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The thermal decomposition of the [Ni(NFA)2(NO3)2]*2H2O (NFA=C16H18FN3O3, norfloxacin) and its kinetics were studied under the non-isothermal condition in nitrogen by TG-DTG and DTA methods. The intermediate and residue for each decomposition were identified from TG curve. The Achar method and the Madhusudanan-Krishnan-Ninan (MKN) method were used to analyze the non-isothermal kinetic data. The possible reaction mechanisms were investigated by comparing the kinetic parameters. The kinetic equation for the third stage and the mathematical expressions for the kinetic compensation effects of the third stage were obtained.