A design of experiments (derived from the Taguchi method) was implemented to optimize experimental conditions of a surfactant free polyol method for the synthesis of PtCo electrocatalysts Considered responses were the active Surface area and the catalytic activity toward oxygen reduction reaction Metallic salt concentration, pH. temperature ramp. addition order of reactants and particle cleaning step were chosen as main parameters according to considerations coming from literature and previous experiments Matrix models describing the behaviour of the synthesis system was elaborated taking into account the effects of each considered parameter and their interactions From this model, an optimized PtCo/C catalyst, in terms of active Surface area and activity towards the oxygen reduction reaction, was synthesized Both the measured values of the active Surface area and the electrocatalytic activity are in very good agreement with the calculated ones from the matrix model Furthermore, actions of parameters and interactions between parameters can be better understood using this method (C) 2009 Elsevier B.V All rights reserved