1、Designation: D 5273 92 (Reapproved 2002)An American National StandardStandard Guide forAnalysis of Propylene Concentrates1This standard is issued under the fixed designation D 5273; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he 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.1. Scope1.1 This guide lists the major grades of propylene concen-trates produced in North America. It includes possib
3、le compo-nents and test methods, both ASTM and other, either actuallyused, or believed to be in use, to test for these properties. Thisguide is not intended to be used or construed as a set ofspecifications for any grade of propylene concentrate.1.2 The values stated in SI units are to be regarded a
4、s thestandard.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.2
5、. Referenced Documents2.1 ASTM Standards:D 2163 Test Method for Analysis of Liquefied Petroleum(LP) Gases and Propene Concentrates by Gas Chromatog-raphy2D 2384 Test Methods for Traces of Volatile Chlorides inButane-Butene Mixtures2D 2504 Test Method for Noncondensable Gases in C2andLighter Hydrocar
6、bon Products by Gas Chromatography2D 2505 Test Method for Ethylene, Other Hydrocarbons, andCarbon Dioxide in High-Purity Ethylene by Gas Chroma-tography2D 2712 Test Method for Hydrocarbon Traces in PropyleneConcentrates by Gas Chromatography2D 3227 Test Method for Thiol Mercaptan Sulfur in Gaso-line
7、, Kerosine, Aviation Turbine, and Distillate Fuels(Potentiometric Method)2D 3246 Test Method for Sulfur in Petroleum Gas by Oxi-dative Microcoulometry3D 3700 Practice for Obtaining LPG Fluid Samples Using aFloating Piston Cylinder3D 4178 Practice for Calibrating Moisture Analyzers3D 4468 Test Method
8、 for Total Sulfur in Gaseous Fuels byHydrogenolysis and Rateometric Colorimetry4D 4629 Test Method for Trace Nitrogen in Liquid Petro-leum Hydrocarbons by Syringe/Inlet Oxidative Combus-tion and Chemiluminescence Detection3D 4864 Test Method for Determination of Traces of Metha-nol in Propylene Conc
9、entrates by Gas Chromatography33. Terminology3.1 Definitions:3.1.1 outaging, npractice of removing a portion of liquidcontents from a conventional sampling cylinder after filling toprovide expansion room.3.1.2 propylene concentrate, nhydrocarbon product con-taining more than 50 % propylene.3.1.2.1 D
10、iscussionGrades of propylene concentrateslisted in this guide are: polymer, 99.0 % minimum propylenecontent; chemical, 92.0 %; and refinery, 60 %.3.2 Symbols:3.2.1 AgDDC, nsilver diethyldithiocarbamate.3.2.2 GC, ngas chromatograph.3.2.3 GC-AED, ngas chromatography atomic emissiondetector.3.2.4 GC-EC
11、D, ngas chromatography electron capturedetector.3.2.5 GC-FPD, ngas chromatography flame photometricdetector.3.2.6 GC-PID, ngas chromatography photoionization de-tector.3.2.7 GC-SCD, ngas chromatography sulfur chemilumi-nescent detector.3.2.8 IC, nion chromatography.3.2.9 ICP-MS, ninductively coupled
12、 plasma-mass spec-trometry.3.2.10 LPG or LP gases, nliquified petroleum gas.4. Significance and Use4.1 This guide is intended to provide information on thelikely composition of propylene concentrates and on probableways to test them. Since there are currently no ASTM test1This guide is under the jur
13、isdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.D0.03on Propylene.Current edition approved Dec. 10, 2002. Published March 2003. Originallyapproved in 1992. Last previous edition approved in 1997 as D 5273 92(1997).2Annual Book
14、of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 05.02.4Annual Book of ASTM Standards, Vol 05.06.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.methods for determining all components of interest, this guideprovides i
15、nformation on other potentially available test meth-ods.4.2 Although this guide is not to be used for specifications,it can provide a starting point for parties to develop mutuallyagreed upon specifications which meet their respective require-ments. It can also be used as a starting point in finding
16、 suitabletest methods for determining various components of propylene.5. Sampling5.1 GeneralSample propylene concentrates are to beanalyzed for trace components by a technique that minimizesor eliminates losses of light components and concentration ofheavy ones. The sections below list some differen
17、t samplingmethods and principles. However, it is not the intent of thisguide to list procedures that are applicable to all samplingsituations. It is strongly recommended that samples be obtainedunder the supervision of a person with wide knowledge andexperience in sampling olefinic liquified petrole
18、um gases. Also,even though this guide does not address the location of asampling point in a line or vessel, the importance of the propersampling location cannot be over-emphasized.5.2 Floating Piston CylinderTest Method D 3700 meetsthe criterion of minimizing or eliminating loss of light com-pounds
19、and concentration of heavy ones. However, some labshave safety codes preventing use of rupture-disc piston con-tainers. Alternative procedures must be used in these labs.5.3 Conventional Outaging MethodThe widely used out-aging technique (that is, the practice of removing a portion ofthe fluid conte
20、nts from a conventional sampling cylinder afterfilling in order to provide expansion room) causes a loss oflight components into the vapor space. Subsequent handling torecapture these light ends in the liquid phases of the sample,such as repressurization of the cylinder contents with an inertgas, wi
21、ll not completely effect their recovery, especially thepermanent gases. However, the loss is not significant to someusers.5.4 Vaporization MethodsVaporization of the sample, ei-ther at the source or in the lab prior to analysis, can cause lossof heavier components, if present, and concentration of l
22、ighterones. Test Method D 2712 describes a low pressure vaporiza-tion sampling technique that is suitable to determine tracecompounds through butadiene.5.5 Reactive and Polar Components:5.5.1 Determination of reactive components, such as certainsulfur compounds and arsine, is generally believed to r
23、equirespecial sample containers, such as TFE-fluorocarbon linedcylinders, or containers that have been specially passivated.5.5.2 It is very difficult to obtain a valid sample to determinetraces of polar compounds, such as water and ammonia, in thelab. On-line analyzers, if available, or sorption of
24、 the analyte atthe sample source for subsequent lab analysis, are believed toyield the most accurate results.6. Composition and Test Methods6.1 Table 1 indicates possible composition ranges andASTM test methods for different grades of propylene concen-trates. Table 2 lists other test methods known o
25、r believed to bein use.TABLE 1 Possible Composition of Propylene ConcentratesComponent Polymer Grade Chemical Grade Refinery Grade Test MethodPropylene, % mass 99.0 + 92 to 99 60 to 90 D 2163Propane, % mass 0.1 to 1.0 1 to 8 10 to 35 D 2163Methane, mg/kg 2 to 100 10 to 1000 10 to 1000 See Table 2Eth
26、ane, mg/kg 2 to 200 10 to 2000 100 to 100 000 See Table 2Acetylene, mg/kg 1 to 10 2 to 100 . D 2712Ethylene, mg/kg 2 to 100 2 to 100 50 to 5000 D 2712Cyclopropane, mg/kg 1 to 10 2 to 500 2 to 500 See Table 2Methylacetylene, mg/kg 1 to 10 2 to 100 10 to 1000 D 2712Propadiene, mg/kg 1 to 10 2 to 100 1
27、0 to 1000 D 2712Butenes, mg/kg 1 to 20 2 to 200 100 to 10 000 D 2712Butanes, mg/kg 2 to 50 10 to 1000 100 to 15 000 See Table 21,3 butadiene, mg/kg 1 to 10 2 to 50 2 to 100 D 2712C5s, mg/kg 1 to 10 2 to 100 2 to 100 See Table 2C6s, and heavier, mg/kg 1 to 10 2 to 100 2 to 100 See Table 2Benzene, mg/
28、kg 0.1 to 10 0.1 to 10 . See Table 2H2, mg/kg 1 to 10 2 to 100 . See Table 2O2, mg/kg 1 to 10 2 to 100 . See Table 2CO, mg/kg 1 to 10 2 to 100 . See Table 2CO2, mg/kg 1 to 10 2 to 100 2 to 100 See Table 2N2, mg/kg 2 to 40 10 to 1000 . See Table 2H2S, mg/kg 0.1 to 10 1 to 20 . See Table 2COS, mg/kg 1
29、 to 10 1 to 10 1 to 50 See Table 2Total S, mg/kg 1 to 10 1 to 10 10 to 250 See Table 2Mercaptan, S, mg/kg 1 to 5 1 to 10 1 to 10 See Table 2Water, mg/kg 1 to 25 2 to 100 2 to 100 See Table 2Total nitrogen, mg/kg 1 to 5 1 to 10 . See Table 2Total chloride, mg/kg 1 to 5 1 to 10 . See Table 2Methanol,
30、mg/kg 1 to 5 1 to 10 . D 4864Other alcohols, mg/kg 1 to 5 1 to 10 . See Table 2Total oxygenates, mg/kg 1 to 5 1 to 10 . See Table 2Arsine, mg/kg 0.1 to 1 0.1 to 1 0.1 to 1 See Table 2Total hydrides, mg/kg 0.1 to 1 0.1 to 1 0.1 to 1 See Table 2D 5273 92 (2002)26.2 Listing of any given component in Ta
31、ble 1 does notmean that the component will be present in all, or even any,propylene products. Inclusion in the list is definitely not arecommendation that all propylene products should be testedfor the component.7. Keywords7.1 propylene; propylene product concentrations; propylenetest methodsASTM In
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33、ly their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand s
34、hould be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which 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 S
35、tandards, 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 6
36、10-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).TABLE 2 Propylene Test Methods (Non-ASTM)Components Possible Test MethodsMethane, ethane, cyclopropane, butanes, and C5s An adaptation of Test Method D 2712 is used by some labs. Others us
37、e a GC wide-bore capillary method.C6s and heavier GC wide-bore capillary or packed high temperature columns, or both, are used by some.Benzene Capillary or packed column GC methods.H2,N2,O2, CO An adaptation of Test Method D 2504 is used by some.CO2An adaptation of Test Method D 2505 is used by some
38、.Carbonyl sulfide A GC-FPD method is currently undergoing ASTM cooperative testing. Other methods used in the industryare GC-PID, GC-conductivity, GC-SCD, UOP-212, and GC in series with a Test Method D 4468-typeanalyzer.Hydrogen sulfide Same as listed above for COS, except there are no methods curre
39、ntly undergoing ASTM testing.Total sulfur Some labs use an adaptation of Test Method D 3246; others use Test Method D 4468 with an oxy-hydrogen pyrolyzer.Mercaptan sulfur Some methods used are: UOP 212; GC-FPD; caustic absorption/potentiometric titration analysis by TestMethod D 3227.Water Obtaining
40、 a valid sample for lab analysis is extremely difficult. Instead of a lab method, an ASTM studygroup developed in 1982 a standard practice for calibrating moisture analyzers, Practice D 4178.Several types of portable and on-line analyzers are available.Total nitrogen (bound) An adaptation of Test Me
41、thod D 4629 is used by some labs; others use microcoulometry.Total chlorides An adaptation of Test Methods D 2384 may be used by some labs; others use reductive microcoulometry.Arsine Some methods known to be in use are:AgDDC absorption/colorimetric finishAgDDC absorption/GFAAS finishdirect GC-ECD m
42、ethoddirect GC-PID methodTotal hydrides MDA scientific toxic gas analyzerAmmonia Some methods in use are:acid absorption/Nessler finishacid absorption/specific ion electrodeacid absorption/IC finishMDA tape methodOther oxygenates GC methods; GC-AED, colorimetric methodsOther alcohols GC methods, both capillary and packed column. Variation of Test Method D 4864D 5273 92 (2002)3
