This paper presents a methodology of dynamic optimization and optimal control of a batch electrochemical reactor where a series of two reactions A reversible arrow B reversible arrow D takes place. The optimization problem is stated as to determine the optimal profiles of the electrode potential which maximize the selectivity of product B, in a given batch period and under specified constraints. The main important steps which are worth to be analyzed prior to any on-line implementation are presented and discussed. Thus, after the formulation of the optimization problem, different dynamic optimization methods have been used for the determination of optimal time-varying profiles of electrode potential. These profiles were then compared to the best uniform operations through the relative improvements of the performance index. The sensitivity analysis of the optimization criterion and control variables to the model parameters was carried out before state observation and implementation of optimal control profiles.