Two different synthesis approaches were utilized with the ambition for the development of efficient and cost effective adsorbents. These methods were simultaneous radiation grafting and emulsion graft polymerization. Poly(acrylonitrile) grafted sepiolite nanohybrid (MS-g-PANγ) has been synthesized using acrylonitrile via simultaneous radiation grafting. The grafting yield was measured by varying the absorbed dose, dose rate and monomer concentration. The acrylonitrile group was chemically modified into amidoxime (MS-g-aoPANγ). The structural and morphological investigations of these nanohybrids were performed by Fourier transform infrared (FT-IR), x-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). Batch adsorption studies were carried out for copper uptake onto amidoximated nanohybrid adsorbents to envisage the effects of pH, adsorbent dose, contact time and initial concentration. Equilibrium was attained within 30 minutes following pseudo-second order kinetics and was well described by the Langmuir isotherm model. The maximum adsorption capacity was found to be 278 mg/g for 5 kGy sample. This environmental friendly and cost effective adsorbent can be used for the removal of copper ion. Same technique was exploited for the synthesis of sepiolite-g-polystyrene nanohybrid (MS-g-PSγ) using Co-60 irradiator in the presence of dichloromethane (DCM) under nitrogen atmosphere and room temperature. The grafting yield was affected by absorbed dose and monomer concentration in the mixture. Sulfonation of synthesized nanohybrid (MS-g-sPSγ) was carried out with sulfuric acid. Both the grafting of styrene and its sulfonation were verified by FT-IR, XRD and FESEM. The gravimetric investigations showed that grafting increased with the absorbed dose. Results showed that the system allowed successful grafting of styrene onto modified sepiolite. Sepiolite-g-polyacrylonitrile nanocomposites (MS-g-PAN) were also synthesized using emulsion graft polymerization. The influence of synthesis parameters (concentrations of monomer, initiator and surfactant) on grafting yield was studied. The nitrile group was chemically modified into amidoxime (MS-g-aoPAN). Maximum grafting of 373% was achieved at 5% acrylonitrile, 1% surfactant and 0.1% initiator xvii concentrations. The structural and morphological changes were observed by FT-IR, XRD, FESEM and TEM. Similar technique was applied for the synthesis of sepiolite-g-polystyrene nanocomposites (MS-g-PS) using styrene. Maximum grafting of 85% was achieved at 3% styrene concentration (w/v). FT-IR, XRD and FESEM confirmed the presence of polystyrene grafts but grafting yield was low (85%). So it can be established that radiation grafting is better route for the synthesis of sepiolite-g-polystyrene nanocomposites as compared to emulsion graft polymerization. The intention of this project was to develop organic-inorganic nanohybrid materials having the aptitude to adsorb toxic metals from waste water. The ambition was successfully achieved by adopting two routes of synthesis i.e. radiation grafting and emulsion graft polymerization.