Objective] To research the feasibility of simultaneous determination of As and Se in soil samples by Hydride Generation-Atomic Fluorescence Spectrometry.[Method] we researched the effects of furnace height, negative high voltage, lamp current, flow rate of carrier gas, flow rate of shield gas, type of reducing agent, acidity concentration and potassium borohydride concentration on the As and Se contents by Atomic Fluorescence Spectrometry.Hydride Generation-Atomic Fluorescence Spectrometry were used to simultaneously detect the As and Se contents in soil samples.[Result] Detection limits of As and Se by Hydride Generation-Atomic Fluorescence Spectrometry were 0.370 and 0.430 ng /mL, respectively.The relative standard deviations of As and Se were 1.28% and 2.73%, respectively.[Conclusion] It is feasible to use Hydride Generation-Atomic Fluorescence Spectrometry to detect the As and Se contents in soil samples, which fully meets the detection requirements of As and Se in soil samples.%[目的]研究采用氢化物发生–原子荧光法同时测定土壤样品中 As 和 Se 含量的可行性。[方法]研究炉高、负高压、灯电流、载气流速、屏蔽气流速、还原剂种类、酸度浓度、硼氢化钾浓度对原子荧光法同时测定 As 和 Se 含量的影响，采用氢化物原子荧光光谱法同时测定土壤样品 As 和 Se 含量。[结果]氢化物发生–原子荧光法测定 As 的检出限为0．370 ng ／mL，Se 的检出限为0．430 ng／mL，As 和 Se的相对标准偏差分别为1．28％和2．73％。[结论]氢化物发生–原子荧光法用于同时测定土壤样品中 As 和 Se 含量可行，能完全满足土壤样中 As、Se 的测定要求。
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