The catalytic oxidation of volatile organic compounds (VOCs), which were benzene and toluene, was studied in the supercritical carbon dioxide($SC-CO_2$) media. In $SC-CO_2$ media, the deep oxidation conversion of VOCs was increased with the temperature and pressure. The deep oxidation conversion in SC -$CO_2$ media is better than that in air media at same pressure condition. This can be explained by the solubility of VOCs in $SC-CO_2$. The many intermediates produced by the partial oxidation of VOCs were detected from off-line samples. The intermediates were Identified as benzene, toluene, benzaldehyde, phenol, naphthalene, 1,1`-biphenyl, benzoic acid, 3-methylphenol, 1,1'-(1,2-ethanediyl)bis- benzene, 1,1'-(1,2-ethene- diyl)bis-benzene, anthracene, and so on. The amount of intermediates was decreased as the molar radio of oxygen to carbon dioxide was decreased. When the molar ratio of oxygen to carbon dioxide was 1 : 16, the deep conversion was kept constant. Thus, the catalytic oxidation process in $SC-CO_2$ media can be combined on-line with supercritical fluid extraction of environmental matrices and supercritical regeneration of used adsorbent. Thus, the nontoxic $SC-CO_2$ media process was suggested as the new VOCs control technology.