The amberlite XAD-2 resin was functionalized with 5-sulfosalicylic acid. Selective method diazo spacer technique (- N=N-) was used for the functionalization of amberlite XAD-2 and the product was abbreviated as 5-SSA-N=NAXAD- 2. Intermediates formed in the reaction were characterized by FTIR method and resulting product was further characterized by FTIR and TGA. Thermo-kinetic parameters were determined by Freeman-Carroll (FC) and Sharp-Wentworth (SW) methods. Activation energy (Ea), free energy changes (ΔG) and entropy change (ΔS) of degradation were calculated by both FC and SW methods. Results were found to be in good agreement. The order of degradation (n) obtained by the FC method was finally confirmed by SW method.