Abstract
Electrochemical CO2 reduction (CO2RR) is a promising way to convert CO2 emissions into sustainable fuels and chemicals, approaching a circular carbon economy. 1 Depending on catalyst type and reaction conditions, different gaseous and liquid products can be obtained from the CO2RR, and their production rates vary with reaction time. Thus, assessing the product distribution online during CO2RR is a key component of any catalytic performance analysis. 2,3 However, while gaseous products are readily analyzed online, liquid products are assessed typically only at the end of the reaction due to the lack of suitable automated liquid sampling and analysis methods. In addition, electrolyzer parameters such as gas flow rates, temperatures and pressures are seldom recorded, causing the loss of significant information on catalysts, electrodes, and electrolyzers behavior.To overcome these issues, we assemble a comprehensive analytical system coupling online gas and liquid product analysis by chromatography (leveraging a special automated liquid sampling valve) with electrochemical protocols to assess CO2RR performance, electrolyzer cell resistance and electrode surface area. In addition, we record CO2 gas flow rates, electrolyzer temperatures, and gas and liquid pressures. 4 To rapidly and reproducibly handle the large and heterogeneous data volume obtained we implement a standardized data pipeline based on our own open-source software,5 which automatically parses the numerous different raw data files, composes a data set following FAIR practices,6 and post-processes and plots the data in a standardized way (see example in Fig. 1 below). We validate the analytical system by carrying out CO2RR at 200 mA/cm2 on Cu gas diffusion electrodes, following the changes in selectivity with reaction time for > 10 gaseous and liquid products, and recording mass flow rates, electrolyzer temperatures and pressures. The modular nature of our analytical system, combined with the standardized data pipeline, allows us to freely increase the number and type of sensors used with minimal impact on the data analysis time, as well as to multiplex our analysis to parallel electrolyzer cells, paving the way for a much deeper and faster understanding of the function of CO2RR catalysts, electrodes, and electrolyzers.
Published Version
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