Chromium orthophosphate was prepared by the soi-gel method from chromium(VI) oxide, orthophosphoric acid, and glycerol, using water as a solvent. Synthesis conditions (solution concentration, glycerol-to-chromium molar ratio, temperature) determine the gelation time but have little effect on the resultant chromium orthophosphate. The presence of excess glycerol favors formation of amorphous dehydrated chromium orthophosphate with a high specific surface area.