Abstract: Copper ore samples were digested with HNO₃-HCl-HClO₄ mixed acid and silver, copper, lead and zinc in sample solutions were then directly determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The determination parameters were systematically studied and optimized. Matrix matching and correction factor methods were used for the correction of matrix effect and spectral interference. The detection limits of the method (dilution factor=500) were 3.15 μg/g for Ag, 4.00 μg/g for Cu, 12.0 μg/g for Pb and 6.00 μg/g for Zn. The reliability of the method has been tested by determination of these elements in polymetallic ore National Standard Reference samples and the results are in agreement with the certified values with precisions of 0.38%~4.55%RSD (n=12).