from the glove box into the reactor. Figure S2.9 illustrates the electrochemical set-up utilized in this study. For recording potentials versus Ag/Ag+, an Ag wire was used as the pseudo-reference electrode. 0.1 mol% Ag OTf in 0.1 mL anhydrous acetonitrile was always used as the reference solution and was separated from the working solution with an ASTM ultrafine frit. Working solutions always contained 0.5 mol% of the electrolyte and were all prepared inside the glove box. NTf2 was always used as the common electrolyte anion and anhydrous acetonitrile was the common solvent for all measurements. A graphite rod (99.99% Sigma Aldrich) was used as the counter electrode. Gas chromatography (Compact GC 4.0, Inter science) was used to analyze the gas products from the reactor. He was used as the carrier gas and the Pulsed Discharge Detector of the GC was calibrated for 1 to 100,000 ppm CO (Carbon Monoxide CP Grade N3.0, Linde). All electrochemical measurements were performed with a Biologic SP-300. RDE measurements were performed using a WaveVortex 10 Electrode Rotator (Pine research). Figure 2.2 illustrates the sensitivity of our non-aqueous setup to the presence of water. The figure showcases the LSV (Linear Sweep Voltammetry) results obtained from the Ni electrode under He purge, with varying levels of residual water concentration. Notably, the findings reveal a discernible increase in the reductive current upon the introduction of water into the system in the potential range of -1.0 to -1.5 V, lower than required for reduction of CO2. The reduction of H2O becomes mass transfer limited in the range of -1.5 V to -2.0 V. To ensure consistent hydrodynamics and minimize variations during linear sweep voltammetry (LSV) and electrolysis (EL) measurements, several parameters were kept constant. These parameters included maintaining a consistent reaction volume size, counter electrode size, and gas flow rate (5 ml/min). These measures were implemented to ensure reliable and meaningful comparisons of the apparent relative activities when studying different electrolytes or electrodes. Prior to any electrochemical measurement, it was ensured that a stable open-circuit
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