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Electron transfer (ET) from ascorbic acid (AA) in aqueous to ferrocene (Fc) in 1,2-dichloroethane (DCE) was probed by the scanning electrochemical microscopy (SECM). The rate constants were extracted from the dependence of the steady-state current at ultramicro- electrode (UME, tip) on the distance between the tip and the phase boundary by comparison to theoretical working cures.