Abstract: A method for the determination of water soluble and exchanged Sb(Ⅲ) and Sb(V) in soil samples was established using hydride generation-atomic fluorescence spectrometry in medium of 0.10 mol/L tartaric acid. The detection limit was remarkably improved and the concentration of KBH4 used was reduced due to the use of pure H2from hydrogen generator and steady Ar-H2 flame. Dosage of masking agent of tartaric acid and tolerance amounts of coexisted elements were also investigated. The detection limits of the method are 0.026 ng/L for Sb(Ⅲ) and 0.019 ng/L for total Sb. The accuracy of the method was verified by recovery tests on spiked samples.