Solid ZrOCl2·8H2O was added in a slow stream to a solution of phosphoric acid or to a solution of TiCl4 in phosphoric acid to obtain granules of amorphous Zr(HPO4)2·nH2O or ZrxTi(1–x) (HPO4)2·nH2O(where x=0.95–0.80). Half of each product had been soaked in ethanol to produce alcohol solvated materials. It was found that the particle size of the resulting materials is very similar to that of ZrOCl2·8H2O, in such a way that it may be controlled indirectly. These materials are suitable for ion-exchange column operations. The relatively high gamma radiation doses of60Co source did not alter its exchange properties. pH-titrations were performed by an automatic titrimeter and the exchange capacities of alkali metal ions were determined by isotopic tracer technique. Effect of drying temperature on the ion exchange properties of Na+, K+ and Cs+ on the granular materials have been studied. Other characterizations were made by usual chemical analysis and thermography.