Abstract: The concentration of antimony is usually determined by hydride generation-atomic fluorescence spectrometry in soil monitoring. Two different digestion methods aqua regia microwave digestion and mixed acid (HNO₃+HClO₄+HF) digestion were introduced to digest the soil samples. Results suggested that aqua regia microwave digestion was effective in detecting the concentration of antimony in soils, and the results of antimony were in good agreement with reference values. The relative standard deviation (RSD) of 9 standard soil detections was 3.6%, and the recoveries of real samples was 96%~102%. The recovery of antimony was only 78%~86% and the RSD value was over 5% processed by mixed acid digestion, which might because the samples were entirely dried out in the process of evaporation.