A rotating cylinder‐collector electrode (RCCE) for the study of electrochemical processes that involve electroactive intermediates and/or products is described. Calibrations of the collector efficiencies for both major and minor sectors have been performed using the ferri/ferrocyanide redox couple over a wide range of rotational velocity (225–3060 rpm). With the minor sector as the collector, a collection efficiency of ∼7.2% was observed, and was found to be independent of rotational velocity over the range considered. However, the collection efficiency increased to ∼67% when the major sector was used as the collector, thereby indicating that the RCCE is a sensitive device for the detection of dissolved electroactive species. The utility of this electrode is illustrated by investigating the anodic behavior of copper and nickel in hydroxide solution at various temperatures between 0° and 80°C.
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