Fuel cell technology offers clean, silent and robust sources of energy for our future needs. Among the five common,fuel cells widely been used, solid polymer electrolyte membrane fuel cell (SPEFC) gives more advantanges in many respects. It is able to generate power more efficiently for both vehicular and stationary in the range of 5 to 500 kW without causing pollution. It's operate at low temperature of 50degreesC at an efficiency of 50 to 60%. Furthermore, it can produce high current density even though it is operating at low temperature (the highest temperature is 90degreesC) and at the pressure of 600 kPa. It's source of fuel are hydrogen and oxygen, while discharge very small quantity of water as the product. In this work, the optimization of electrocatalyst for fuel cell electrode using various mixed oxide materials was carried out. The elucidation of active site species that contribute to the performance of the fuel cell was achieved using X-Ray Photoelectron Spectroscopy, X-ray Diffraction and Scanning Electron Microscopy techniques. The result of testing using laboratory scale fuel cell model reveals that the flow rate of fuel gases, the pretreatment of electrocatalysts and the composition of mixed oxide electrocatalysts, play important roles in determining the best performance of the working SPEFC fuel cell system.