A comparative study of the radiolysis of used transformer oil and oil containing 1, 2, 4-trichlorbenzene (TCB) under the influence of gamma-radiation was carried out. Dependence of concentration of H2, H2O2, pH-indicator and IR-spectra of γ-irradiated samples from absorbed doses in the range of 4…136 kGy was studied. The pH-value dependence and concentration of hydrogen peroxide as a function of the absorbed dose is studied. Irradiation leads to increasing of acidity, related with dechlorination of TCB molecules. It is found that during the radiolysis of transformer oil containing TCB in the presence of dissolved oxygen, radiation-initiated oxidation of the oil takes place (formation of H2O2, CO2).