Determination of lead in urine is important in industrial hygiene and toxicology. Dithizone method has been principally used for the determination of lead in urine, which gives accurate results in skilful hands but is usually complex and time-consuming. Atomic absorption spectrophotometry is a new simple method and several procedures have been described. However, the influences of pH and the presence of chelating agents during treatment of lead poisoning are not clear. The purpose of this study was to find out the effect of pH and chelating agents on the determination of lead using Shimadzu atomic absorption/flame spectrophotometer, model AA-610. The results obtained were as follows: 1. The atomic absorption spectrophotometry(AAS) could be applied without prior acid digestion to specimens in the absence of chelating agents. The absorbance at $2,170;{AA}$, though more sensitive, was more noisy electronically. Therefore, we selected the wavelength of $2,833;{AA}$ plus scale expansion. 2. The optimal pH was in the range from 2 to 3. 3. The sensitivity was $0.075{mu}g/ml/%$ and detection limit was about $0.2{mu}g/ml$. 4. In the presence of EDTA, lead could not be completely determined without prior acid digestion. 5. On specimens from patients receiving penicillamine therapy, a comparison was made between the values obtained with dithizone method and AAS method with prior acid digestion. The results of comparison showed a very good agreement.