Chitosan and chitosan/ hexamethylenetetramine (HMT) macrospheres were prepared respectively by dropping chitosan and chitosan/HMT (in wt/wt ratios of 1:1 and 1:3) solutions in aq. NaOH solution.Here, HMT served as an additional nitrogen precursor for in-situ N-doping with chitosan derived activated carbon (AC). The as-formed macrospheres were impregnated using ZnCl 2 , freeze-dried, and carbonized at 500°C under inert atmosphere to yield ACs of average size 2.6 mm. All the samples were characterized using SEM, EDS, CHNS Analyzer, TGA, FT-IR, Raman, XRD and BET surface area analyzer. All the samples showed mesoporous characteristics. The surface area of the AC without HMT, with 1:1 HMT, and 1:3 HMT were 391.502, 259.017, and 111.717 m 2 /g respectively. Similarly, the pore volumes of AC without HMT, with 1:1 HMT and 1:3 HMT were 0.138, 0.095 and 0.075 cc/g respectively. The chitosan/HMT derived AC possessed higher N-content and better thermal stability, however exhibited lower surface properties with increasing HMT content. Deterioration in adsorption capacity of chitosan/HMT derived AC may be attributed to the physical cross-linking of chitosan polymer chains induced by increase in pH with addition of HMT and also the intermolecular H-bonding interaction between HMT and chitosan, which in turn reduces the surface area of as-formed N-doped ACs progressively.