ASTM D5303-20

Standard Test Method for Trace Carbonyl Sulfide in Propylene by Gas Chromatography

SIGNIFICANCE AND USE
5.1 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.  
5.2 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.  
5.3 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 9.  
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.

General Information

• Status: Published
• Publication Date: 30-Jun-2020
• ICS: 71.080.10 - Aliphatic hydrocarbons
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.D0.03 - Propylene

Standards Content (Sample)

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.
Designation:D5303 −20
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* Hydrogenolysis and Rateometric Colorimetry
E355PracticeforGasChromatographyTermsandRelation-
1.1 This test method covers the determination of traces of
ships
carbonyl sulfide (COS) in propylene. It is applicable to COS
E840PracticeforUsingFlamePhotometricDetectorsinGas
concentrations from 0.5mg⁄kg to 4.0mg⁄kg (parts per million
Chromatography
by mass). See Note 1.
NOTE 1—The lower limit of this test method is believed to be below
3. Terminology
0.1mg⁄kg, depending on sample size and sensitivity of the instrumenta-
tionbeingused.However,thecooperativetestingprogramwasconducted 3.1 Definitions:
in the 0.5 to 4.0 range due to limitations in preparing commercial test
3.1.1 Additional terminology related to the practice of gas
mixtures.
chromatography can be found in Practice E355.
1.2 The values stated in SI units are to be regarded as 3.1.2 liquefied petroleum gas (LPG), n—hydrocarbon gases
standard. No other units of measurement are included in this
that can be stored or handled in the liquid phase through
standard. compression or refrigeration, or both.
3.1.2.1 Discussion—LPG’s generally consist of C and C
1.3 This standard does not purport to address all of the 3 4
alkanes and alkenes or mixtures thereof and containing less
safety concerns, if any, associated with its use. It is the
than 10% by volume of higher carbon number material.Vapor
responsibility of the user of this standard to establish appro-
pressure does not normally exceed 2000kPa at 40ºC.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
3.2 Definitions of Terms Specific to This Standard:
Specific hazards statements are given in Section 9.
3.2.1 propane/propene mixtures, n—mixtures primarily
1.4 This international standard was developed in accor-
composed of propane and propene where one of these compo-
dance with internationally recognized principles on standard-
nents is usually in the concentration range of 30% to 85% by
ization established in the Decision on Principles for the
mass with the other comprising the majority of the remainder.
Development of International Standards, Guides and Recom-
Commercial Propane in Specification D1835 is typically this
mendations issued by the World Trade Organization Technical
sort of product mixture.
Barriers to Trade (TBT) Committee.
3.2.1.1 Discussion—Other components may be present,
usually at less than 10% by mass.
2. Referenced Documents
2
4. Summary of Test Method
2.1 ASTM Standards:
D1835Specification for Liquefied Petroleum (LP) Gases
4.1 A procedure is given for removing a sample from the
D3609Practice for Calibration Techniques Using Perme-
sample cylinder, separating COS from propylene, detecting
ation Tubes
COS, calibrating the detector, quantitating COS content in the
D4468Test Method for Total Sulfur in Gaseous Fuels by
sample, and assaying the gas standard. General comments and
recommended techniques are given.
4.2 Arelativelylargevolumeofsampleisinjectedintoagas
1
This test method is under the jurisdiction of ASTM Committee D02 on
chromatograph having a single packed column, operated iso-
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.D0.03 on Propylene.
thermally at 10°C to 50°C, that separates COS from propyl-
CurrenteditionapprovedJuly1,2020.PublishedJuly2020.Originallyapproved
ene. COS is detected with a flame photometric detector.
in 1992. Last previous edition approved in 2019 as D5303–19. DOI: 10.1520/
D5303-20.
4.3 Calibrationdata,basedonpeakareas,areobtainedusing
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
a known gas standard blend of COS in the range expected for
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
the sample. The COS peak area in the sample is measured and
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the concentration of COS calculated.
*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 ----------
...

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 − 19 D5303 − 20
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*
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 89.
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:
D1835 Specification for Liquefied Petroleum (LP) Gases
D3609 Practice for Calibration Techniques Using Permeation Tubes
D4468 Test Method for Total Sulfur in Gaseous Fuels by Hydrogenolysis and Rateometric Colorimetry
E355 Practice for Gas Chromatography Terms and Relationships
E840 Practice for Using Flame Photometric Detectors in Gas Chromatography
3. Terminology
3.1 Definitions:
3.1.1 Additional terminology related to the practice of gas chromatography can be found in Practice E355.
3.1.2 liquefied petroleum gas (LPG), n—hydrocarbon gases that can be stored or handled in the liquid phase through
compression or refrigeration, or both.
3.1.2.1 Discussion—
LPG’s generally consist of C and C alkanes and alkenes or mixtures thereof and containing less than 10 % by volume of higher
3 4
carbon number material. Vapor pressure does not normally exceed 2000 kPa at 40 ºC.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 propane/propene mixtures, n—mixtures primarily composed of propane and propene where one of these components is
usually in the concentration range of 30 % to 85 % by mass with the other comprising the majority of the remainder. Commercial
Propane in Specification D1835 is typically this sort of product mixture.
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 May 1, 2019July 1, 2020. Published June 2019July 2020. Originally approved in 1992. Last previous edition approved in 20122019 as
D5303 – 92 (2012).D5303 – 19. DOI: 10.1520/D5303-19.10.1520/D5303-20.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 − 20
3.2.1.1 Discussion—
Other components may be present, usually at less than 10 % by mass.
4. Summary of Test Method
4.1 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.
4.2 A relatively large volume of sample is injected into a gas chromatograph having a single packed column, operated
isothermally at 10 °C to 50 °C, that separates COS from propyl
...