Removal of volatile organic compounds (VOCs) from air by a separation process is common engineering practice. Adsorption process has been widely recognized as an effective means of controlling emissions to the atmosphere and, in some applications, of recovering recyclable materials from process exhaust streams. In addition, owing to industrial availability, many researches related to adsorption and hot purge gas, especially ambient gas or nitrogen, regeneration on activated carbon or zeolite applications were published. However, very few focused on the steam regeneration in spite of excellent efficiency. Moreover, model estimation of steam regeneration has little been reported. The adsorption and steam regeneration dynamics of VOCs (toluene and acetone) in the fixed bed were studied experimentally and theoretically. Toluene as a non-polar solvent is insoluble in water, while acetone as a polar solvent is soluble in water. Their adsorption capacity and steam regeneration were compared to each other at various operating conditions. The adsorption isotherms of acetone and toluene vapors on the adsorbents exhibit type-II (BDDT classification) in the experimental range as multilayer adsorption. On the other hands, water vapor shows type-V adsorption isotherm with condensation phenomena. Considering the physical properties and isotherms of the adsorbates, mathematical model is developed to predict the dynamic characteristics of steam regeneration in the fix bed. And all simulations are performed by gPROMS PDE solver.