Hybrid chitosan-resorcinol/formaldehyde xerogels were synthesized, and the effect of including minor quantities of chitosan on the consequent activated carbon was investigated. The resulting activated carbon were characterized by different techniques. Clear changes were found in the structure of activated carbon as a result of including chitosan in the synthesis. The results showed that the disorder ratio of crystal lattice decreased from 0.750 to 0.628 when increasing the concentration of chitosan from 0 to 0.037 wt%. The micropores increased from ~0.3% to ~1.0%, mesopores increased from ~11.2% to ~32.9% and macropores decreased from ~88.4% to ~66.1%. The total pore volume decreased from 1.040 to 0.238 cm3/g and the total pore surface area decreased from 912.3 to 554.4 m2/g. On the other hand, the average pore width decreased from 2.3 to 0.8 nm and the average particle size decreased from 224 to 149 nm. Nano-scale Scanning Electron Microscope (NanoSEM) morphology indicated a critical composition of chitosan (0.022 wt%) that affects the structure and thermal stability of activated carbon produced.