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Although electron transfer reactions at liquid–liquid interfaces have been thoroughly studied in the presence of deliberately added potential determining ions or phase transfer catalysts, little is known about these reactions in the absence of the above species. Here, we report the formation of hydrogen peroxide (H₂O₂) in a liquid–liquid two-phase system with only an electron donor (decamethylferrocene) solution in trifluorotoluene (TFT) and a proton donor solution (HClO₄) in water. To detect H₂O₂, we used fluorescent microscopy and scanning electrochemical microscopy (SECM). We applied a potential sweep program to the SECM probe to overcome the electrode deactivation. To provide insight into the reaction rate and mechanism, we fitted SECM results to finite elements simulations. From the results of UV–vis spectroscopy, we determined a H₂O₂ partition coefficient of 0.03 and the standard Gibbs energy of H …