In this research NiFe2O4 nano crystals were synthesized and modified by 2-acrylamido-2-methylpropanesulfonic acid (AMPS). FE-SEM analysis proved the successful production of the NiFe2O4/ AMPS nanocomposites. Heterogeneous polyvinyl chloride (PVC) based cation exchange membranes were modified by NiFe2O4 / AMPS. Sodium flux of the modified membranes had an increasing trend and sample 2 (containing 1.0 % wt. NiFe2O4 / AMPS) had 17.5% improvement for ionic flux. Prepared membrane containing 1.0 % nanocomposites could separate Pb2+ (98%), Cu2+ (48%), Ni2+ (34%). The membrane current efficiency in Pb2+ removal was higher than 70%.