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Flow Electrolyzer Mass Spectrometry with a Gas-Diffusion Electrode Design.

Bjorn Hasa1, Matthew Jouny1, Byung Hee Ko1

  • 1Center for Catalytic Science and Technology, Department of Chemical and Biomolecular Engineering, University of Delaware, Newark, DE, 19716, USA), and.

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Summary

A new flow electrolyzer mass spectrometry (FEMS) technique detects gas intermediates in electrochemical reactions at high current densities. This method elucidated the oxygen source in acetaldehyde formation during carbon monoxide reduction.

Keywords:
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Area of Science:

  • Electrochemistry
  • Analytical Chemistry
  • Catalysis

Background:

  • Operando mass spectrometry is crucial for studying catalyst surfaces in electrochemical systems.
  • Conventional methods struggle with gas reactants due to low solubility and limited current density.

Purpose of the Study:

  • To develop a novel technique for detecting reactive intermediates in gas-involved electrochemical reactions.
  • To investigate the electrochemical carbon monoxide reduction reaction (eCORR) mechanism on copper catalysts.

Main Methods:

  • Development of flow electrolyzer mass spectrometry (FEMS) using a gas-diffusion electrode.
  • High current density electrochemical experiments (>100 mA cm⁻²).
  • Isotopic labeling studies to trace oxygen origins.

Main Results:

  • FEMS successfully detected volatile/gaseous species at high current densities.
  • The oxygen in acetaldehyde intermediates during eCORR originates from the reactant CO.
  • Ethanol and n-propanol products primarily contained solvent oxygen.

Conclusions:

  • FEMS is a powerful tool for operando analysis of electrochemical reactions with gas reactants.
  • Direct experimental evidence for an isotopic scrambling mechanism in acetaldehyde formation was provided.
  • The findings offer new insights into the eCORR pathway and catalyst surface chemistry.