Experimentally, two-stage oxidation of spent low-level radioactive resin was found by thermo- gravimetric analysis (TGA). About 24% of the spent resins was oxidized at 600 to 900 K. Online Fourier transform infrared spectra showed that the decomposition of the -SO3H species in the resin to SO2 occurred at 670 and 1020 K. The numerical calculation from TGA weight loss data at different heating rates showed that the global activation energies for oxidation of the spent resins were 108 to 138 kJmol-1. The reaction orders for resin and oxygen were about 1.0 and 3.5, respectively. The global rate equations for oxidation of the resin in the first and second stages can be expressed as dx1/dt (s-1) = 2.3 × 107 (s-1)exp[-117 900(Jmol-1)/T(K)][1 - x (%)]0.82 [O2 (vt%)]3.5 (x denotes the reaction conversion) and dx2/dt = 8.4 × 1017 exp(-239 500/RT) (1 - x)0.9[O2]4.5, respectively.