Adsorption technology can effectively handle the volatile organic compounds (VOCs) from waste gas. However the adsorption of VOCs at elevated temperature (>30oC) and high humidity conditions results in competitive adsorption between VOCs and the moisture. Furthermore, physical adsorption at an elevated temperature is the cause of degradation in the regeneration process performance. In this study, toluene as waste organic solvent in air at elevated temperature and high humidity was used to measure performance. The effects of the SiO2/Al2O3 ratio of zeolites, the adsorbent material coated on adsorption regenerative rotors, on the adsorption performance of toluene with respect to temperature (30~50oC) and relative humidity (50~90%RH) have been investigated. The adsorption of toluene decreased as relative humidity and adsorption temperature rose. The result shows that Htype ZSM5 (SiO2/Al2O3=100) zeolite exhibited the highest adsorption capacity for toluene at elevated temperature and humidity conditions. The physical and chemical adsorption of toluene on acid sites of zeolite were confirmed by this study. Keywords : Adsorption, Relative humidity, SiO2/Al2O3 ratio, VOCs, Zeolite