Abstract: Cleaned and dried hair sample was dissolved with mixture acid of nitric acid and perchloric acid. The hydride generation of PbH4 and determination of lead content in the sample were performed automatically by the use of hyphenated instrumentation of the WHG-102A2 FI-Hydride generator and the GGX-9 Atomic absorption spectrometer. Optimum conditions of the determination,including the amount of K3Fe(CN)6 required,the temperature of atomization,the effect of HClO4 and the test for interfering substances,were studied. Detection limit of this method was found to be 0.25 μg·L-1. Precision of the method was tested at the concentration level of 8 μg·g-1,giving the value of RSD (n=10) of 3.0%.