A comprehensive study was performed for a thermally treated activated carbon to evaluate the influence of this treatment on the physical and chemical properties of the mineral activated carbon, as well as the adsorption toward phenol and methylene blue. After the heat treatment, surface area decreased and total pore volume diminished about 8.5%, and the total basic groups decreased 18% while the total acid groups increased 8% in comparison with the raw activated carbon. Equilibrium adsorption of phenol and methylene blue was described well with the Freundlich and Langmuir isotherm models, respectively. Adsorption kinetics of phenol and methylene blue was predicted adequately with the empirical pseudo-second-order model, the intraparticle diffusion model, and the homogeneous solid diffusion model, but mass transfer coefficients of the diffusion models help to better understand the adsorption phenomenon. Intraparticle diffusion seems to be the ratecontrolling step in the adsorption process, and heat-treated activated carbon in an inert atmosphere was a better adsorbent for both phenol and methylene blue than raw activated carbon.