This thesis consists of two research problems in the water decontamination area. In the first work, the main focus is to understand the structure and photocatalytic activity of titanium dioxide with graphene (G-TiO2) which is synthesized by using sol-gel method. The photocatalytic activity of TiO2 is limited by the short electron hole pair recombination time. Graphene, with high specific surface area and unique electronic properties, can be used as a good support for TiO2 to enhance the photocatalytic activity. The obtained G-TiO2 photocatalysts has been characterized by X-Ray Diffraction (XRD), Raman Spectroscopy, Transmission Electron Microscopy (TEM), FTIR Spectroscopy and Ultraviolet visible (UV-vis) Spectroscopy. This prepared G-TiO2 nanocomposite exhibited excellent photocatalysis degradation on methyl orange (MO) under irradiation of simulated sunlight. Such enthralling photocatalyst may find substantial applications in various fields. The primary objective of the second work is to understand the nanocomposite structure of SiO2 coated over graphene (G) nanoplatelets. An attempt has been made to synthesize G-SiO2 nanocomposite using sol-gel technique. The G-SiO2 nanocomposite is characterized using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Raman spectroscopy, FTIR spectroscopy, and Electrochemical and Electrical measurement technique, respectively. In this work, G-SiO2 nanoparticles with the water containing salts of zinc is added, and allowed to settle in water. The ZnCl2 ix concentration displays a whitish color solution which has turned to colorless within one or two hours of treatment with G-SiO2 nanocomposites. The presence of heavy metal is tested using electrochemical cyclic voltammetry (CV) technique. The CV measurement on the water treated with G-SiO2 has been tested for several days to understand the presence of heavy metals in water. Interestingly, the near complete separation has been observed by treating the heavy metal contaminated water sample for one to two days in presence of G-SiO2 nanoparticles. The redox potential observed for the heavy metal has been found to diminish as a function of treatment with respect to time, and no redox peak is observed after the treatment for four to five days. Further test using EDS measurement indicates that the heavy metal ions are observed within the G-SiO2 nanocomposite. The recovery of G-SiO2 nanocomposite is obtained by washing using deionized water. Our experimental finding indicates that the G-SiO2 nanocomposite could be exploited for potential heavy metals cleaning from waste or drinking water.