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Ultrafast cyclic voltammetry was used to study the redox behavior of a gold electrode in acetonitrile. The direct electrochemical evidence of the dissociation and adsorption behavior of acetonitrile at gold electrodes was found. It could be stated that two consecutive redox paths are involved, each with a special adsorption state acting as the reaction intermediate. The mean value,obtained of the electron-transfer rate constant of the second path, was 1.3 × 105 s-1 with a standard deviation of 0.24 × 105 s-1.