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The electrochemical reduction of benzene on a smooth Pt electrode has been studied by confocal microprobe Raman spectroscopy. The results show that benzene can be reduced directly to cyclohexane, which is insoluble in water, adhered onto the electrode surface to form the third phase. After the drops have been formed on the electrode surface, the relative concentration of benzene to cyclohexane in the drops will rather increase with prolonging the time at a certain electrode potential, although it decreases with the negative shift of the electrode potential at first.