Engelhard titanosilicate ETS-10 was synthesized using Degussa P25 as the titanium source. Metal-exchanged microporous titanium silicate M-ETS-10 (M = Fe, Co, Ni, Cu, and Ag) samples were prepared by ion exchange with respective metal salt solutions. The synthesized samples were characterized by powder X-ray diffraction, BET surface area, thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and UV-vis diffuse reflectance measurements (DRS). The photocatalytic activity of these samples was investigated for the decomposition of nitrobenzene (NB). The pristine ETS-10 and transition-metal-ion-exchanged ETS-10 samples were found to be active photocatalysts that can decompose nitrobenzene under UV irradiation. Results demonstrated that silver-ion-exchanged ETS-10 shows the highest photocatalytic activity for degradation and mineralization of nitrobenzene.