PVA/TiO2 nanocomposite membranes developed were investigated for chemical, mechanical, and gas separation properties. PVA/TiO2 dispersion offers good optical property and less aggregation, as shown by UV-vis photospectroscopy. FT-IR spectra suggest strong interaction between PVA and TiO2. Mechanical properties of the composite membranes were enhanced by the addition of TiO2. Permeation results show that the addition of TiO2 up to 20wt.% increased the selectivity of gas pairs O-2/N-2,N- H-2/N-2,N- H-2/CO2, and CO2/N-2 by 60%, 55%, 23%, and 26% respectively, with a corresponding decrease in the permeability. At higher loading of TiO2, a reverse trend was observed.