A novel Polyaniline based hybrid cation exchange material has been synthesized by the simple sol-gel method. FTIR, TGA/DTA, XRD, SEM, and TEM have been done for characterization of the material. The preliminary study of the physicochemical properties (ion exchange capacity, pH titrations, effect of concentration and effect of temperatures etc.) was also carried out. The synthesized material has been favored by reproducible and granulometric nature. The material was found to be fairly stable in dilute solution of common acids, bases and most of the organic solvents. On the basis of distribution coefficients (K-d values), the material has been found suitable for some important quantitative binary separations (e.g. Cd2+-Pb2+, Zn(2+)pb(2+), Er3+-Pb2+, Zn2+-Al3+, Cu2+-Al3+) on its columns. The limits of detection and quantification for Pb2+ ions were found to be 0.54 mu g L-1 and 1.8 mu g L-1 respectively. The electrical conductivity of the material was found to be in semiconductor region (10(-4) to 10(-3) S Cm-1). Based on experimental observations it was found to be suitable for the separation and determination of metal pollutants in water samples. The practical utility of the material has been established by the removal of Pb2+ ion from industrial wastewater. (C) 2014 Elsevier B.V. All rights reserved.