This study explores the removal rate of nitrobenzene (NB) using a new gas-liquid-liquid (G-L-L) three-phase ozone-loaded system consisting of a gaseous ozone, an aqueous solvent phase, and a fluorinated solvent phase (perfluorodecalin, or FDC). The removal rate of NB was quantified in relation to six factors including (1) initial pH, (2) initial NB dosage, (3) gaseous ozone dosage, (4) free radical scavenger, (5) FDC pre-aerated gaseous ozone, and (6) reuse of FDC. NB removal rate is positively affected by the first three of these factors. Compared with the conventional gas-liquid (water) (G-L) two-phase ozonation system, the free radical scavenger (tertiary butyl alcohol) has much less influence on the removal rate of NB in the G-L-L system. The FDC-loaded ozone acts as an ozone reservoir and serves as the main reactive phase in the G-L-L three-phase system. The reuse of FDC has little influence on the removal rate of NB. These experimental results suggest that the oxidation efficiency of ozonation in the G-L-L three-phase system is better than that in the conventional G-L two-phase system.