A new hybrid process combining adsorption and ozonation is examined as an alternative treatment for Volatile Organic Compounds (VOC). The physical adsorption of ozone was clarified on a ZSM-5 zeolite. Oxidation of two industrial solvents was achieved on two zeolites and followed with temperature profiles and sub-products detection. Total regeneration of the fixed bed was achieved with a complete mineralization of organic compounds. Detection and identification of sub-products traces allowed us to suspect oxidation reactive species. A mass balance on oxygen showed that all the inlet ozone was used for organic compounds oxidation. A selective oxidation was achieved, allowing the separation and the recovery of minor compound.