A hydride atomic fluorescence spectrometry has been developed for the determination of trace arsenic and mercury in medicinal animal horns. This method was simple, rapid and sensitive. The samples were digested with HNO3-HClO4(5:1), under the optimum conditions, the allowable amounts of 26 coexist elements were determined. The detection limits of this method were as follows: As 1.50 ng.mL-1, Hg 0.80 ng.mL-1. The relative standard deviations of 11 determinations were 1.2%-2.3% for As and 2.5%-4.7% for Hg. The recoveries were 98.9%-103.8% for As and 95.4%-105.0% for Hg.

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