A method for the estimation of gallium, indium and thallium present in bauxite and its beneficiation products, in zinc slags and in silicate materials has been developed. The three elements are separated from the major matrix and interferents by solvent extraction into methylisobutylketone in HBr medium and the determination carried out in the emission mode of atomic absorption spectrometer. The limit of determination for gallium is 0:1 mu g/ml whereas for indium and thallium it is 0.2 mu g/ml in the final solution.