Abstract: The hydride generation of Pb from alkaline solution by atomic absorption spectrometry was studied. The K₃Fe(CN)₆ and sodium tartaric were used as oxidant and coordinate agent, and the mass concentrations of NaOH and KBH₄ in the test solution were 3.6 g/L and 1 g/L respectively. The test solution was acidified with 12.5 g/L oxalic acid to generate the hydride of Pb. The sensitivity and detection limit were 0.073 ng/ mL and 0.20 ng/ mL, respectively. The allowable values of Fe, Co, Ni in the test solution of 25 mL were 30, 3, 3 mg with this system, and it was enough to determine Pb in iron and steel without seperation of the matrix. The method was experimentally used to determine Pb in iron and steel with a satisfactory result.