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In-Situ and Real-Time Monitoring of Oxygen Evolution during Kolbe Reaction by Scanning Electrochemical Microscopy

In this study, the oxygen evolution during the Kobe reaction was in-situ and real-time monitored by scanning electrochemical microscopy (SECM) in tip-generation substrate-collection (TG/SC) mode. A typical Kolbe reaction involving the acetate electro-oxidation was used as a study model. To this end, the TG/SC method of acetate electro-oxidation was performed at a 10 μm-diameter tip Pt disk microelectrode positioned ~1.2 μm away from a 50 μm-diameter substrate Pt disk microelectrode. The substrate Pt was employed as an efficient catalyst to monitor the byproduct O 2 produced at the tip by the catalytic reduction at an appropriate electrode potential. The linear scanning voltammetry (LSV) results indicated that O 2 evolution during acetate oxidation depended on both the electrode potential and acetate concentration. At low potentials (<2.4V vs. Ag/AgCl), the current of O 2 evolution dominated the acetate oxidation reaction in 0.1 M HClO 4 electrolyte, while O 2 evolution was inhibited at the joint condition of higher potentials (>2.4V) and elevated concentrations of acetate, resulting in better current efficiencies of acetate oxidation. The inhibition effect of O 2 evolution was also confirmed in alkaline electrolytes, consistent with the reported literature dealing with other traditional detection techniques. In sum, the proposed detection technique based on in-situ and real-time dynamic monitoring of oxygen evolution was accurate and sensitive, thereby promising for the study of broad range of reactions involving the generation of oxygen species.