A new hybrid inorganic-organic cation exchanger acrylamide zirconium (IV) arsenate has been synthesized, characterized and its analytical application explored. The effect of experimental parameters Such as mixing ratio of reagents, temperature, and pH on the properties of material has been studied. FTIR, TGA, X-ray, UV-vis spectrophotometry, SEM and elemental analysis were used to determine the physiochemical properties of this hybrid ion exchanger. The material behaves as a monofunctional acid with ion-exchange capacity of 1.65 meq/g for Na+ ions. The chemical stability data reveals that the exchanger is quite stable in mineral acids, bases and fairly stable in organic solvents, while as thermal analysis shows that the material retain 84% of its ion-exchange capacity up to 600 C. Adsorption behavior of metal ions in solvents with increasing dielectric constant has also been explored. The sorption studies reveal that the material is selective for Pb2+ ions. The analytical utility of the material has been explored by achieving some binary separations of metal ions on its column. Pb2+ has been selectively removed from synthetic mixtures containing Mg2+, Ca2+, Sr2+, Zn2+ and Cu2+, Al3+, Ni2+, Fe3+. In order to demonstrate practical utility of the material quantitative separation of the Cu2+ and Zn2+ in brass sample has been achieved on its columns. (c) 2008 Elsevier B.V. All rights reserved.