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This study demonstrated a technique to regenerate spent activated carbon using solvent desorption followed by thermal decomposition of pollutants. Dichloromethane is used as solvent for desorption and thermal reactor under inert (N 2 , CO 2 ) atmosphere used for thermal reactivation of the spent carbon. Physical, chemical, functional chemistry and thermal behavior of the samples before and after treatment are featured by means of pH, bulk density, moisture content, ash content, Fourier transform infrared spectroscopy, thermo-gravimetric differential thermal analysis. The adsorptive property of the activated spent carbon is quantified using methylene blue and iodine as model compounds. After reactivation, methylene blue and iodine number adsorption is improved from 5 to 96 % and from 10 to 99 %, respectively. This regenerated carbon applied for paper mill and pharmaceutical effluents. 95 and 94 % of the COD reduction and color removal are observed by spent reactivated carbon.