A catalytic procedure for the determination of ultratrace aluminum was proposed based on Al3+ catalyzed H2O2-gallocyanime redox reaction in hexamine-hydrochloric acid buffer medium. The calibration graph is linear for 0 similar to 200 mu g/L Al3+, and the detection limit is 1.2 mu g/L. The interfering effect of Fe3+ and Cu2+ could be effectively eliminated by extraction with cupferron-chloroform and dithizone-carbon tetrachloride, and that of Cr(VI) by reducing to Cr(III). The procedure has been used to determine the aluminum content in human hair, tea and wastewater, and the results were satisfactory.