The synthesis of mesoporous activated carbons from calcium (Ca) and iron (Fe) exchanged sub-bituminous and bituminous coals was analyzed. The flame coal and gas coal were used as starting materials. Prior to carbonization and activation with steam, the coals were loaded with Fe by ion-exchange of Ca preloaded coal. The Ca and Fe contents in high temperature ash of loaded coals were determined by atomic absorption spectroscopy. The results show that Ca and Fe exchanged sub-bituminous and bituminous coal produced activated carbon with significant mesoporosity. The gas coal was more susceptible to mesoporosity development than the flame coal.