1、Designation: D5273 18Standard 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 number in parentheses
2、 indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This guide covers a list of the major grades of propyleneconcentrates produced in North America. It includes possiblecomponents and test methods, both ASTM
3、 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 units of measurement
4、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, health, and environmental practices and deter-mine the applicability of regula
5、tory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Org
6、anization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D2163 Test Method for Determination of Hydrocarbons inLiquefied Petroleum (LP) Gases and Propane/PropeneMixtures by Gas ChromatographyD2384 Test Methods for Traces of Volatile Chlorides inButane-Butene Mi
7、xturesD2504 Test Method for Noncondensable Gases 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 Determination of Hydrocarbon Im-purities in High Purity
8、 Propylene by Gas ChromatographyD3227 Test Method for (Thiol Mercaptan) 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 Pist
9、on CylinderD4178 Practice for Calibrating Moisture AnalyzersD4468 Test Method for Total Sulfur in Gaseous Fuels byHydrogenolysis and Rateometric ColorimetryD4629 Test Method for Trace Nitrogen in Liquid Hydrocar-bons by Syringe/Inlet Oxidative Combustion and Chemi-luminescence DetectionD4864 Test Me
10、thod for Determination of Traces of Metha-nol in Propylene Concentrates by Gas Chromatography(Withdrawn 2016)3D5454 Test Method for Water Vapor Content of GaseousFuels Using Electronic Moisture AnalyzersD6667 Test Method for Determination of Total VolatileSulfur in Gaseous Hydrocarbons and Liquefied
11、 PetroleumGases by Ultraviolet FluorescenceD6729 Test Method for Determination of Individual Com-ponents in Spark Ignition Engine Fuels by 100 MetreCapillary High Resolution Gas ChromatographyD7423 Test Method for Determination of Oxygenates in C2,C3, C4, and C5 Hydrocarbon Matrices by Gas Chroma-to
12、graphy and Flame Ionization DetectionD7994 Test Method for Total Fluorine, Chlorine, and Sulfurin Liquid Petroleum Gas (LPG) by Oxidative Pyrohydro-lytic Combustion Followed by Ion Chromatography De-tection (Combustion Ion Chromatography-CIC)D8098 Test Method for Permanent Gases in C2and C3Hydrocarb
13、on Products by Gas Chromatography and PulseDischarge Helium Ionization Detector1This guide is under the jurisdiction of ASTM Committee D02 on PetroleumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.D0.03 on Propylene.Current edition approved July 1, 2018
14、. Published August 2018. Originallyapproved in 1992. Last previous edition approved in 2012 as D5273 92 (2012).DOI: 10.1520/D5273-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume infor
15、mation, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoho
16、cken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organi
17、zation Technical Barriers to Trade (TBT) Committee.12.2 UOP Standard:4UOP 212 Hydrogen Sulfide, Mercaptan Sulfur, and Carbo-nyl Sulfide in Hydrocarbon Gases by PotentiometricTitrationUOP 603 Trace CO and CO2in Hydrogen and LightGaseous Hydrocarbons by GC3. Terminology3.1 Definitions:3.1.1 outaging,
18、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 DiscussionGrades of propylene concentrates listedin this guide are: polymer, 9
19、9.0 % 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.3.2.4 GC-ECD, ngas chromatography electron capturedetector.3.2.5 GC-FPD, ngas chro
20、matography 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 plasma-mass spec-trometry.3.2.10 LPG or LP gases, nliquefied petroleum
21、 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 testmethods for determining all components of interest, this guideprovides information on other potenti
22、ally 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 suitabletest methods for d
23、etermining various components of propylene.5. Sampling5.1 GeneralSample propylene concentrates are to be ana-lyzed for trace components by a technique that minimizes oreliminates losses of light components and concentration ofheavy ones. The sections below list some different samplingmethods and pri
24、nciples. 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 liquefied petroleum gases.Also, even thoug
25、h this guide does not address the location of asampling point in a line or vessel, the importance of the propersampling location 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
26、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 contents from a conventional sam
27、pling 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, will not completely effect th
28、eir 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 lighterones. Test Method D27
29、12 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 requirespecial sample contain
30、ers, such as glass-lined, TFE-fluorocarbon-lined cylinders, or other containers that have beenspecially passivated.5.5.2 It is very difficult to obtain a valid sample to determinetraces of polar compounds, such as oxygen, water, andammonia, in the lab. Online analyzers, if available, or sorptionof t
31、he analyte at the sample source for subsequent lab analysis,are believed to yield 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 or
32、 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. Inclusion in the list is definitely not arecommendation that all propylene products should be testedfor the component.7. Keywords7.1 propylene;
33、propylene product concentrations; propylenetest methods4Available from ASTM International at www.astm.org, or contact ASTMCustomer Service at serviceastm.org.D5273 182TABLE 1 Possible Composition of Propylene ConcentratesComponent Polymer Grade Chemical Grade Refinery Grade Test MethodPropylene, % m
34、ass 99.0 + 92 to 99 60 to 90 D2163 or D2712Propane, % mass 0.1 to 1.0 1 to 8 10 to 35 D2163 or D2712Methane, mg/kg 2 to 100 10 to 1000 10 to 1000 D2163 or D2712Ethane, mg/kg 2 to 200 10 to 2000 100 to 100 000 D2163 or D2712Acetylene, mg/kg 1 to 10 2 to 100 . D2163 or D2712Ethylene, mg/kg 2 to 100 2
35、to 100 50 to 5000 D2163 or D2712Cyclopropane, mg/kg 1 to 10 2 to 500 2 to 500 D2163 or D2712Methylacetylene, mg/kg 1 to 10 2 to 100 10 to 1000 D2163 or D2712Propadiene, mg/kg 1 to 10 2 to 100 10 to 1000 D2163 or D2712Butenes, mg/kg 1 to 20 2 to 200 100 to 10 000 D2163 or D2712Butanes, mg/kg 2 to 50
36、10 to 1000 100 to 15 000 D2163 or D27121,3 butadiene, mg/kg 1 to 10 2 to 50 2 to 100 D2163 or D2712C5s, mg/kg 1 to 10 2 to 100 2 to 100 D2163 or D2712C6s, and heavier, mg/kg 1 to 10 2 to 100 2 to 100 D2163 or D2712Benzene, mg/kg 0.1 to 10 0.1 to 10 . D6729H2, mg/kg 1 to 10 2 to 100 . See Table 2O2,
37、mg/kg 1 to 10 2 to 100 . See Table 2CO, mg/kg 1 to 10 2 to 100 . UOP 603, see Table 2CO2, mg/kg 1 to 10 2 to 100 2 to 100 UOP 603, 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 VolatileS, mg/kg 1 to
38、10 1 to 10 10 to 250 D6667, 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 . D4629, see Table 2Total chloride, mg/kg 1 to 5 1 to 10 . See Table 2Methanol, mg/kg 1 to 5 1 to 10 . D7423, D4864, see
39、 Table 2Other alcohols, mg/kg 1 to 5 1 to 10 . D7423, see Table 2Total oxygenates, mg/kg 1 to 5 1 to 10 . D7423, 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 Tes
40、t MethodsMethane, ethane, cyclopropane, butanes, and C5s An adaptation of Test Method D2712 is used by some labs. Others use an adaptation of Test MethodD2163.C6s and heavier An adaptation of Test Method D2163.Benzene An adaptation of Test Method D6729.H2,N2,O2, CO An adaptation of Test Method D2504
41、 is used by some. Test Method D8098 GC-PDHID, UOP 603 (CO).CO2An adaptation of Test Method D2505 is used by some. Test Method D8098 GC-PDHID, UOP 603 (CO2).Carbonyl sulfide A GC-FPD method is currently undergoing ASTM cooperative testing. Other methods used in the industryare GC-PID, GC-conductivity
42、, 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 methods currently undergoing ASTM testing.Total sulfur Some labs use an adaptation of Test Method D3246; others use Test Method D4468 with an oxy-hydrogenpyr
43、olyzer. Test Method D6667 or Test Method D8098 GC-MS method.Mercaptan sulfur Some methods used are: UOP 212; GC-FPD; caustic absorption/potentiometric titration analysis by TestMethod D3227. Test Method D8098 GC-MS method.Water Obtaining a valid sample for lab analysis is extremely difficult. Instea
44、d 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. Adaptation of Test Method D5454.Total nitrogen (bound) Test Method D4629. Others use microcoulometry methods.To
45、tal chlorides An adaptation of Test Methods D2384 may be used by some labs; others use reductive microcoulometry.Test Method D7994, Combustion IC.Arsine Some methods known to be in use are:AgDDC absorption/colorimetric finishAgDDC absorption/GFAAS finishdirect GC-ECD methoddirect GC-PID methodTotal
46、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 methods, Test Method D7423Other alcohols GC methods, both capillary
47、and packed column. Variation of Test Method D4864, D7423D5273 183SUMMARY OF CHANGESSubcommittee D02.D0 has identified the location of selected changes to this standard since the last issue(D5273 92 (2012) that may impact the use of this standard. (Approved July 1, 2018.)(1) Revised subsections 5.5.1
48、 and 5.5.2. (2) Revised Table 1 and Table 2.ASTM 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 validity of any such patent rights, and
49、 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 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 technical committee, which you may attend. If you feel that your comments have n
