Abstract
Scanning electrochemical microscopy (SECM) was employed to study the rate of the second-order homogeneous reaction of a species electrogenerated at an ultramicroelectrode tip. Oxidation of 4-nitrophenolate in acetonitrile to the phenoxy1 radical took place at a gold ultramicroelectrode (5-pm diameter) held in close proximity to a larger substrate electrode that detected the tip-generated species. A radical dimerization rate constant of 1.2 (*0.3) X 108 M-' s-I was determined. Approximate analytical equations for the treatment of irreversible kinetics following electron transfer were developed to simplify the analysis of feedback and collection data for both first- and second-order reactions. The effect of possible interference by the reference material added to allow precise determination of the tipsubstrate spacing (benzoquinone or ferrocene) was also investigated.
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