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The charge transfer processes across the interface between two immiscible electrolyte solutions (ITIES) can be employed for energy storage and conversion, solvent extraction, or sensing or in life sciences. Among them are catalytic reactions, which have only been recently studied. Here H₂O₂ generation is studied with decamethylferrocene (DMFc) as electron donor at the interface between tetrahexylammonium perchlorate solution in 1,2-dichloroethane (1,2-DCE) and aqueous HClO₄. These conditions are unfavorable for proton transfer across ITIES because of positive Galvani potential difference. Voltammetry with 1,2-DCE droplet modified electrode shows that DMFc oxidation is accompanied by ClO₄^– insertion into the organic phase. The reaction progress was followed by UV–vis spectroscopy, voltammetry, and scanning electrochemical microscopy (SECM). In the first and last method, horseradish peroxidase …