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Measuring Dissolved Methane in Aquatic Ecosystems Using An Optical Spectroscopy Gas Analyzer
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In-Line Combustion System for the Measurement of δ13C-CH4 in Gas Reference Materials Using Optical Isotope Ratio

Aimee Hillier1, Eric Mussell-Webber1, Emily Hopkinson1

  • 1National Physical Laboratory, Hampton Road, Teddington, Middlesex TW11 0LW, U.K.

Analytical Chemistry
|June 9, 2025
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Accurate stable carbon isotope ratio measurements of methane (δ13C-CH4) are crucial for tracking emissions. This study presents a reliable method using combustion and optical isotope ratio spectroscopy for certifying δ13C-CH4 in air reference materials.

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Area of Science:

  • Environmental Science
  • Analytical Chemistry
  • Atmospheric Science

Background:

  • Stable carbon isotope ratios in methane (δ13C-CH4) are vital for identifying methane emission sources.
  • Accurate and reproducible reference materials are essential for global atmospheric monitoring networks.
  • Existing methods require reliable calibration standards for precise δ13C-CH4 determination.

Purpose of the Study:

  • To develop and validate a method for certifying the δ13C-CH4 of methane in synthetic air reference materials.
  • To ensure traceability to the Vienna Pee Dee Belemnite (VPDB) scale for accurate atmospheric measurements.
  • To establish high reproducibility for δ13C-CH4 measurements in air reference materials.

Main Methods:

  • Methane (CH4) in synthetic air reference materials was converted to carbon dioxide (CO2) via direct combustion.
  • The δ13C-CO2 of the combustion product was analyzed using optical isotope ratio spectroscopy (OIRS).
  • Measurements were performed against CO2 reference materials traceable to the δ13CVPDB scale.

Main Results:

  • Four reference materials with distinct δ13C-CH4 values (-39.07‰ and -51.91‰) were certified.
  • Measurement reproducibility within 0.17‰ was achieved between paired reference materials.
  • Combined expanded uncertainties (k=2) ranged from 0.4‰ to 1.5‰, with negligible flow rate sensitivity.

Conclusions:

  • The combustion system coupled with OIRS provides a robust method for measuring δ13C-CH4.
  • This method enables the certification of δ13C-CH4 in air reference materials traceable to the VPDB scale.
  • The developed technique supports accurate atmospheric monitoring and source attribution of methane emissions.