Abstract: A method for the determination of arsenic, antimony and bismuth in copper ores by hydride generation-atomic fluorescence spectrometry was developed. The sample was dissolved by aqua regia and copper was then effectively separated by using Fe3+as coprecipitation agent in ammonium hydroxide solution. Arsenic, antimony and bismuth in the sample solution were determined by hydride generationatomic fluorescence spectrometry. The detection limits of the method are 0.19 μg/g for arsenic, 0.052 μg/g for antimony and 0.049 μg/g for bismuth. The precisions (RSD, n=10) of the method are 5.87%for arsenic, 7.58% for antimony and 2.42% for bismuth.