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Hydrogen or hydrogen peroxide can be generated in liquid–liquid biphasic systems, where the organic phase contains sufficiently strong electron donor (whose redox potential is lower than the potential of reversible hydrogen electrode). H₂O₂ generation with acidified aqueous phase occurs prior to H₂ evolution when oxygen is present. No other organic solvent than highly toxic 1,2-dichloroethane (DCE) has been reported in biphasic system for H₂ or H₂O₂ generation. In this work, we have used trifluorotoluene (TFT) instead of carcinogenic DCE, and studied these reactions in TFT–water biphasic system. To evaluate H₂ flux, scanning electrochemical microscopy potentiometric approach curves to the TFT–water interface were recorded. H₂O₂ was detected voltametrically at a microelectrode located in the vicinity of the interface. H₂ and H₂O₂ are formed and both reactions occur also in the absence of a …