1、Designation: D5273 92 (Reapproved 2012)Standard Guide forAnalysis of Propylene Concentrates1This standard is issued under the fixed designation D5273; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A num
2、ber in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 includes possiblecomponents and test m
3、ethods, 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 regarded asstandard. No other unit
4、s 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 determine the applica-bility of regul
5、atory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D2163 Test Method for Analysis of Liquefied Petroleum(LP) Gases and Propene Concentrates by Gas Chromatog-raphyD2384 Test Methods for Traces of Volatile Chlorides inButane-Butene MixturesD2504 Test Method for Noncondensable Ga
6、ses in C2andLighter Hydrocarbon Products by Gas ChromatographyD2505 Test Method for Ethylene, Other Hydrocarbons, andCarbon Dioxide in High-Purity Ethylene by Gas Chroma-tographyD2712 Test Method for Hydrocarbon Traces in PropyleneConcentrates by Gas ChromatographyD3227 Test Method for (Thiol Mercap
7、tan) Sulfur inGasoline, Kerosine, Aviation Turbine, and Distillate Fuels(Potentiometric Method)D3246 Test Method for Sulfur in Petroleum Gas by Oxida-tive MicrocoulometryD3700 Practice for Obtaining LPG Samples Using a Float-ing Piston CylinderD4178 Practice for Calibrating Moisture AnalyzersD4468 T
8、est Method for Total Sulfur in Gaseous Fuels byHydrogenolysis and Rateometric ColorimetryD4629 Test Method for Trace Nitrogen in Liquid PetroleumHydrocarbons by Syringe/Inlet Oxidative Combustion andChemiluminescence DetectionD4864 Test Method for Determination of Traces of Metha-nol in Propylene Co
9、ncentrates 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 concentrate, nhydrocarbon product con-taining more than 50 % propylene.3.1.2.1
10、DiscussionGrades of propylene concentrates listedin this guide are: polymer, 99.0 % minimum propylene content;chemical, 92.0 %; and refinery, 60 %.3.2 Abbreviations:3.2.1 AgDDC, nsilver diethyldithiocarbamate.3.2.2 GC, ngas chromatograph.3.2.3 GC-AED, ngas chromatography atomic emissiondetector.3.2.
11、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.3.2.7 GC-SCD, ngas chromatography sulfur chemilumi-nescent detector.3.2.8 IC, nion chromatography.3.2.9 ICP-MS, ninductively
12、coupled plasma-mass spec-trometry.3.2.10 LPG or LP gases, nliquefied petroleum gas.1This guide is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.D0.03on Propylene.Current edition approved Dec. 1, 2012. Published D
13、ecember 2012. Originallyapproved in 1992. Last previous edition approved in 2007 as D527392(2007).DOI: 10.1520/D5273-92R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, re
14、fer 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 States14. Significance and Use4.1 This guide is intended to provide information on thelikely composition of propylene concentrates
15、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 specifications,it can provide a starting point for par
16、ties 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 propylene concentrates are to be ana-lyzed for trace comp
17、onents by a technique that minimizes oreliminates 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 applicable to all samplingsituations. It is stron
18、gly 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, the importance of the propersampling location
19、cannot be overemphasized.5.2 Floating Piston CylinderTest Method D3700 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 con-tainers. Alternative procedures must be used
20、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 oflight components into the vapor space. Subsequent
21、 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 to someusers.5.4 Vaporization MethodsVaporizati
22、on 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 D2712 describes a low pressure vaporiza-tion sampling technique that is suitable to determine tracecompounds through butadiene.5.5 R
23、eactive 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 specially passivated.5.5.2 It is very difficult to obt
24、ain 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.6. Composition and Test Methods6.1 Table 1 indica
25、tes 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 present in all, or even any,propylene products. I
26、nclusion in the list is definitely not arecommendation that all propylene products should be testedfor the component.7. Keywords7.1 propylene; propylene product concentrations; propylenetest methodsD5273 92 (2012)2TABLE 1 Possible Composition of Propylene ConcentratesComponent Polymer Grade Chemical
27、 Grade Refinery Grade Test MethodPropylene, % mass 99.0 + 92 to 99 60 to 90 D2163Propane, % mass 0.1 to 1.0 1 to 8 10 to 35 D2163Methane, 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 2Acetylene, mg/kg 1 to 10 2 to 100 . D2712Ethylene, mg/
28、kg 2 to 100 2 to 100 50 to 5000 D2712Cyclopropane, 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 D2712Propadiene, mg/kg 1 to 10 2 to 100 10 to 1000 D2712Butenes, mg/kg 1 to 20 2 to 200 100 to 10 000 D2712Butanes, mg/kg 2 to 50 10 to 1000 100 to 15 000
29、See Table 21,3 butadiene, mg/kg 1 to 10 2 to 50 2 to 100 D2712C5s, 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 100 . See Table 2O2, mg/kg 1 to 10 2 to 100 . See Table 2C
30、O, 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 to 10 10 to 250 See Table 2Mercaptan, S, mg/kg 1 to 5 1 to
31、 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 . D4864Other alcohols, mg/kg 1 to 5 1 to 10 . See Table 2Total oxygenates, mg/kg 1 to 5 1 to 10
32、. 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 C5s An adaptation of Test Method D2712 is used by some lab
33、s. 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 D2504 is used by some.CO2An adaptation of Test Method D2505 is us
34、ed 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 D4468-type ana-lyzer.Hydrogen sulfide Same as listed above for COS, except there are no me
35、thods currently undergoing ASTM testing.Total sulfur Some labs use an adaptation of Test Method D3246; others use Test Method D4468 with an oxy-hydrogenpyrolyzer.Mercaptan sulfur Some methods used are: UOP 212; GC-FPD; caustic absorption/potentiometric titration analysis by TestMethod D3227.Water Ob
36、taining 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 D4178. Severaltypes of portable and online analyzers are available.Total nitrogen (bound) An adaptation of Te
37、st Method D4629 is used by some labs; others use microcoulometry.Total chlorides An adaptation of Test Methods D2384 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-EC
38、D 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 GC methods; GC-AED, colorimetric methodsOther alcohols GC methods,
39、both capillary and packed column. Variation of Test Method D4864D5273 92 (2012)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the val
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