1、Designation: D 4424 90 (Reapproved 2001)e1An American National StandardStandard Test Method forButylene Analysis by Gas Chromatography1This standard is issued under the fixed designation D 4424; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEWarning notes were placed in the text editorially in January 2001.1. Scope1.1 This test method cove
3、rs 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 X1 may becapable of t
4、he 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-buten
5、e-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 respo
6、nsibilityof 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:E 260 Practice for Packed Column Gas Chromatography23.
7、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. Calibr
8、ation 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 processi
9、ngrequirements 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 the scope.5.2 DetectorEither a thermal
10、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 tru
11、e 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 i
12、nstalled 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 c
13、hromatographic 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 h
14、eight of the lesser component. A list ofsatisfactory columns is given in Appendix X1.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.D0.04 on C4 Hydrocarbons.Current edition approved Jan. 10, 20
15、01. Published November 1990. Originallypublished as D 4424 84. Last previous edition D 4424 84.2Annual Book of ASTM Standards, Vol 03.06.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.5 RecorderA recorder with a full-scale respons
16、e of 2 sor less and a maximum rate of noise of 60.3 % of full scale.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 with
17、in the time desired for the analysis.7. Calibration7.1 A standard blend containing the components to beanalyzed may be either made or purchased from a commercialsource. Inject the calibration blend under identical conditionsas will be used for the samples. Record the chromatogram andcalculate the fa
18、ctors to be used for analysis by using the peakareas as measured by either manual, mechanical, or electronicmeans.7.2 Relative response factors may be used if they areavailable.NOTE 1Practice E 260 procedures may be helpful to those using thistest method.8. Procedure8.1 If a vapor sample is to be in
19、jected using a gas samplevalve, a representative portion of the liquid butylenes must betaken and vaporized into a suitable container. As a suggestion,a small, 5 or 10 mL aliquot of liquid butylenes under pressurein a valved, 5 or 10-mL sample cylinder can be expanded intoa larger container as a vap
20、or. Then this resultant vapor wouldbe injected into the chromatograph.8.2 If a liquid sampling valve is used, pressure the samplecylinder to at least 1100 kPa (160 psig) with either helium ornitrogen.8.3 Take the sample after the proper preparation has beendone and inject it into the gas chromatogra
21、phic column usingthe appropriate sampling valve. Record the chromatogramusing as low an attenuation as possible to insure all peaks areon scale and as large as possible.8.4 Measure the peak areas after all peaks have eluted.Measurement may be automatic by using either mechanical orelectronic integra
22、tors or computers.9. Calculations9.1 Calculate the concentration of each component using thefollowing equation:Ci5 Ai3 Fi3 100/(Ai3 Fi! (1)where:Ci= concentration of the i-th component,Ai= peak area of the i-th component,Fi= calibration factor for the i-th component, and(Ai3 Fi= sum of all products
23、of peak areas timescalibration factors.10. Precision and Bias10.1 The precision section shall be developed after coop-erative interlaboratory study program.10.2 BiasSince there is no accepted reference materialsuitable for determining bias for the procedure in this testmethod, bias cannot be determi
24、ned.11. Keywords11.1 butylene; c1-c4hydrocarbons; gas chromatographyAPPENDIX(Nonmandatory Information)X1. SUGGESTED COLUMNSX1.1 Column A.Column 2.1 m by 3.2-mm (7 ft by18-in.) outside diametersteel packed with 20 % diisopropyl phthalate on 60/80 meshNAW Chromosorb P; followed by 15.2 m by 3.2-mm (50
25、 ft by18-in.) outside diameter stainless steel packed with 20 %dimethyl sulfolane on 60/80 mesh NAW Chromosorb P.Carrier Gas, helium at 30 cm3/min.Column Oven Temperature, ambient.Sample Valve, 1-L liquid valve.X1.2 Column B.Column 12.2 m by 3.2-mm (40 ft by18-in.) outside diameterstainless steel pa
26、cked with 16 % sebaconitrile on 80/100 meshAW Chromosorb P; followed by 1.8 m by 3.2-mm (6 ft by18-in.) outside diameter stainless steel packed with 80/100mesh OPN/Porasil C Durapak; followed by 1.2 m by 3.2-mm(4 ft by18-in.) outside diameter stainless steel packed with80/100 mesh phenylisocyanate o
27、n Porasil C Durapak.Carrier Gas, hydrogen at 30 cm3/min.Column Oven Temperature, 40C.Sample Valve, 1-L liquid valve.D 4424 90 (2001)e12ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this stand
28、ard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andi
29、f not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, wh
30、ich you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 4424 90 (2001)e13
