A.II. Experiments with frit between anolyte and catholyte A supplementary experiment was conducted using a graphite electrode contained within a capillary tube, isolated from the catholyte by a glass frit. Figure A.II.1(left) showcases the initial setup of the cell before electrolysis, while Figure A.II.1 (right) depicts the same cell after undergoing 30 minutes of electrolysis. Evidently, the experiment exhibited significant degradation and subsequent deposition of graphite at the frit. Despite this degradation, CO continued to be produced with a high faradaic efficiency from the catholyte. However, the deposition of graphite led to the termination of the experiment within 30 minutes. Interestingly, this form of degradation was not observed in our standard experiments where the catholyte and anolyte were not separated. This observation suggests that, in our conventional setup, the CO2 reduction reaction facilitates the reactants required for the oxidation reaction. As no other discernible product was identified, and in light of our ATR-FTIR study in Chapter 6, we propose the involvement of carbonate as an oxygen carrier in this reaction. Figure A.II.1. Images of the reactor before (left) and after (right) electrolysis with 0.5 molar MM NTf2 in dry anhydrous acetonitrile. The working electrode is Au wire, and the counter electrode is graphite. The counter electrode is separated from the catholyte with a frit.
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