The adsorption technique using fly ash composite material has been applied for the removal of Cr(VI) from aqueous samples. Batch experiments have been carried out for the adsorption of Cr(VI) onto fly ash composite material. The effects of various process parameters, namely, pH, adsorbent dosage, initial Cr(VI) concentration and contact time has been studied in batch systems. Maximum metal removal ratio was observed at pH 5.0~5.5, and the sorption reaction was an endothermic process. The results revealed that the hexavalent chromium is considerably adsorbed on this adsorbent and it could be an economical method for the removal of hexavalent chromium from aqueous systems.