The transient spectra of aqueous CCl4solution by laser flash photolysis (LFP) was studied in this paper. The transient absorption band (λmax<300nm) of aqueous CCl4solution bubbled with N2was attributed to the trichloromethyl radical (CCl3·) with a 2nd-order decayed reaction rate of 3.80 × 108mol−1·L·s−1. The transient absorption band (λmax320nm) of the same solution bubbled with O2was attributed to the peroxytrichloromethyl radical (CCl3O2·) with a 1st-order decay reaction rate of 1.9 × 104s−1. The transient absorption band around 330 nm of aqueous CCl4solution always exists insolutions bubbled with either N2or O2and was attributed to the solvated chlorine atom (Cl). COCl2as a photolysis product of aqueous CCl4solution, in the presence of O2, was observed directly in the transient absorption spectra. The results indicate that CCl4can be degraded by the photooxidation process.