Abstract
Triple-potential-step chronoamperometry (TPSCA) has been used to identify either the previously disputed or the unidentified anodic process that arises in the electroreduction of diazodiphenylmethane, diethyl diazomalonate, and fluorenone hydrazone. In each of the three systems, slow heterogeneous electron transfer at a platinum electrode in DMF-0.1 M (n-Bu) 4NClO 4 causes the separation between the anodic peak for the reoxidation of the unreacted anion radical of the starting material and the corresponding cathodic peak to exceed 0.7 V. The scope and limitations of the TPSCA method for a reaction scheme involving quasi-reversible heterogeneous electron transfer followed by an irreversible homogeneous chemical reaction are discussed.
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