Rice samples were digested by a mixture of nitric and perchloric acids (4∶1, V/V). Dithizone was used to chelate mercury ion in the sample solution, and the mercury complex was dispersed in ethanol before being extracted into carbon tetrachloride. Thus, a method of determining mercury in rice by dispersion liquid micro extraction-atomic fluorescence spectrometry was established. The operating parameters of the instrument and optimal experimental conditions of dispersive liquid-liquid microextraction were optimized, including the best complex acidity, the amount of complexing agent, extraction solvent type, the amount of dispersant dosage, and the extraction time. Experiments showed that under optimal conditions, the linear range was 0.005~25 μg·L-1 and the correlation coefficient was 0.996 6 with the detection limit of 0.003 μg·L-1, the relative standard deviation (RSD) of 3.84%, and the recovery 95%~105% . The method is proven to be a sensitive, rapid, and accurate,way which can detect effectively trace amounts of mercury in rice.