Abstract: | The electrochemical oxidation of cobalt(II) at gold, boron‐doped diamond, basal and edge plane pyrolytic graphite, and highly oriented pyrolytic graphite electrodes in aqueous solutions containing NH3 has been studied using cyclic voltammetry, with subsequent chemical and electrochemical processes explained in detail. Furthermore, the electro‐reduction of Co(NH3)6]3+ in the presence of different electrolytes has also been studied to obtain a better understanding of the oxidation pathway of the Co(II)‐ammine complexes. In aqueous solution the mechanism can be described by the following scheme: |