An electrolyte-probe screening method was proposed for combinatorial electrochemical analysis, which is not only suitable for half-cell but also for full-cell electrochemical research. The accuracy of this method was examined by investigating the electrochemical oxidation of methanol in an electrode array for various methanol I air cells. Reproducible voltage-current curves were obtained for various parallel experiments in the same electrode array. The effects of catalyst loading and methanol concentration on the discharge performance for the methanol I air cells were observed by fast screening the anode electrodes in the array containing different catalyst loadings and various methanol concentrations, respectively.