Both UV Photolysis and Phtocatalytic Oxidation Processing are an emerging technology for the abatemant of Volatile Organic Compounds (VOCs) in atmospheric -pressure air streams. However, each process has some drawbacks of their own. The former is little known as an application for air pollution treatment, so it has been a rare choice in the field. Therefore we have to do more experiment and study for its application for treatment of VOCs. Although the latter has been used in the industrial fields, it still has a difficulty in decomposing high concentrations of VOCs. To solute these problems, we have been studying simultaneous application of those two technologies. We have studied the effects of background gas composition and gas temperature on the decomposition chemistry. It has shown that concentration of TCE and B.T.X., diameter of reactor, and wavelength of lamp have effects on decomposition efficiency. When using Photolysis Process only, the rates of fractional conversion of each material are found at TCE 79%, Benzene 65%, Toluene 68%, Xylene 76%. In case of Photocatalytic Oxidation Process only, the rates of fractional conversion decreased drastically above 30 ppm. When there two methods were combined, the rates of fractional conversion of each material are enhanced such as TCE 93%, Benzene 75%, Toluene 81%, Xylene 90%. Therefore, we conclude that the combination of Photolysis-Photocatalytic Oxidation process is more efficient than each individual process.