Abstract: When the irradiated uranium-aluminum alloy components are dissolved, in order to automatically adjust the amount of nitric acid during dissolving, and ensure dissolution go smoothly, it is necessary to rapidly analyze concentration of the aluminum. In acetic acid-sodium acetate buffering system, the interference caused by a small amount of uranium and Hg²⁺ can be eliminated by adding a certain amount of Cl^-. Through adding an excessive amount of disodium EDTA standard solution and selecting an appropriate indicator, Al³⁺ in this system can be determined indirectly with zinc standard solution which is used to back titrate EDTA in the experiment. And titration apparatus operated by manipulator, which is suited to be operated in hot cell, have been developed. For 1.6 mol/L Al³⁺, the recovery of the results is 99.47%-100.56%, and the precision is better than 0.36%. The analysis requirement of samples is satisfied.