ASTM D5303-19
(Test Method)Standard Test Method for Trace Carbonyl Sulfide in Propylene by Gas Chromatography
Standard Test Method for Trace Carbonyl Sulfide in Propylene by Gas Chromatography
SIGNIFICANCE AND USE
4.1 In processes producing propylene, COS usually remains with the C3 hydrocarbons and must be removed, since it affects product quality. COS acts as a poison to commercial polymerization catalysts, resulting in deactivation and costly process downtime.
4.2 Accurate gas chromatographic determination of trace COS in propylene involves unique analytical problems because of the chemical nature of COS and idiosyncracies of trace level analyses. These problems result from the reactive and absorptive nature of COS, the low concentration levels being measured, the type of detector needed, and the interferences from the propylene sample matrix. This test method addresses these analytical problems and ways to properly handle them to assure accurate and precise analyses.
4.3 This test method provides a basis for agreement between two laboratories when the determination of trace COS in propylene is important. The test method permits several calibration techniques. For best agreement between two labs, it is recommended that they use the same calibration technique.
SCOPE
1.1 This test method covers the determination of traces of carbonyl sulfide (COS) in propylene. It is applicable to COS concentrations from 0.5 mg/kg to 4.0 mg/kg (parts per million by mass). See Note 1.
Note 1: The lower limit of this test method is believed to be below 0.1 mg/kg, depending on sample size and sensitivity of the instrumentation being used. However, the cooperative testing program was conducted in the 0.5 to 4.0 range due to limitations in preparing commercial test mixtures.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 8.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation:D5303 −19
Standard Test Method for
Trace Carbonyl Sulfide in Propylene by Gas
1
Chromatography
This standard is issued under the fixed designation D5303; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* E840PracticeforUsingFlamePhotometricDetectorsinGas
Chromatography
1.1 This test method covers the determination of traces of
carbonyl sulfide (COS) in propylene. It is applicable to COS
3. Summary of Test Method
concentrations from 0.5mg⁄kg to 4.0mg⁄kg (parts per million
by mass). See Note 1.
3.1 A procedure is given for removing a sample from the
sample cylinder, separating COS from propylene, detecting
NOTE 1—The lower limit of this test method is believed to be below
COS, calibrating the detector, quantitating COS content in the
0.1mg⁄kg, depending on sample size and sensitivity of the instrumenta-
tionbeingused.However,thecooperativetestingprogramwasconducted sample, and assaying the gas standard. General comments and
in the 0.5 to 4.0 range due to limitations in preparing commercial test
recommended techniques are given.
mixtures.
3.2 Arelativelylargevolumeofsampleisinjectedintoagas
1.2 The values stated in SI units are to be regarded as
chromatograph having a single packed column, operated iso-
standard. No other units of measurement are included in this
thermally at 10°C to 50°C, that separates COS from propyl-
standard.
ene. COS is detected with a flame photometric detector.
1.3 This standard does not purport to address all of the
3.3 Calibrationdata,basedonpeakareas,areobtainedusing
safety concerns, if any, associated with its use. It is the
a known gas standard blend of COS in the range expected for
responsibility of the user of this standard to establish appro-
the sample. The COS peak area in the sample is measured and
priate safety, health, and environmental practices and deter-
the concentration of COS calculated.
mine the applicability of regulatory limitations prior to use.
Specific hazards statements are given in Section 8. 3.4 The COS gas standard blend is assayed prior to use for
1.4 This international standard was developed in accor-
calibration.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Significance and Use
Development of International Standards, Guides and Recom-
4.1 Inprocessesproducingpropylene,COSusuallyremains
mendations issued by the World Trade Organization Technical
withtheC hydrocarbonsandmustberemoved,sinceitaffects
3
Barriers to Trade (TBT) Committee.
product quality. COS acts as a poison to commercial polym-
erization catalysts, resulting in deactivation and costly process
2. Referenced Documents
downtime.
2
2.1 ASTM Standards:
4.2 Accurate gas chromatographic determination of trace
D3609Practice for Calibration Techniques Using Perme-
COSinpropyleneinvolvesuniqueanalyticalproblemsbecause
ation Tubes
ofthechemicalnatureofCOSandidiosyncraciesoftracelevel
D4468Test Method for Total Sulfur in Gaseous Fuels by
analyses. These problems result from the reactive and absorp-
Hydrogenolysis and Rateometric Colorimetry
tive nature of COS, the low concentration levels being
measured, the type of detector needed, and the interferences
from the propylene sample matrix. This test method addresses
1
This test method is under the jurisdiction of ASTM Committee D02 on
these analytical problems and ways to properly handle them to
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.D0.03 on Propylene.
assure accurate and precise analyses.
Current edition approved May 1, 2019. Published June 2019. Originally
4.3 Thistestmethodprovidesabasisforagreementbetween
approved in 1992. Last previous edition approved in 2012 as D5303–92(2012).
DOI: 10.1520/D5303-19.
two laboratories when the determination of trace COS in
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
propylene is important. The test method permits several
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
calibrationtechniques.Forbestagreementbetweentwolabs,it
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. is recommended that they use the same calibration technique.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5303−19
5. Interferences 6.6 Data Handling System—Any commercially available
GC integr
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5303 − 92 (Reapproved 2012) D5303 − 19
Standard Test Method for
Trace Carbonyl Sulfide in Propylene by Gas
1
Chromatography
This standard is issued under the fixed designation D5303; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Scope*
1.1 This test method covers the determination of traces of carbonyl sulfide (COS) in propylene. It is applicable to COS
concentrations from 0.50.5 mg ⁄kg to 4.04.0 mg mg/kg ⁄kg (parts per million by mass). See Note 1.
NOTE 1—The lower limit of this test method is believed to be below 0.10.1 mg mg/kg, ⁄kg, depending on sample size and sensitivity of the
instrumentation being used. However, the cooperative testing program was conducted in the 0.5 to 4.0 range due to limitations in preparing commercial
test mixtures.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 8.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D3609 Practice for Calibration Techniques Using Permeation Tubes
D4468 Test Method for Total Sulfur in Gaseous Fuels by Hydrogenolysis and Rateometric Colorimetry
E840 Practice for Using Flame Photometric Detectors in Gas Chromatography
3. Summary of Test Method
3.1 A procedure is given for removing a sample from the sample cylinder, separating COS from propylene, detecting COS,
calibrating the detector, quantitating COS content in the sample, and assaying the gas standard. General comments and
recommended techniques are given.
3.2 A relatively large volume of sample is injected into a gas chromatograph having a single packed column, operated
isothermally at 1010 °C to 50°C,50 °C, that separates COS from propylene. COS is detected with a flame photometric detector.
3.3 Calibration data, based on peak areas, are obtained using a known gas standard blend of COS in the range expected for the
sample. The COS peak area in the sample is measured and the concentration of COS calculated.
3.4 The COS gas standard blend is assayed prior to use for calibration.
4. Significance and Use
4.1 In processes producing propylene, COS usually remains with the C hydrocarbons and must be removed, since it affects
3
product quality. COS acts as a poison to commercial polymerization catalysts, resulting in deactivation and costly process
downtime.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.D0.03 on Propylene.
Current edition approved Dec. 1, 2012May 1, 2019. Published December 2012June 2019. Originally approved in 1992. Last previous edition approved in 20072012 as
D5303–92(2007).D5303 – 92 (2012). DOI: 10.1520/D5303-92R12.10.1520/D5303-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5303 − 19
4.2 Accurate gas chromatographic determination of trace COS in propylene involves unique analytical problems because of the
chemical nature of COS and idiosyncracies of trace level analyses. These problems result from the reactive and absorptive nature
of COS, the low concentration levels being measured, the type of detector needed, and the interferences from the propylene sample
matrix. T
...
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