A novel technique has been devised for the synthesis of microporous alpha-Cr2O3 (eskolaite). The technique was based on the formation of amorphous-Cr2O3 onto microporous activated carbon through adsorption-reduction of dichromate ions (Cr2O72-) at the activated carbon/aqueous solution interface. Then, the Cr2O3-loaded carbon was thermally processed under oxidizing conditions to remove the carbon and ;recover the chromium oxide as alpha-Cr2O3. Both the Cr2O3-loaded carbon and the synthetic product were characterized by XRD. SEM, surface area and pore volume measurements. The synthetic eskolaite assayed 97.3% Cr2O3 and its specific surface area was 15.48 m(2)/g and pore size of 16.1 angstrom. (C) 2012 Elsevier Inc. All rights reserved.