A simple, rapid and useful method for thedetermination of water-soluble antimony(Ⅲ) and antimony(Ⅴ) in soil was established using hydride generation atomic fluorescence spectrometry. The method was based on the different chemical reaction efficiency between Sb(Ⅲ) and Sb(Ⅴ) with KBH₄ in the media of HCl. The amounts of Sb(Ⅲ) and Sb(Ⅴ) can be obtained through measuring antimony fluorescence intensities before and after reduction with reductant. The effects of HCl and KBH₄ on the sensitivities of Sb(Ⅲ) and Sb(Ⅴ) were investigated, and the interferences from coexistent elements were studied. The reduction efficiencies of both reductants were compared. The detection limits of the method were 1.11ng·g^-1 for Sb(Ⅲ) and 1.57ng·g^-1 for Sb(Ⅴ). The accuracy of the method was verified by recovery experiments on spiked real soil samples.