Abstract: A method for the determination of trace germanium in copper, lead and zinc ores by hydride generation-atomic fluorescence spectrometry (HG-AFS) was developed. Samples were digested with mixed acid of HCl-HNO₃-H₂SO₄ and extracted with hot phosphoric acid. Trace Ge in the sample solution was then determined by HG-AFS. The determination condition was optimized through the experiments and the tolerance of the interference elements on the determination was also tested. The detection limit of the method for Ge was 20.64 ng/g with the detection range of 0.20~100 μg/g. The reliability of the method was tested by determination of trace Ge in National Standard Reference copper, lead and zinc ore samples with satisfactory results.