An advanced cation-exchange nano-composite poly-o-toluidine Ce(IV) phosphate was synthesized by sol-gel technique by incorporating Ce(IV) phosphate precipitate with the matrix of poly-o-toluidine. The material showed good ion-exchange behavior and used successfully in separation of metal ions. The conductivity of the composite was found within the range of 10(-2) to 10(-3) S/cm(-1); measured by four-in-line probe DC electrical conductivity measuring technique. The conductivity is at the border of metallic and semiconductor region. Ion-exchange kinetics for few divalent metal ions was evaluated by particle diffusion-controlled ion-exchange phenomenon at four different temperatures. The particle diffusion mechanism is confirmed by the linear tau (dimensionless time parameter) versus t (time) plots. The exchange processes thus controlled by the diffusion within the exchanger particle for the systems studies herein. Some physical parameters like self-diffusion coefficient (D (0)), energy of activation (E (a)), and entropy of activation (a dagger SA degrees) have been evaluated under conditions favoring a particle diffusion-controlled mechanism.