A composite cation exchange material acetonitrile stannic(IV) selenite was prepared under different experimental conditions. The ion exchange capacity of the material was improved from 0.75 to 1.83meq g-1 in comparison to its inorganic counterpart, stannic selenite. The material was characterized on the basis of X-ray, TGA, FTIR, and SEM studies. Ion-exchange capacity, pH titration, elution behavior, and distribution studies were also carried out to determine the preliminary ion-exchange properties of the material. Furthermore, it was investigated that this ion exchange material has a good reusability after 8 times regeneration. The sorption behavior of metal ions was studied in nonionic surfactants namely triton x-100 and tween. On the basis of distribution coefficient studies, several binary separations of metal ions viz- Pb2+-Th4+, Ni2+-Th4+, Ni2+-Zn2+, Cu2+-Ce4+, Al3+-Bi3+, and Al3+Zn2+ was achieved on the packed column of this ion exchange material. The practical applicability of this cation-exchanger was demonstrated in the separation of Th4+ from a synthetic mixture of Th4+, Ca2+, Sr2+, Ni2+, and Mg2+ as well as Cu2+ and Zn2+ from a brass alloy sample. Thus, all the studies suggest that acetonitrile stannic(IV) selenite has excellent potential for the removal of metal ionic pollutant species from aqueous media effectively.