The surface crystal structures of polycrystalline electrodes that are not stable and the difficulties in obtaining reproducible results lead to several difficulties in working with such electrodes. For this reason especially in the recent years intensive search is being carried out. For this goal noble metal platinum is especially selected because of its high electrocatalytic effect. But obtaining single crystal surfaces and preparing electrode from these surfaces turn out to be difficult. During the thermal procedure, surface changes and due to the pretreatment that are adapted different current-potential curves are obtained. In this review by giving the preparation methods of single crystal platinum and gold electrodes voltammetric studies have been explained with these electrodes.