A B S T R AC TIn the present endeavour, zirconium amino tris(methylenephosphonic acid) (ZrATMP)-a novel hybrid ion exchange material of the class of tetravalent metal acid (TMA) salts has been synthesized by sol gel method. Physico-chemical and instrumental methods of analysis [Elemental analysis (ICP-AES, CHN analysis), FTIR, TGA, XRD and SEM] have been used to characterize the material. Cation exchange capacity (CEC) has been determined and the distribution behaviour of metal ions Co 2+ , Ni 2+ , Cu 2+ , Zn 2+ , Cd 2+ , Hg 2+ , Pb 2+ , Ce 3+ and Th 4+ in aqueous and various electrolyte media/concentrations determined and confi rmed with breakthrough capacity values.