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Electrochemical Synthesis of High-Value Chemicals: Detection of Key Reaction Intermediates and Products Combining Gas Chromatography–Mass Spectrometry and in Situ Infrared Spectroscopy

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journal contribution
posted on 03.05.2019, 00:00 by Bethan J. V. Davies, Matthias Arenz, Jan Rossmeisl, María Escudero-Escribano
Herein, we present a methodology for the combination of analytical techniques that allow for the detailed investigation of electrochemical interfaces for electrocatalytic synthesis reactions. We have focused our analysis on the electrosynthesis of dimethyl carbonate (DMC) by methanol carbonylation with a Pd electrocatalyst. DMC is a versatile chemical that could be produced electrochemically, rather than by traditional, energy intensive, and hazardous methods. The electrochemical and analytical techniques used are cyclic voltammetry, constant potential electrolysis, in situ spectroelectrochemistry, and quantitative chemical analysis by headspace gas chromatography–mass spectroscopy. The combination of techniques results in a thorough investigation of the activity, selectivity and efficiency of the process, showing that Pd produces DMC, but suffers from low activity, low selectivity, and low efficiency as well as poor stability. The method presented could be applied to the investigation of other electrochemical synthesis reactions.