A method for determination of the contents of Bi in soils and sediments by atomic fluorescence spectrophotometry (AFS) was established by using aqua regia as the dissolved medium. In this paper, the instrument parameters, load flow and reducing agent concentration were optimized. Compared with microwave digestion and electric heating plate digestion, water bath digestion demonstrated the better digestion efficiency and was most commonly used. Under the optimal experimental conditions, the detection limit (LOD) was 0.01 mg·kg-1 (sample quantity 0.500 0 g, sample volume 50 mL), and the limit of quantitation (LOQ) was 0.04 mg·kg-1. The results were in good agreement with the centified value, and the relative error was -4.7%~-2.0%. For determination of soil and sediment actual samples, the relative standard deviation (RSD) were 2.5%~3.4% and 3.1%~3.4%, respectively, and the recoveries of the method respectively ranged from 97.6%~102% and 99.5%~104%.