The thermochemical decomposition of agricultural by-product corn cob impregnated with ZnCl2, as a precursor material for producing the activated carbons, was investigated by thermogravimetric (TG) analysis at the heating rate of 5 and 10°C min–1 under a controlled atmosphere of nitrogen (60 ml min–1). The appearance of a peak in the differential thermogravimetric plot (DTG) in the temperature range of 400–600°C is significantly related to the extent of impregnation. The DTG curve of the sample impregnated with the optimal impregnation ratio of 175% (i.e., the ratio of ZnCl2 mass of 87.5 g in the 200 cm3 of water to corn cobmass of 50 g), which yields an optimal BET surface area of the activated carbon and displays a DTG peak at about 500°C. This may be partially due to the intense chemical activation and results in the formation of a porous structure in the activated solid residue. This observation is also in close agreement with previous results at optimal pyrolysis temperatures of 500°C and with similar experimental conditions. In order to support the results in the TG-DTG analysis, the development of pore structure of the resulting activated carbons thus obtained by previous studies was also examined and explained using the scanning electron microscopy (SEM).