A new crystalline Inorganic ion exchanger, stannic vanadophosphate, has been synthesized by treating vanadophosphorlc acid with stannic chloride (sample 1). When 0.1 M solutions of sodium orthophosphate, sodium metavanadate, and stannic chloride are mixed in the volume ratio of 4:1:1, the amorphous stannic vanadophosphate (sample 2) is obtained. A comparative study of samples 1 and 2 has been made with respect to their ion-exchange behavior, the ir and x-ray spectra and values. Three binary separations (I) ln3+-Ga3+, (II) Mg2+-Ca2+, and (III) Mn2+-Ni2+ have been achieved using sample 11n the column. In3+, Mg2+, and Mn2+ were removed with water, Ga3+ with 0.1 HN03 while Ca2+ and Nl2+ were eluted with 1 % NH4N03.