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Controlled-potential coulometry, also known as potentiostatic coulometry, employs a three-electrode system in which the working electrode's potential is precisely regulated using a potentiostat. Platinum working electrodes are utilized for positive potentials, while mercury pool electrodes are favored for extremely negative potentials. The platinum counter electrode is separated from the analyte using a membrane or salt bridge to avoid interference in the analysis.
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Interfacial electrochemical methods focus on the phenomena occurring at the boundary between an electrode and a solution, as opposed to bulk methods that concentrate on the solution's overall properties. These interfacial methods are classified as either static or dynamic based on the presence of a nonzero current in the electrochemical cell and the consistency of analyte concentrations. Static methods, such as potentiometry, measure the cell's potential without any significant current...
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Operando Impedance Spectroscopy Informed Dynamic Internal Resistance Compensation Mitigates Bubble-Induced

Blaž Tomc1,2, Miha Hotko1,2, Aleš Marsel1,3

  • 1Laboratory for Electrocatalysis, Department of Materials Chemistry, National Institute of Chemistry, Ljubljana 1000, Slovenia.

ACS Electrochemistry
|December 10, 2025
PubMed
Summary

This study introduces dynamic internal resistance (IR) compensation to accurately measure catalyst performance during gas-evolving electrochemical reactions. This real-time, self-correcting approach overcomes bubble interference for reliable electrochemical CO2 reduction studies.

Keywords:
IR compensationbubbleselectrochemical CO2 reductionelectrochemical impedance spectroscopyoperandostability

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Area of Science:

  • Electrochemistry
  • Materials Science
  • Chemical Engineering

Background:

  • Gas bubble formation during electrochemical reactions hinders precise potential control.
  • Conventional methods like surface engineering or cell design have limitations in managing bubble-induced artifacts.
  • Accurate catalyst performance evaluation is crucial for advancing electrochemical CO2 reduction (ECO2R).

Purpose of the Study:

  • To develop a dynamic internal resistance (IR) compensation method for real-time adaptation to bubble fluctuations.
  • To enable accurate assessment of catalyst performance and stability during gas-evolving reactions.
  • To improve mechanistic insight into catalyst degradation during ECO2R.

Main Methods:

  • Implemented operando electrochemical impedance spectroscopy (EIS) for continuous electrolyte resistance (ROhm) measurement.
  • Developed a Python control loop to extract EIS data and dynamically adjust IR compensation.
  • Applied the dynamic IR compensation approach to electrochemical CO2 reduction (ECO2R) on copper catalysts.

Main Results:

  • Effectively suppressed bubble-induced artifacts, ensuring stable potential control.
  • Enabled accurate and reliable performance evaluation of copper catalysts during prolonged ECO2R.
  • Facilitated reliable assessment of catalyst instability under realistic operating conditions.

Conclusions:

  • Dynamic IR compensation is essential for accurate catalyst evaluation in gas-evolving electrochemical reactions.
  • This self-correcting approach enhances the reliability of ECO2R stability studies.
  • The method provides crucial mechanistic insights into catalyst degradation by mitigating potential shifts.