The effects of three synthesis variables on the electrochemical properties of TiO2 prepared by the Pechini method are described. To minimize the number of experiments, a factorial design was used. It was shown that, in the presence of nitrobenzene, the temperature and the number of layers were the most important variables. The effects of these variables on the cathodic charges measured by cyclic voltammetry were -0.75 and 2.76 mC cm(-2), respectively. Explanations of these findings are based on the effect of the conditions of preparation on the morphology and microstructure of the electrodes.