VOCs such as acetone, benzene, toluene, ethylbenzene were adsorbed in a fixed-bed adsorber using zeolite synthesized from coal fly ash and 4 kinds of activated carbon at 101.3 kPa. The adsorber was operated batchwise with the charge of 5 g adsorbent to obtain the breakthrough curve of VOCs. Experiments were carried out at 40 ℃, nitrogen flow rate of 70 cm3/min and sparger temperature of 30 ℃. The deactivation model was tested for these curves by combining the adsorption of VOCs and the deactivation of adsorbent particles. The observed values of the adsorption rate constant and the deactivation rate constant were evaluated through analysis of the experimental breakthrough data using a nonlinear least square technique. The experimental breakthrough data were fitted very well to the deactivation model than the adsorption isotherm models in the literature. Also, adsorption capacities of adsorbents were obtained from the breakthrough curve to observe the correlation between adsorption capacity and the physical properties of VOCs.