ABSTRACT. Oxidation-reduction cycling (ORC) procedures are widely used for cleaning nanoparticle surfaces when investigating their electrocatalytic activities. In this work, the effect of ORC on the surface structures and electrocatalytic oxygen reduction activity of Au electrodes is analyzed. Different structural changes and variations in electrocatalysis are observed depending on the initial structure of the Au electrodes, such as flat bulk, nanoporous, nanoplate, or dendritic Au. In particular, dendritic Au structures lost their sharp-edge morphology during the ORC process, resulting in a significant decrease in its electrocatalytic oxygen reduction activity. The results shown in this paper provide an insight into the pretreatment of nanoparticle-based electrodes during investigation of their electrocatalytic activities.