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• A new DEMS system incorporating microreactor and ion-exchange membrane was constructed. • The constructed DEMS system can quantitatively analyze CO 2 evolution reactions of catalyst-loaded carbon electrodes in alkaline electrolyte solutions. • The corrosion behavior of a Pt-loaded carbon is similar to that in the acidic electrolytes except for the onset of the carbon corrosion. • La 0.6 Ca 0.4 CoO 3 and Ca 2 FeCoO 5 show electrochemical carbon corrosion activity, while La 0.4 Sr 0.6 MnO 3 does not show distinct electrochemical carbon corrosion activity. CO 2 evolution is involved in various main and side reactions of electrochemical systems, such as carbon corrosion reactions and alcohol oxidation reactions. Differential electrochemical mass spectroscopy (DEMS) has been intensively applied to analyze the partial current of the CO 2 evolution reaction in acidic and neutral electrolyte solutions. However, the quantitative analysis of the CO 2 evolution reaction in alkaline electrolyte solutions has not been successful when catalyst-loaded carbon electrodes were applied, due to the high solubility of CO 2 in the electrolyte. In this study, we develop a new DEMS system combining microreactor and ion exchange membrane to quantitatively analyze CO 2 evolution reactions of catalyst-loaded carbon electrodes in alkaline electrolyte solutions. The calibration constant, which correlates the mass signal of m / z = 44 to the partial current of the CO 2 evolution reaction, is successfully obtained from the Faradaic current and the mass signal of CO stripping voltammetry. We analyze carbon corrosion reactions of Pt and metal oxide-loaded carbon electrodes to demonstrate the effectiveness of the constructed system. The corrosion behavior of the Pt-loaded carbon is similar to that in the acidic electrolytes except for the onset potential of the carbon corrosion. La 0.6 Ca 0.4 CoO 3 and Ca 2 FeCoO 5 show electrochemical carbon corrosion activity, while La 0.4 Sr 0.6 MnO 3 does not show distinct electrochemical carbon corrosion activity.
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Ikezawa et al. (2023) studied this question.
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