Abstract: Content of lead in calcium carbonate was determined by hydride generation-atomic fluorescence spectrometry (HG-AFS)．Samples were treated by hydrochloric acid.Instrument conditions,concentration of hydrochloric acid,prereducing agent dosage,reducing agent dosage,and interferance of coexisting elements were investigated．Detection limit of the method was 0．028 μg/L with relative standard deviation of 0.84%and recovery rate of 98.7%～103.9%.Method can be used in routine inspection of lead in calcium carbonate as it has simple operation,high sensitivit,and good reproducibility as well as its precision and accuracy are both meet requirements of daily examination.