Abstract: In this paper, the method of hydride generation-atomic fluorescence spectrometry was used for the simultaneous determination of arsenic and mercury in soil. The experimental results showed that the detection limit of arsenic was 0.14 mg·kg^-1, and the detection limit of mercury was 0.004 mg·kg^-1. The correlation coefficient R of standard curve was 0.999 9, and the RSD of precision and accuracy of arsenic and mercury was all less than 10%. The method met the requirements of agro-geology for the analysis and testing of arsenic and mercury, and had the value of popularization.