Nano Pt particles were dispersed on carbon-based supports by a polyol process for a catalyst application in a polymer electrolyte fuel cell. We tried to optimize the effect of pH on the electrostatic forces between the support and the Pt colloids. We investigated the relationship among the surface charges on the carbon support, the solution pH, and the concentration of a glycolate, and the Pt particle size. The produced catalyst with nano Pt particles on the support was evaluated by the long-term cyclic voltammetry (CV) performance test and compared with the results from a commercial catalyst. Our experimental results reveal that the pH-control can modify the particle size distribution and the dispersion of the nano Pt particles. This resulted in a cost-effective method for the synthesis of highly Pt loaded Pt/C catalysts for fuel cells better than a commercial catalyst system.