ASTM D7676-23

Standard Practice for Screening Organic Halides Contained in Hydrogen or Other Gaseous Fuels

SIGNIFICANCE AND USE
5.1 Low operating temperature fuel cells such as proton exchange membrane fuel cells 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 14687, SAE J2719, and the California Code of Regulations, or as specified in regulatory codes.  
5.2 Although not intended for application to gases other than hydrogen, techniques within this screening method can be applied to other gaseous samples requiring total halogenated hydrocarbon content determination. The method must be validated when used to test fuels or other gaseous samples that may contain interfering compounds.
SCOPE
1.1 This practice covers the screening of organic halide content of gaseous fuels using electron capture detection. Although primarily intended for determining organic halides in hydrogen used as a fuel for fuel cell or internal combustion engine powered vehicles, this screening method can also be used, if qualified, to measure organic halides in other gaseous fuels and gaseous matrices.  
1.2 The procedure described in this method was designed to screen organic halides in hydrogen to a level much less than required by SAE J2719 and the California Code of Regulations, Title 4, Division 9, Chapter 6, Article 8, Sections 4180 – 4181. It will yield false positive result to other compounds that show response to the electron capture detector (ECD). Samples that do not pass the criteria of this screening process shall be tested to quantify and qualify the contaminants using Test Method D7892.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.4 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.  
1.5 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: 31-Oct-2023
• ICS: 27.075 - Hydrogen technologies
• Technical Committee: D03 - Gaseous Fuels
• Drafting Committee: D03.14 - Hydrogen and Fuel Cells

Relations

• Replaces: ASTM D7676-18 - Standard Practice for Screening Organic Halides Contained in Hydrogen or Other Gaseous Fuels
• Effective Date: 01-Nov-2023
• Refers: ASTM D1265-23a - Standard Practice for Sampling Liquefied Petroleum (LP) Gases, Manual Method
• Effective Date: 01-Dec-2023
• Refers: ASTM D1265-23 - Standard Practice for Sampling Liquefied Petroleum (LP) Gases, Manual Method
• Effective Date: 01-Mar-2023

Overview

ASTM D7676-23: Standard Practice for Screening Organic Halides Contained in Hydrogen or Other Gaseous Fuels provides practical guidance for detecting low levels of organic halides in hydrogen fuel gas and other gaseous matrices. High purity hydrogen is crucial in low-temperature fuel cell applications, such as proton exchange membrane (PEM) fuel cells, to ensure peak performance and longevity. This practice employs electron capture detection (ECD) as a screening tool, helping to confirm that hydrogen used for fuel cell or combustion engine vehicles meets stringent quality requirements. The method aligns with guidelines in ISO 14687, SAE J2719, and the California Code of Regulations for hydrogen fuel contaminants.

Key Topics

• Purpose and Scope

  • Primary focus is the detection of organic halides in hydrogen, but applicable to other high-purity gaseous fuels after validation.
  • Designed as a screening method to rapidly assess contamination at levels significantly below regulatory limits.
  • Serves as a pass/fail test; samples failing screening should undergo further quantitative analysis.

• Analytical Technique

  • Uses a gas chromatograph (GC) equipped with an electron capture detector (ECD) for sensitivity to trace halogenated hydrocarbons.
  • Relies on calibration gases and blank testing to ensure system accuracy and minimize false positives.

• Interferences and Precautions

  • Electron capture detectors are sensitive to compounds such as oxygen and water, which can cause positive bias.
  • Strict requirements for gas purity and equipment cleanliness are essential to prevent contamination and erroneous readings.
  • Safety practices for handling hydrogen and other pressurized gases are emphasized.

• Regulatory Context

  • Aligns with specifications and purity levels outlined in referenced standards and regulations governing hydrogen fuel quality.
  • Designed to meet or exceed purity requirements relevant for fuel cell vehicles.

Applications

• Hydrogen Fuel Quality Control

  • Ensures hydrogen intended for PEM fuel cells or internal combustion vehicles is free of contaminating organic halides, helping prolong equipment life and meet compliance standards.

• Production and Distribution

  • Suitable for hydrogen production facilities, distributors, and refueling stations who must guarantee product quality.
  • Screening method can be integrated into routine quality assurance protocols for rapid compliance verification.

• Broader Gaseous Fuels Assessment

  • While aimed at hydrogen, the screening technique can be adapted for other gaseous fuels (e.g., natural gas, syngas) after appropriate method validation, supporting a wide range of energy applications where fuel purity is critical.

• Regulatory and Research Use

  • Useful in laboratory and regulatory settings for pre-screening samples before more intensive, quantitative analysis as dictated by sectors demanding ultra-high fuel purity.

Related Standards

• ASTM D7892 - Quantitative determination of organic halides and related compounds in hydrogen fuel by GC/MS.
• ISO 14687 - International specifications for hydrogen fuel quality, including PEM fuel cell applications.
• SAE J2719 - Establishes hydrogen fuel quality guidelines for fuel cell vehicles.
• California Code of Regulations Title 4 - State-level requirements for hydrogen fuel contaminants.
• ASTM D1265, D3700, D4150, D7606 - Cover sampling and terminology relevant to gaseous fuels and hydrogen quality assurance.

By following ASTM D7676-23, organizations can reliably screen for organic halides in hydrogen and ensure compliance with both national and international regulations, supporting safe and efficient integration of hydrogen as a clean energy carrier.

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: D7676 − 23
Standard Practice for
Screening Organic Halides Contained in Hydrogen or Other
Gaseous Fuels
This standard is issued under the fixed designation D7676; 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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This practice covers the screening of organic halide
content of gaseous fuels using electron capture detection. D1265 Practice for Sampling Liquefied Petroleum (LP)
Gases, Manual Method
Although primarily intended for determining organic halides in
hydrogen used as a fuel for fuel cell or internal combustion D3700 Practice for Obtaining LPG Samples Using a Float-
ing Piston Cylinder
engine powered vehicles, this screening method can also be
used, if qualified, to measure organic halides in other gaseous D4150 Terminology Relating to Gaseous Fuels
D7606 Practice for Sampling of High Pressure Hydrogen
fuels and gaseous matrices.
and Related Fuel Cell Feed Gases
1.2 The procedure described in this method was designed to
D7892 Test Method for Determination of Total Organic
screen organic halides in hydrogen to a level much less than
Halides, Total Non-Methane Hydrocarbons, and Formal-
required by SAE J2719 and the California Code of
dehyde in Hydrogen Fuel by Gas Chromatography/Mass
Regulations, Title 4, Division 9, Chapter 6, Article 8, Sections
Spectrometry
4180 – 4181. It will yield false positive result to other
2.2 ISO Standard:
compounds that show response to the electron capture detector
ISO 14687 Hydrogen Fuel — Product Specification
(ECD). Samples that do not pass the criteria of this screening
2.3 SAE Standard:
process shall be tested to quantify and qualify the contaminants
SAE J2719 Hydrogen Fuel Quality for Fuel Cell Vehicles
using Test Method D7892.
2.4 Additional Document:
1.3 The values stated in SI units are to be regarded as
California Code of Regulations Title 4, Division 9, Chapter
standard. The values given in parentheses after SI units are
6, Article 8, Sections 4180 – 4181
provided for information only and are not considered standard.
3. Terminology
1.4 This standard does not purport to address all of the
3.1 Definitions—For definitions of general terms used in
safety concerns, if any, associated with its use. It is the
D03 Gaseous Fuels standards, refer to Terminology D4150.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
3.2 Definitions of Terms Specific to This Standard:
mine the applicability of regulatory limitations prior to use.
3.2.1 electron capture detector (ECD), n—detects organic
1.5 This international standard was developed in accor-
halides by the reduction of a standing detector current due to
dance with internationally recognized principles on standard-
the capture of detector current electrons by the halogenated
ization established in the Decision on Principles for the
hydrocarbons.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Barriers to Trade (TBT) Committee.
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.
Available from International Organization for Standardization (ISO), ISO
This practice is under the jurisdiction of ASTM Committee D03 on Gaseous Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
Fuels and is the direct responsibility of Subcommittee D03.14 on Hydrogen and Geneva, Switzerland, http://www.iso.org.
Fuel Cells. Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale,
Current edition approved Nov. 1, 2023. Published November 2023. Originally PA 15096, http://www.sae.org.
approved in 2018. Last previous edition approved in 2018 as D7676 – 18. DOI: Available from California Department of Food and Agriculture, 1220 N Street,
10.1520/D7676-23. Sacramento, CA 95814, https://www.cdfa.ca.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7676 − 23
3.2.2 organic halide, n—any compound containing carbon 6.2 The electron capture detector is very sensitive, typically
and a halogen (fluorine, chlorine, bromine, or iodine). capable of measuring organic halides to 0.0001 ppm(v). Any
interfering contamination of carrier and detector gases with
3.2.3 total organic halides, n—the sum concentration of all
either organic halides, oxygen, or water can render the ECD
compounds containing carbon and at least one halide (fluorine,
detector either unusable or result in a positive bias. All supply
chlorine, bromine, or iodine).
and dilution gases must be of the highest purity and in-line
3.3 Acronyms:
purification may be required.
3.3.1 ECD—electron capture detector
6.3 All components in contact with the carrier, detector, and
3.3.2 GC—gas chromatograph
sample gases must be cleaned and free of halogen contamina-
tion. Metal to metal seals shall be used whenever possible.
4. Summary of Screening Method
Teflon seals shall be avoided.
4.1 The screening of organic halides in hydrogen and other
7. Apparatus
gaseous fuels can be challenging due to need to measure total
7.1 The apparatus and analytic parameters below have been
organic halides to 50 ppb(v) to satisfy hydrogen fuel contami-
successfully used to satisfy the measurement requirements
nant requirements specified in ISO 14687, SAE J2719, and the
described in this standard. Other parameters can be used
California Code of Regulations.
provided measurement requirements and quality assurance
4.2 Organic halides, at any detectable concentration, are not
objectives can be satisfied.
normally present in hydrogen. Any contamination observed
7.1.1 Gas Chromatograph, with electron capture detector
will be due to improper maintenance or cleaning of equipment;
and electronic signal integrator, computer, or other recording
therefore, any positive result should be cause for further testing
device
and evaluation.
7.1.2 Gas Sampling System, with 1 mL sample loop or other
4.3 A gas chromatograph (GC) equipped with an ECD
sample loop volume satisfying organic halide measurement
detector and gas sampling system with a 1 mL sample loop is
needs.
typically used. The GC column is replaced by a length of blank
8. Reagents and Materials
tubing. Carrier gas and detector flows are set to manufacturer’s
specifications.
8.1 Helium Carrier/makeup Gas with Minimum Specifica-
tions: Oxygen < 0.5 ppm(v), Water < 0.2 ppm(v), Total Hy-
4.4 The sample gas is injected into the inlet of the GC-ECD
drocarbons < 0.1 ppm(v), Carbon Monoxide < 0.1 ppm(v),
system through the blank tubing and the ECD detector. A signal
Carbon Dioxide < 0.1 ppm(v).
is produced as organic halides pass though the detector. The
signal is sent to a computer, integrator, or
...

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: D7676 − 18 D7676 − 23
Standard Practice for
Screening Organic Halides Contained in Hydrogen or Other
Gaseous Fuels
This standard is issued under the fixed designation D7676; 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 practice covers the screening of organic halide content of gaseous fuels using electron capture detection. Although
primarily intended for determining organic halides in hydrogen used as a fuel for fuel cell or internal combustion engine powered
vehicles, this screening method can also be used, if qualified, to measure organic halides in other gaseous fuels and gaseous
matrices.
1.2 The procedure described in this method was designed to screen organic halides in hydrogen to a level much less than required
by SAE J2719 and the California Code of Regulations, Title 4, Division 9, Chapter 6, Article 8, Sections 4180 – 4181. It will yield
false positive result to other compounds that show response to the ECD detector. electron capture detector (ECD). Samples that
do not pass the criteria of this screening process shall be tested to quantify and qualify the contaminants using Test Method D7892.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for
information only and are not considered standard.
1.4 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.
1.5 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
2.1 ASTM Standards:
D1265 Practice for Sampling Liquefied Petroleum (LP) Gases, Manual Method
D3700 Practice for Obtaining LPG Samples Using a Floating Piston Cylinder
D4150 Terminology Relating to Gaseous Fuels
D7606 Practice for Sampling of High Pressure Hydrogen and Related Fuel Cell Feed Gases
D7892 Test Method for Determination of Total Organic Halides, Total Non-Methane Hydrocarbons, and Formaldehyde in
Hydrogen Fuel by Gas Chromatography/Mass Spectrometry
This practice is under the jurisdiction of ASTM Committee D03 on Gaseous Fuels and is the direct responsibility of Subcommittee D03.14 on Hydrogen and Fuel Cells.
Current edition approved Dec. 15, 2018Nov. 1, 2023. Published February 2019November 2023. Originally approved in 2018. Last previous edition approved in 2018 as
D7676 – 18. DOI: 10.1520/D7676-18.10.1520/D7676-23.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7676 − 23
2.2 ISO Standard:
ISO TS 14687-214687 Hydrogen Fuel — Product Specification — Part 2: Proton Exchange Membrane (PEM) Fuel Cell
Applications for Road Vehicles
2.3 SAE Standard:
SAE J2719 Hydrogen Fuel Quality for Fuel Cell Vehicles
2.4 Additional Document:
California Code of Regulations Title 4, Division 9, Chapter 6, Article 8, Sections 4180 – 4181
3. Terminology
3.1 Definitions—For definitions of general terms used in D03 Gaseous Fuels standards, refer to Terminology D4150.
3.2 Definitions:Definitions of Terms Specific to This Standard:
3.2.1 electron capture detector (ECD), n—detects organic halides by the reduction of a standing detector current due to the capture
of detector current electrons by the halogenated hydrocarbons.
3.1.2 fuel cell grade hydrogen, n—hydrogen satisfying the specifications in SAE J2719.
3.2.2 organic halide, n—any compound containing carbon and a halogen (fluorine, chlorine, bromine, or iodine).
3.2.3 total organic halides, n—the sum concentration of all compounds containing carbon and at least one halide (fluorine,
chlorine, bromine, or iodine).
3.3 Acronyms:
3.3.1 ECD—electron capture detector
3.3.2 GC—gas chromatograph
4. Summary of Screening Method
4.1 The screening of organic halides in hydrogen and other gaseous fuels can be challenging due to need to measure total organic
halides to 0.05 μmol50 ppb(v)⁄mol (50 ppb) to satisfy hydrogen fuel contaminant requirements specified in ISO TS 14687-2,
14687, SAE J2719, and the California Code of Regulations.
4.2 Organic halides, at any detectable concentration, are not normally present in hydrogen. Any contamination observed will be
due to improper maintenance or cleaning of equipment; therefore, any positive result should be cause for further testing and
evaluation.
4.3 A gas chromatograph (GC) equipped with an ECD detector and gas sampling system with a 1 mL sample loop is typically
used. The GC column is replaced by a length of blank tubing. Carrier gas and detector flows are set to manufacturer’s
specifications.
4.4 The sample gas is injected into the inlet of the GC-ECD system through the blank tubing and the ECD detector. A signal is
produced as organic halides pass though the detector. The signal is sent to a computer, integrator, or other recording device.
4.5 This standard is intended to provide a pass/fail test of presence of organic halides. Its use to rigorously quantify organic halides
in gaseous fuels has not been demonstrated. Some fuels may contain contaminates that would preclude the use of this method.
5. Significance and Use
5.1 Low operating temperature fuel cells such as proton exchange membrane fuel cells (PEFCs) require high purity hydrogen for
Available from International Organization for Standardization (ISO), ISO Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
Switzerland, http://www.iso.org.
Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale, PA 15096, http://www.sae.org.
Available from California Department of Food and Agriculture, 1220 N Street, Sacramento, CA 95814, https://www.cdfa.ca.gov.
D7676 − 23
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, 14687, SAE J2719, and the California Code of Regulations, or as specified in regulatory codes.
5.2 Although not intended for application to gases other than hydrogen, techniques within this screening method can be applied
to other gaseous samples requiring total halogenated hydrocarbon content determination. The method must be validated when used
to test fuels or other gaseous samples that may contain interfering compounds.
6. Interferences
6.1 Other Electron Capturing Sensitive Compounds, most notably oxygen, water, and other oxygen
...