Optimization of lead hydride generation has been performed and a regression model of the efficiency (chemical yield, E %) of plumbane generation has been derived from experimental data. The effect of various chemical and instrumental parameters on hydride generation and trapping in an absorbing solution of Ce(IV)-KI, with subsequent determination of lead by graphite-furnace atomic absorption spectrometry (GF-AAS) has been studied, in an effort to optimize conditions for preconcentration and determination of nanogram amount of lead. Characteristic concentrations are 1 μg/1 in absorbing solution and 0.2 μg/1 in a 50-ml aliquot of sample solution and the corresponding limits of detection are ca. 4 and 1 μg/1, respectively.