A series of activated carbons with high surface area were prepared from walnut shell using chemical activation with ZnCl₂. In this research the carbonization stage was carried out at 500°C. The performance of the synthesized carbons evaluated in adsorption of benzene and toluene from waste gas. The influence of impregnation ratio on the characteristics of synthesized activated carbons as well as their adsorption capacity was investigated. The ratio of activation agent to walnut shell was selected in the range of 0.5–2.0 wt/wt. The synthesized activated carbons were characterized using XRD, SEM, BET and FTIR techniques. The highest activated carbon production yield was obtained at impregnation ratio of 1.5 wt/wt. The XRD analysis illustrated that peaks intensity decreased with increasing impregnation ratio showing that amorphous property of samples was increased. The SEM analysis revealed successful pore development in synthesized activated carbons obtained at high impregnation ratios. The surface area of the activated carbons increased with increasing impregnation ratio and its maximum value reached 2643 m²?g^-1 at impregnation ratio of 2/1. FTIR analysis indicated that the relative amount of different acidic surface groups on synthesized carbons was a function of impregnation ratio. Experimental results for benzene and toluene adsorption showed a high potential of employing synthesized impregnated activated carbon for treatment of waste gas. Generally, the amount of VOC adsorbed on the surface was affected by physicochemical properties of synthesized activated carbons.