Hybridization technique provides overall up gradation owing to the combination of two or more processes and system demonstration provides the confidence in operation particularly related to nuclear plant generated waste effluent treatment (NPGWET). Here, NPGWET has been envisaged as a three stage process (a) Polymer Complexation, (b) Ultrafiltration (UF), and (c) Resin bed treatment. This concept was applied effectively by using a 20L lab scale experimental capacity set–up. In complexation stage, with 1% polyethylene imine (PEI) aqueous solution and 0.5% total metal ions [that includes Uranium (U) 10 ppm, Cu 80 ppm Fe 35 ppm Mg 560 ppm Gd 2 ppm etc, pH-7.8] has been passed through UF membrane unit followed by a polyacrylamidehydroxamate (PAH) resin bed, where outlet “U” concentration was found below 10 ppb. The Iron (Fe) and Fe+U loaded metal ions samples were characterized by XRD and Mössbauer spectroscopy techniques.