A hybrid process combining adsorption and ozonation was examined as an alternative treatment for odorous volatile organic compounds (VOCs). Methyl ethyl ketone (MEK) was chosen to study the influence of operating parameters. Two synthetic aluminosilicates (faujasite-Y and ZSM-5) were tested for adsorption and reactivity with ozone. The adsorption equilibrium measurement on both adsorbents showed that adsorption performance depends on temperature but is not sensitive to relative humidity, due to the hydrophobic properties of the materials. Adsorbed VOCs were oxidized at low temperature when ozonated flow was sent to the reactor. Regeneration of the fixed bed was achieved at the same time, releasing mainly CO2 and H2O. Intermediates of oxidation, such as 2,3-butanedione and acetic acid, were identified, leading to incomplete mineralization. The influence of concentration and humidity are discussed. Four successive cycles were tested: after the first adsorption/ozonation cycle, the adsorption efficiency was not affected during subsequent cycles. These results show that the same sample of adsorbent can be used in the treatment process for a long time. Ozonation regeneration is a promising process for VOC removal.