with a consistent Faradaic efficiency for CO production. Figure S2.8 further supports the influence of the counter electrode choice. It displays images of an Au voltammetry electrode before and after conducting linear sweep voltammetry (LSV) experiments for CO2 reduction, with Ag employed as the counter electrode. The deposition of silver on the Au electrode during the experiment results in a noticeable transformation, resembling the appearance of silverish. However, when using graphite as the counter electrode, no significant changes in the electrode's appearance are observed after the voltammetry experiments. These observations emphasize the importance of selecting the appropriate counter electrode material in non-aqueous electrochemical CO2 reduction studies to minimize unwanted side reactions and artifacts. Glassware to prepare electrolyte solutions. All glassware intended for solution preparation underwent a thorough cleaning process. Firstly, the glassware was sonicated in Milli-Q water for a duration of 10 minutes. Following that, a subsequent round of sonication was conducted using ethanol for an additional 10 minutes. This ensured the removal of impurities or residues from the glass surfaces, ensuring a clean environment for solution preparation. After the cleaning process, the glassware was dried at a temperature of 200 degrees Celsius for a minimum of 2 hours, immediately transferred to the glove box antechamber while hot, where Figure 2.1. Chronoamperometry results for Au electrode under CO2 purging with 0.5 mol% of MM NTf2 as electrolyte in anhydrous acetonitrile. (a) with Au and Ag as counter electrode. and (b) with graphite as counter electrode. Both experiments were performed at -1.8 V vs. Ag/Ag+. The higher current observed for the experiment with graphite is due to the larger size of the working electrode (Au foil). a b
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