Atomic fluorescence spectrometric determination of lead in water is carried out. The results obtained show that linearity is good(the related average coefficient is 0.999 0 in standard curve 0.00 ~ 10.00 μg/L). The precision is better(the relative standard deviation is 0.96% ~ 3.52%). The accuracy and sensitivity are higher(the recovery rate is 90.3% ~ 108.4%, detection limit is 0.09 μg/L). It is a pretty good method for the determination of lead in water.