In this study, electrochemical and spectroscopic characterization of home-made CeO2, activated carbon-based Ag-Cu electro-catalysts, and preliminary anode polarization results in a direct ethanol fuel cell test system were presented. Ag-Cu transition metal couples were impregnated onto carbon and cerium oxide supports by wet impregnation, ion exchange, and co-precipitation techniques. Wet impregnation technique was selected for further spectroscopic analysis and fuel cell testing due to its easy metal loading advantage and highest peak currents in ethanol-containing electrolyte environment. When Ag and Cu were loaded 37.5 and 12.5 wt.% onto carbon and cerium oxide by wet impregnation technique, XPS analysis indicated an appreciable amount of Ag and Ag2O and a high amount of CuO. In cerium oxide-based samples atomic percentage of oxygen fits well with the stoichiometry of CuO/CeO2. Preliminary results show that BET surface area and the current peaks exhibit a close resemblance (highest BET surface area indicates highest anodic dissolution current), which is thought to be due to the high accessibility of copper layers impregnated onto cerium oxide and activated carbon in H2SO4 electrolyte environment. Hydrogen reduction of CeO2-based samples prepared by wet impregnation at 750 degrees C greatly improved anode polarization and onset oxidation potential.