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ASTM D7652-11

(Test Method)

Standard Test Method for Determination of Trace Hydrogen Sulfide, Carbonyl Sulfide, Methyl Mercaptan, Carbon Disulfide and Total Sulfur in Hydrogen Fuel by Gas Chromatography and Sulfur Chemiluminescence Detection (Withdrawn 2020)

Standard Test Method for Determination of Trace Hydrogen Sulfide, Carbonyl Sulfide, Methyl Mercaptan, Carbon Disulfide and Total Sulfur in Hydrogen Fuel by Gas Chromatography and Sulfur Chemiluminescence Detection (Withdrawn 2020)

SIGNIFICANCE AND USE
Low operating temperature fuel cells such as proton exchange membrane fuel cells (PEMFCs) require high purity hydrogen for maximum material performance and lifetime. Sulfur compounds are present in many of the materials used in hydrogen production and small quantities typically remain after processing and purification. Part-per-billion concentrations of sulfur gases such as hydrogen sulfide (H2S), carbonyl sulfide (COS) and mercaptans diminish single fuel cell capacity.
SCOPE
1.1 This test method describes a procedure primarily for the determination of hydrogen sulfide, carbonyl sulfide, methyl mercaptan, and carbon disulfide (Table 1) in hydrogen fuels for fuel cell vehicles (FCV) by gas chromatograph with sulfur chemiluminescence detection. The reporting limit is 0.02 ppbv (nanomole per mole as volume), based upon the analysis of a 500 mL hydrogen sample. The procedures described in this method were designed to satisfy sulfur contaminant determination requirements contained in SAE TIRJ2719 and the California Code of Regulations, CFR , Title 4, Division 9, Chapter 6, Article 8, Sections 4180 – 4181.
1.2 This test method can be extended to other sulfur species in hydrogen fuel that are eluted through a chromatographic column.  
1.3 This test method can be modified to analyze all sulfur compounds present without chromatographic separation; thus, providing a total sulfur estimation without speciation (Appendix X1).
1.4 If any new sulfur compounds need to be analyzed in hydrogen fuel, the calibration or spiking sulfur standards must include these new compounds after their method detection limit study. In addition, no co-elution is allowed in the chromatographic analysis of the calibration standard containing both the newly added and the existing sulfur target compounds. If necessary, the chromatographic conditions may be modified to achieve this goal.
1.5 Although, primarily intended for determining sulfur in hydrogen used as a fuel for fuel cell or internal combustion engine powered vehicles, this test method can also be used to measure sulfur compounds in other gaseous fuels and gaseous matrices provided data quality objectives are satisfied.
1.6 The values stated in SI units are standard. The values stated in inch-pound units are for information only.  
1.7 Mention of trade names in this standard does not constitute endorsement or recommendation for use. Other manufacturers of equipment or equipment models can be used.
1.8 Alternative Detectors—This test method is written primarily for the use of sulfur chemiluminescent detectors but other detectors can be used provided they can detect hydrogen sulfide, carbonyl sulfide, methyl mercaptan, and carbon disulfide at 0.02 ppbv in hydrogen and meet data quality objectives for the intended use.  
1.9 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 and health practices and determine the applicability of regulatory limitations prior to use. For safety issues related to liquid nitrogen, refer to material safety data sheet (MSDS) from liquid nitrogen supplier.
WITHDRAWN RATIONALE
This test method describes a procedure primarily for the determination of hydrogen sulfide, carbonyl sulfide, methyl mercaptan, and carbon disulfide (Table 1) in hydrogen fuels for fuel cell vehicles (FCV) by gas chromatograph with sulfur chemiluminescence detection.
Formerly under the jurisdiction of Committee D03 on Gaseous Fuels, this test method was withdrawn in June 2020 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

Status
Withdrawn
Publication Date
28-Feb-2011
Withdrawal Date
01-Jun-2020
ICS
27.075 - Hydrogen technologies
Technical Committee
D03 - Gaseous Fuels
Drafting Committee
D03.14 - Hydrogen and Fuel Cells
Current Stage
Ref Project

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ASTM D7652-11 - Standard Test Method for Determination of Trace Hydrogen Sulfide, Carbonyl Sulfide, Methyl Mercaptan, Carbon Disulfide and Total Sulfur in Hydrogen Fuel by Gas Chromatography and Sulfur Chemiluminescence Detection (Withdrawn 2020)ASTM D7652-11 - Standard Test Method for Determination of Trace Hydrogen Sulfide, Carbonyl Sulfide, Methyl Mercaptan, Carbon Disulfide and Total Sulfur in Hydrogen Fuel by Gas Chromatography and Sulfur Chemiluminescence Detection (Withdrawn 2020)
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ASTM D7652-11 - Standard Test Method for Determination of Trace Hydrogen Sulfide, Carbonyl Sulfide, Methyl Mercaptan, Carbon Disulfide and Total Sulfur in Hydrogen Fuel by Gas Chromatography and Sulfur Chemiluminescence Detection (Withdrawn 2020)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D7652 −11
Standard Test Method for
Determination of Trace Hydrogen Sulfide, Carbonyl Sulfide,
Methyl Mercaptan, Carbon Disulfide and Total Sulfur in
Hydrogen Fuel by Gas Chromatography and Sulfur
1
Chemiluminescence Detection
This standard is issued under the fixed designation D7652; 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 1.6 The values stated in SI units are standard. The values
stated in inch-pound units are for information only.
1.1 Thistestmethoddescribesaprocedureprimarilyforthe
1.7 Mention of trade names in this standard does not
determination of hydrogen sulfide, carbonyl sulfide, methyl
mercaptan,andcarbondisulfide(Table1)inhydrogenfuelsfor constitute endorsement or recommendation for use. Other
manufacturersofequipmentorequipmentmodelscanbeused.
fuel cell vehicles (FCV) by gas chromatograph with sulfur
chemiluminescence detection.The reporting limit is 0.02 ppbv
1.8 Alternative Detectors—This test method is written pri-
(nanomole per mole as volume), based upon the analysis of a
marily for the use of sulfur chemiluminescent detectors but
500 mL hydrogen sample. The procedures described in this
other detectors can be used provided they can detect hydrogen
method were designed to satisfy sulfur contaminant determi-
sulfide, carbonyl sulfide, methyl mercaptan, and carbon disul-
nation requirements contained in SAE TIRJ2719 and the
fide at 0.02 ppbv in hydrogen and meet data quality objectives
California Code of Regulations, CFR , Title 4, Division 9,
for the intended use.
Chapter 6, Article 8, Sections 4180 – 4181.
1.9 This standard does not purport to address all of the
1.2 Thistestmethodcanbeextendedtoothersulfurspecies
safety concerns, if any, associated with its use. It is the
in hydrogen fuel that are eluted through a chromatographic
responsibility of the user of this standard to establish appro-
column.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For safety issues
1.3 This test method can be modified to analyze all sulfur
related to liquid nitrogen, refer to material safety data sheet
compounds present without chromatographic separation; thus,
(MSDS) from liquid nitrogen supplier.
providing a total sulfur estimation without speciation (Appen-
dix X1).
2. Referenced Documents
2
1.4 If any new sulfur compounds need to be analyzed in
2.1 ASTM Standards:
hydrogen fuel, the calibration or spiking sulfur standards must
D5504TestMethodforDeterminationofSulfurCompounds
include these new compounds after their method detection
in Natural Gas and Gaseous Fuels by Gas Chromatogra-
limit study. In addition, no co-elution is allowed in the
phy and Chemiluminescence
chromatographic analysis of the calibration standard contain-
D7606Practice for Sampling of High Pressure Hydrogen
ing both the newly added and the existing sulfur target
and Related Fuel Cell Feed Gases
3
compounds. If necessary, the chromatographic conditions may
2.2 SAE Standards:
be modified to achieve this goal.
SAETIRJ2719InformationReportoftheDevelopmentofa
Hydrogen Quality Guideline for Fuel Cell Vehicles
1.5 Although, primarily intended for determining sulfur in
4
2.3 California Code of Regulations:
hydrogen used as a fuel for fuel cell or internal combustion
CaliforniaCodeofRegulationsTitle4,Division89,Chapter
engine powered vehicles, this test method can also be used to
6, Article 8, Sections 4180–4181.
measure sulfur compounds in other gaseous fuels and gaseous
matrices provided data quality objectives are satisfied.
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
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD03onGaseous the ASTM website.
3
Fuels and is the direct responsibility of Subcommittee D03.14 on Hydrogen and AvailablefromSAEInternational(SAE),400CommonwealthDr.,Warrendale,
Fuel Cells. PA 15096-0001, http://www.sae.org.
4
Current edition approved March 1, 2011. Published March 2011. DOI 10. AvailablefromtheOfficeofAdministrativeLaw,300CapitolMall,Suite1250,
1520/D7652–11. Sacramento, CA 95814–4339.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7652−11
TABLE 1 Trace Sulfur Contaminates
Compound Formula MW BC°C MP°C CAS No.
Hydrogen sulfide H S 34.08 -61 -86 7783–06–4
2
Carbonyl sulfide COS 60.07 -50 -139 463–58–1
Methyl maercaptan
...

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5.1 Proton exchange membranes (PEM) used in fuel cells are susceptible to contamination from a number of species that can be found in hydrogen. It is critical that these contaminants be measured and verified to be present at or below the amounts stated in SAE J2719 and ISO 14687 to ensure both fuel cell longevity and optimum efficiency. Contaminant concentrations as low as single-figure ppb(v) for some species can seriously compromise the life span and efficiency of PEM fuel cells. The presence of contaminants in fuel-cell-grade hydrogen can, in some cases, have a permanent adverse impact on fuel cell efficiency and usability. It is critical to monitor the concentration of key contaminants in hydrogen during the production phase through to delivery of the fuel to a fuel cell vehicle or other PEM fuel cell application. In ISO 14687, the upper limits for the contaminants are specified. Refer to SAE J2719 (see 2.3) for specific national and regional requirements. For hydrogen fuel that is transported and delivered as a cryogenic liquid, there is additional risk of introducing impurities during transport and delivery operations. For instance, moisture can build up over time in liquid transfer lines, critical control components, and long-term storage facilities, which can lead to ice buildup within the system and subsequent blockages that pose a safety risk or the introduction of contaminants into the gas stream upon evaporation of the liquid. Users are reminded to consult Practice D7265 for critical thermophysical properties such as the ortho/para hydrogen spin isomer inversion that can lead to additional hazards in liquid hydrogen usage.
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1.1 This test method describes contaminant determination in fuel cell grade hydrogen as specified in relevant ASTM and ISO standards using cavity ring-down spectroscopy (CRDS). This standard test method is for the measurement of one or multiple contaminants including, but not limited to, water (H2O), oxygen (O2), methane (CH4), carbon dioxide (CO2), carbon monoxide (CO), ammonia (NH3), and formaldehyde (H2CO), henceforth referred to as “analyte.”  
1.2 This test method applies to CRDS analyzers with one or multiple sensor modules (see 6.2 for definition). This test method describes sampling apparatus design, operating procedures, and quality control procedures required to obtain the stated levels of precision and accuracy.  
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ASTM D7675-22(Test Method)
Standard Test Method for Determination of Total Hydrocarbons in Hydrogen by FID-Based Total Hydrocarbon (THC) Analyzer

SIGNIFICANCE AND USE
5.1 Low operating temperature fuel cells such as proton exchange membrane fuel cells (PEM-FC) require high purity hydrogen for maximum material performance and lifetime. Analysis to 0.1 part per million (ppm(v)) concentration of THCs (measured as CH4) in hydrogen is necessary for ensuring a feed gas of sufficient purity to satisfy fuel cell system needs as defined in SAE J2719 or as specified in regulatory codes.  
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5.3 Although not intended for application to gases other than hydrogen, techniques within this test method can be applied to other non-hydrocarbon gas samples requiring THC content determination. This can be achieved by using a zero gas and a calibration gas that consist of the same background gas as the actual sample. As an example, for the THC determination of nitrogen, the instrument zero point must be determined with a high purity grade of nitrogen (99.999 % and 4 in nitrogen in the appropriate range. This will correct for any interferences caused by the background gas.
SCOPE
1.1 This test method describes a procedure for total hydrocarbons (THC’s) measurement in hydrogen intended as a fuel on a methane (C1) basis. The determination of THC on a C1 basis is an analytical technique where all the hydrocarbons are assumed to have the same response as methane (CH4). Sensitivity from 0.1 parts per million by volume (ppm(v), µmol/mol) up to 1000 ppm(v) concentration is achievable. Higher concentrations can be analyzed using appropriate dilution techniques. This test method can be applied to other gaseous samples requiring analysis of trace constituents provided an assessment of potential interferences has been accomplished.  
1.2 This test method is a Flame Ionization Detector-based (FID-based) hydrocarbon analysis method without the use of separation columns. Therefore, this method does not provide speciation of individual hydrocarbons. Several varieties of instruments are manufactured and can be used for this method.  
1.2.1 This method provides a measure of THC “as CH4,” because all hydrocarbon species are quantified the same as CH4 response, which is the sole species used for calibration. Magnitude of the FID response to an atom of carbon is dependent on the chemical environment of this atom in the molecule. This method provides the THC result as if all carbon atoms are from aliphatic, aromatic, olefinic, or acetylenic compounds, where the detector response caused by these atoms is approximately relative to the number of carbon atoms present in the molecule. Other types of molecules, including those containing oxygen or chlorine atoms, will respond differently and usually much lower than the corresponding aliphatic hydrocarbon. Therefore, other methods (Test Methods D7653, D7892, or equivalent) must be utilized to determine the exact constituents of the THC response determined by this method.  
1.3 The proper handling of compressed gas cylinders containing air, nitrogen, hydrogen, or helium requires the use of gas regulators to preclude over-pressurization of any instrument component  
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Standard Test Method for Determination of Total Organic Halides, Total Non-Methane Hydrocarbons, and Formaldehyde in Hydrogen Fuel by Gas Chromatography/Mass Spectrometry

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5.1 Low operating temperature fuel cells such as PEMFCs require high purity hydrogen for optimal performance and longevity. Organic halides and formaldehyde can react with catalyst in PEMs and non-methane hydrocarbons degrade PEM stack performance.
SCOPE
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ASTM D7650-21(Practice)
Standard Practice for Sampling of Particulate Matter in High Pressure Gaseous Fuels with an In-Stream Filter

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5.1 This sampling procedure is used to collect a particulate filter sample containing particulates 0.2 µm or larger in size to be used to measure the size and concentration of particulates in a gaseous fuel stream.
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1.1 This practice is primarily for sampling particulates in gaseous fuels up to a nominal working pressure (NWP) of 70 MPa (10 152 psi) using an in-stream filter. This practice describes sampling apparatus design, operating procedures, and quality control procedures required to obtain the stated levels of precision and accuracy.  
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5.1 Low operating temperature fuel cells such as proton exchange membrane fuel cells (PEMFCs) require high purity hydrogen for maximum performance. The following are the reported effects (SAE TIR J2719) of the compounds determined by this test method.  
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ASTM D7676-18(Practice)
Standard Practice for Screening Organic Halides Contained in Hydrogen or Other Gaseous Fuels

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5.1 Low operating temperature fuel cells such as proton exchange membrane fuel cells (PEFCs) require high purity hydrogen for maximum material performance and lifetime. Analysis to at least 0.05 µmol/mol concentration of total halogenated (measured as methyl fluoride) in hydrogen is necessary for assuring a feed gas of sufficient purity to satisfy fuel cell system needs as defined in ISO TS 14687-2, SAE J2719, and the California Code of Regulations, or as specified in regulatory codes.  
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SCOPE
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ASTM D7265-12(2018)(Specification)
Standard Specification for Hydrogen Thermophysical Property Tables

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1.1 The thermophysical property tables for normal hydrogen are for use in the calculation of the pressure-volume-temperature (PVT), thermodynamic, and transport properties of hydrogen for process design and operations, particularly as they relate to hydrogen fuel cell applications. Tables are provided for gaseous hydrogen at temperatures between 50 K and 500 K at pressures to 50 MPa. These tables were developed by the National Institute of Standards and Technology from a Standard Reference Database product REFPROP, version 9.0.  
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ASTM D7651-17(Test Method)
Standard Test Method for Gravimetric Measurement of Particulate Concentration of Hydrogen Fuel

SIGNIFICANCE AND USE
5.1 Low operating temperature fuel cells such as proton exchange membrane fuel cells (PEMFCs) require high purity hydrogen for maximum material performance and lifetime. Measurement of particulates in hydrogen is necessary for assuring a feed gas of sufficient purity to satisfy fuel cell and internal combustion system needs as defined in SAE J2719. The particulates in hydrogen fuel for fuel cell vehicles (FCV) and gaseous hydrogen powered internal combustion engine vehicles may adversely affect pneumatic control components, such as valves, or other critical system components. Therefore, the concentration of particulates in the hydrogen fuel should be limited as specified by ISO 14687-2, SAE J2719, or other hydrogen fuel quality specifications.  
5.2 Although not intended for application to gases other than hydrogen fuel, techniques within this test method can be applied to gas samples requiring determination of particulate concentration.
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1.1 This test method is primarily intended for gravimetric determination of particulate concentration in hydrogen intended as a fuel for fuel cell or internal combustion engine powered vehicles. This test method describes operating and quality control procedures required to obtain data of known quality satisfying the requirements of SAE J2719. This test method can be applied to other gaseous samples requiring determination of particulates provided the user’s data quality objectives are satisfied.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM D7606-17(Practice)
Standard Practice for Sampling of High Pressure Hydrogen and Related Fuel Cell Feed Gases

SIGNIFICANCE AND USE
5.1 Hydrogen is delivered to fuel cell powered automotive vehicles and stationary appliances at pressures up to 87.5 MPa. The quality of hydrogen delivered is a significant factor in maximizing fuel cell efficiency and life span. Contamination can occur during the production of fuel cell feed gases, contaminating storage containers, station tubing, and fuel lines used for fuel delivery. Collection of a representative fuel sample without the introduction of contaminants even as low as parts-per-billion (ppb) per contaminant during collection is crucial for assessing the quality of fuel in real world applications.  
5.2 This practice is intended for application to high pressure, high purity hydrogen; however, the apparatus design and sampling techniques may be applicable to collection of other fuel cell feed gases. Many of the techniques used in this practice can be applied to lower pressure/lower purity gas streams.
SCOPE
1.1 This standard practice describes a sampling procedure of high pressure hydrogen at fueling stations operating at 35 or 70 megapascals (MPa) using a hydrogen quality sampling apparatus (HQSA).  
1.2 This practice does not include the analysis of the acquired sample. Applicable ASTM standards include but are not limited to test methods referenced in Section 2 of this practice.  
1.3 This practice is not intended for sampling and measuring particulate matter in high pressure hydrogen. For procedures on sampling and measuring particulate matter see ASTM D7650 and D7651.  
1.4 The values stated in SI units are standard. The values stated in inch-pounds are for information only.  
1.5 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.  
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Standard Test Method for Visualizing Particulate Sizes and Morphology of Particles Contained in Hydrogen Fuel by Microscopy

SIGNIFICANCE AND USE
5.1 Low temperature fuel cells such as proton exchange membrane fuel cells (PEMFCs) require high purity hydrogen for maximum material performance and lifetime. The particulates in hydrogen used in FCVs and hydrogen powered internal combustion vehicles may adversely affect pneumatic control components, such as valves or other critical system components. The visualization of the size and morphology of particles is an important tool for determining particle origin as well as for devising particle formation reduction strategies.
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1.1 This test method is primarily intended for visualizing and measuring the sizes and morphology of particulates in hydrogen used as a fuel for fuel cell or internal combustion engine powered vehicles. This test method describes procedures required to obtain size and morphology data of known quality. This test method can be applied to other gaseous samples requiring determination of particulate sizes and morphology provided the user’s data quality objectives are satisfied.  
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