Abstract: This paper investigates the adsorption of uranium on the polyaluminium and the determination of uranium in the solution containing aluminum ion using Arsenazo Ⅲ. Research shows that: the error of uranium determination using Arsenazo Ⅲ is less than 10% when the concentration of aluminum is less than 0.1 mol/L in the 1∶1 hydrochloric acid medium, molar absorption coefficient is 10³ L/(mol•cm). When OH^- is two times aluminum in the polyaluminum and the concentration of aluminum is 5.64×10^-3 mol/L, the removal rate of uranium can reach 90% or more. Therefore, polyaluminum is a kind of very good uranium adsorption materials, and it can realize the volume reduction of the waste water containing uranium, thus reducing the costs of nuclear waste disposal.