A method for simultaneous determination of mercury and selenium in soil was established-Aqua regia digestion in water Bath and double channel atomic fluorescence spectrometry, aqua regia digestion in the water bath digestion and AFS determination conditions were optimizedf. The method detection limit was 0.002 μg/L, mercury, selenium. The detection limit is 0.100 μg/L; the relative standard deviation is 0.002 0%~0.034 0% of mercury, the relative standard deviation of selenium is 0.001 8%~0.058 0%; the recovery rate of mercury was 95.6%~101.4%, and the recovery rate of selenium was 96.4%~103%. The method is rapid, simple, accurate, reliable, and applicable to the determination of mercury and selenium in large quantities in soil samples at the same time.%建立王水水浴消解-双道原子荧光光谱法同时测定土壤中的汞和硒的方法，优化王水水浴消解和AFS测定条件。该法的汞检出限为0.002μg/L，硒的检出限为0.100μg/L；汞的相对标准偏差为0.0020%～0.0340%，硒的相对标准偏差为0.0018%～0.0580%；汞的加标回收率为95.6%～101.4%，硒的加标回收率为96.4%～103.0%。该法操作快速、简便，结果准确、可靠，适用于大批量土壤样品中汞和硒的同时测定。
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