Nanocomposites of Co:TiO 2 were prepared by wet chemical methods. The prepared samples were characterized by XRD, SEM, BET, FTIR and UV-Visible spectra. The XRD analysis confirmed the presence of rutile and anatase both phases were present. It is found that rutile phase was more dominant. Applying the Scherrer's calculations through which particle size was found 35 and 80 nm in case of Co:TiO 2 and pure TiO 2 respectively. SEM image of Co:TiO 2 and TiO 2 were observed and both found in nanodiamension. The photocatalytic degradation of acetic acid was done at different condition of concentration, amount of photocatalyst and type of catalyst. The effective photodegradation of acetic acid were found at low concentration and photodegradation increases with decrease the concentration of acetic acid. The prominent degradation of acetic acid was found in the presence of nanocomposites Co:TiO 2 as compared with TiO 2 .