Abstract: In this paper, a method for the determination of silver in lead concentrate powder samples by flame atomic absorption spectrometry was developed. The sample was dissolved with HCl-(NH₄)HF₂-HNO₃-HClO₄ and in the medium of 10% HCl, Ag in the sample solution was determined by air-acetylene flame atomic absorption spectrometer at wavelength of 328.1 nm. Sample digestion condition and instrument operation parameters were also studied and optimized. The detection limit of the method was 1.2 μg/g for Ag. The reliability of the method has been tested by determination of Ag in national standard reference lead concentrate powder sample (GBW 07167) and the result is in agreement with certified value with precision of 2.2%~4.3% RSD(n=12). The method provides the advantages of high efficiency and simple operation.