COS,the low c
11、oncentration levels beingmeasured,the type of detector needed,and the interferencesfrom the propylene sample matrix.This test method addressesthese analytical problems and ways to properly handle them toassure accurate and precise analyses.4.3 This test method provides a basis for agreement betweent
12、wo laboratories when the determination of trace COS inpropylene is important.The test method permits severalcalibration techniques.For best agreement between two labs,itis recommended that they use the same calibration technique.5.Interferences5.1 Hydrogen sulfide(H2S)or sulfur dioxide(SO2)can bepre
13、sent in the propylene and must be separated from COS.(SeeNote 2.)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.D0.03 on Propylene.Current edition approved Dec.1,2012.Published Dec
14、ember 2012.Originallyapproved in 1992.Last previous edition approved in 2007 as D530392(2007).DOI:10.1520/D5303-92R12.2For 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
15、 standards Document Summary page onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 NOTE2H2S and SO2are separated from COS with the CarbopackBHT 100 columns or with the Chromosil 300 column.6.Apparatus6.1 Gas Chromatograph
16、Any gas chromatograph(GC)equipped with a flame photometric detector/electrometer sys-tem(FPD),as described in 6.2,may be used.A GC/FPDequipped with an output signal linearizer is also permitted.6.2 Detector System,flame photometric detector,eithersingle or dual burner design.Noise level must be no more thanone recorder chart division(see 6.5).The signal for COS mustbe at least twice the noise level at the 0.1 mg/kg level.Adiscussion of this detector is presented in Practice E840.Theelectrometer
