Abstract: The sample of lead concentrate was leached for 40 min in hot solution of acetic acid-ammonium acetate at 20-50℃, and then the content of lead in the leaching solution was determined by flame atomic absorption spectrometry (FAAS). The interference of Fe³⁺ was eliminated with stannous chloride; and the interference of the leaching medium was eliminated by the matrix matching method. Linear relationship between the mass concentration of lead and its corresponding absorbance was kept within the range of 10 mg·L^-1, with detection limit (3s) of 0.36 mg·L^-1. Values of recovery obtained by standard addition method were found in the range of 94.4%-104%. The proposed method was applied to the analysis of sample of lead concentrate, giving values of RSD (n=7) in the range of 1.1%-4.1%.