Cyclic voltammetry is the most widely used technique acquiring qualitative information about electrochemical reactions. The power of cyclic voltammetry results from its ability to rapidally provide considerable information on the thermodynamics of redox processes, on the kinetics of the heterogeneous electron-transfer reactions, and on coupled chemical reactions or adsorption processes. Cyclic voltammetry is often the first experiment performed in an electro-analytical study. In particular, it offers rapid location redox potentials of electro-active species, and convenient evaluation of the effect of media upon the redox process. In our lab., we use Cyclic Voltammeter (CV) system (Fig. 1) for the electrochemical characterization of the thin film and nanostructured catalysts for our fuel-cell studies.