In this paper, the atomic fluorescence (AFS-9760) method used for the determination of total arsenic in soil was verified based on three national quality control samples GSS-8, GSS-25, and GSF-3. Under the conditions of negative pressure of 270 V, carrier gas flow of 300 mL/min, and shield flow of 1 000 mL/min, the detection limit of the method was 0.009 2 mg/kg; the precision of GSS-8, GSS-25, and GSF-3 was 3.96%, 1.47% and 1.08%, and the accuracy was 3.07%, 2.13%, 2.93% respectively. In addition, the matters needing attention during this experiment, such as reagent factor, instrument conditions, calibration curve, etc., were summarized. It provides certain reference for the determination of total arsenic content in soil by atomic fluorescence spectrometry.