Proceedings of MATSUS Fall 2023 Conference (MATSUSFall23)
DOI: https://doi.org/10.29363/nanoge.matsus.2023.169
Publication date: 18th July 2023
Gaining a deep understanding of the factors governing electrocatalytic reactions requires reliable measurement of the identity and amount of the products generated at the electrode as a function of electrochemical parameters. Detecting these products in real-time enables the observation of otherwise inaccessible, fast and transient phenomena. Coupling mass spectrometry (MS) with electrochemistry (EC) allows for real-time detection with outstanding sensitivity. Several methods have been employed in the monitoring of volatile products: Differential Electrochemical Mass Spectrometry (DEMS) [1] and On-line Electrochemical Mass Spectrometry (OLEMS) [2] have been used successfully to study reaction mechanisms of aqueous systems. Similarly, Online Electrochemical Mass Spectrometry (OEMS) [3] has helped improve our understanding of gas evolution in batteries.
To fully exploit the potential of coupled EC-MS, it is of importance to be able to quantify the amounts of products evolved to accurately relate these amounts to the electrochemical charge passed. To this end, calibration of the MS signals is required. In aqueous systems, MS calibration for some important analytes can be carried out by generating the analyte electrochemically on a catalyst yielding this analyte at close to 100 % faradaic efficiency. Nonetheless, this approach is limited to few analytes, and is especially challenging in non-aqueous systems.
In this contribution, we show how a simple gas-based procedure using chip-based Electrochemistry-Mass Spectrometry (EC-MS) can be used for calibration of electrochemically accessible analytes such as hydrogen and oxygen in aqueous systems. We then demonstrate how we can extend this procedure to analytes not accessible via electrochemical calibration, as well as to non-aqueous electrolytes. We illustrate how quantitative chip-based EC-MS can be used for the identification of surface adsorbates in electrochemical oxidation reactions, and consequently aid in elucidating the role of these species in steering selectivity. [4,5] Finally, we attest the method’s usefulness in non-aqueous systems for studying electrocatalytic reactions such as nitrogen reduction, as well as gas evolution in Li-ion batteries.
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