The rotating disk electrode system is used for electrocatalysts’ performance testing. The experimental test bench consists of a three-electrode cell, a potentiostant, a Pt plate counter electrode and a reversible hydrogen reference electrode. Electrochemical active surface area of the developed electrocatalysts is measured in N₂ saturated HClO₄ solution using cyclic voltammetry method. Electrochemical performance of the developed electrocatalysts is studied in O₂ saturated HClO₄ solution to simulate the cathode side of PEMFC environment under operating conditions.