ASTM D5273-1992(2007) Standard Guide for Analysis of Propylene Concentrates《丙烯浓聚物分析的标准指南》.pdf

1、Designation: D 5273 92 (Reapproved 2007)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 covers a list of the major grades of propyleneconcentrates produced in North America. It includ

3、es possiblecomponents and test methods, both ASTM and other, eitheractually used, or believed to be in use, to test for theseproperties. This guide is not intended to be used or construedas a set of specifications for any grade of propylene concen-trate.1.2 The values stated in SI units are to be re

4、garded 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 deter

5、mine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 2163 Test Method for Determination of Hydrocarbons inLiquefied Petroleum (LP) Gases and Propane/PropeneMixtures by Gas ChromatographyD 2384 Test Methods for Traces of Volatile Chlorides inButa

6、ne-Butene MixturesD 2504 Test Method for Noncondensable Gases in C2andLighter Hydrocarbon Products by Gas ChromatographyD 2505 Test Method for Ethylene, Other Hydrocarbons, andCarbon Dioxide in High-Purity Ethylene by Gas Chroma-tographyD 2712 Test Method for Hydrocarbon Traces in PropyleneConcentra

7、tes by Gas ChromatographyD 3227 Test Method for (Thiol Mercaptan) Sulfur in Gaso-line, Kerosine, Aviation Turbine, and Distillate Fuels(Potentiometric Method)D 3246 Test Method for Sulfur in Petroleum Gas by Oxi-dative MicrocoulometryD 3700 Practice for Obtaining LPG Samples Using a Float-ing Piston

8、 CylinderD 4178 Practice for Calibrating Moisture AnalyzersD 4468 Test Method for Total Sulfur in Gaseous Fuels byHydrogenolysis and Rateometric ColorimetryD 4629 Test Method for Trace Nitrogen in Liquid Petro-leum Hydrocarbons by Syringe/Inlet Oxidative Combus-tion and Chemiluminescence DetectionD

9、4864 Test Method for Determination of Traces of Metha-nol in Propylene Concentrates by Gas Chromatography3. 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 concen

10、trate, nhydrocarbon product con-taining more than 50 % propylene.3.1.2.1 DiscussionGrades of propylene concentrateslisted in this guide are: polymer, 99.0 % minimum propylenecontent; chemical, 92.0 %; and refinery, 60 %.3.2 Abbreviations:3.2.1 AgDDC, nsilver diethyldithiocarbamate.3.2.2 GC, ngas chr

11、omatograph.3.2.3 GC-AED, ngas chromatography atomic emissiondetector.3.2.4 GC-ECD, ngas chromatography electron capturedetector.3.2.5 GC-FPD, ngas chromatography flame photometricdetector.3.2.6 GC-PID, ngas chromatography photoionization de-tector.1This guide is under the jurisdiction of ASTM Commit

12、tee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.D0.03on Propylene.Current edition approved Nov. 1, 2007. Published January 2008. Originallyapproved in 1992. Last previous edition approved in 2002 as D 527392(2002).2For referenced ASTM standards, visit

13、 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-295

14、9, United States.3.2.7 GC-SCD, ngas chromatography sulfur chemilumi-nescent detector.3.2.8 IC, nion chromatography.3.2.9 ICP-MS, ninductively coupled plasma-mass spec-trometry.3.2.10 LPG or LP gases, nliquefied petroleum gas.4. Significance and Use4.1 This guide is intended to provide information on

15、 thelikely composition of propylene concentrates and on probableways to test them. Since there are currently no ASTM testmethods for determining all components of interest, this guideprovides information on other potentially available test meth-ods.4.2 Although this guide is not to be used for speci

16、fications,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 suitabletest methods for determining various components of propylene.5. Sampling5.1 GeneralSample propylen

17、e 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 different samplingmethods and principles. However, it is not the intent of thisguide to list procedures that are ap

18、plicable to all samplingsituations. It is strongly recommended that samples be obtainedunder the supervision of a person with wide knowledge andexperience in sampling olefinic liquefied petroleum gases.Also, even though this guide does not address the location of asampling point in a line or vessel,

19、 the importance of the propersampling location cannot be overemphasized.5.2 Floating Piston CylinderTest Method D 3700 meetsthe criterion of minimizing or eliminating loss of light com-pounds and concentration of heavy ones. However, some labshave safety codes preventing use of rupture-disc piston c

20、on-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 contents from a conventional sampling cylinder afterfilling in order to provide expansion room) causes a loss ofl

21、ight 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, will not completely effect their recovery, especially thepermanent gases. However, the loss is not significant

22、 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 lighterones. Test Method D 2712 describes a low pressure vaporiza-tion sampling technique that is suitable to

23、 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 requirespecial sample containers, such as TFE-fluorocarbon linedcylinders, or containers that have been speci

24、ally 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. Online analyzers, if available, or sorption of the analyte atthe sample source for subsequent lab analysis, are believed toyield the most accurate results.

25、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 or believed to bein use.6.2 Listing of any given component in Table 1 does notmean that the component will be

26、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 methodsD 5273 92 (2007)2TABLE 1 Possible Composition of Prop

27、ylene 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 2Ethane, mg/kg 2 to 200 10 to 2000 100 to 100 000 See Table 2Ac

28、etylene, 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 10 to 1000 D 2712Butenes, mg/kg 1 to 20 2 to 200 100 to 10 0

29、00 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/kg 0.1 to 10 0.1 to 10 . See Table 2H2, mg/kg 1 to 10 2 to

30、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 to 10 1 to 10 1 to 50 See Table 2Total S, mg/kg 1 to 10 1

31、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, mg/kg 1 to 5 1 to 10 . D 4864Other alcohols, mg/kg 1 to 5 1

32、 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 2TABLE 2 Propylene Test Methods (Non-ASTM)Components Possible Test MethodsMethane, ethane, cyclopropane, butanes, and

33、 C5s An adaptation of Test Method D 2712 is used by some labs. Others use 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 250

34、4 is used by some.CO2An adaptation of Test Method D 2505 is used by some.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

35、 sulfide Same as listed above for COS, except there are no methods currently 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 absorptio

36、n/potentiometric titration analysis by TestMethod D 3227.Water Obtaining 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. Severaltypes of portable and online

37、analyzers are available.Total nitrogen (bound) An adaptation of Test Method 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 abs

38、orption/colorimetric finishAgDDC absorption/GFAAS finishdirect GC-ECD methoddirect 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

39、 GC methods; GC-AED, colorimetric methodsOther alcohols GC methods, both capillary and packed column. Variation of Test Method D 4864D 5273 92 (2007)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. User

40、s of this standard 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

41、five years andif 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 technica

42、l 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 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 5273 92 (2007)4