A novel hybrid cation exchange material of the class of tetravalent metal acid (TMA) salt, titanium diethylene triamine pentamethylene phosphonate (TiDETPMP) has been synthesized by the sol gel method. The material has been analyzed by spectroscopy and thermal methods. Physico-chemical and ion exchange characteristics have also been studied. The distribution coefficient (Kd) has been determined in aqueous as well as various electrolyte media/concentrations for Co2+, Ni2+, Cu2+, Zn2+ (transition metal ions) and Cd2+, Hg2+, Pb2+, Bi3+ (heavy metal ions) using TiDETPMP. Based on the differential affinity/selectivity, the breakthrough capacity (BTC) and elution behavior of various metal ions towards TiDETPMP, a few binary and ternary metal ions separations have been carried out.