采用硝酸分解样品,用聚环氧琥珀酸(PESA)掩蔽基体,建立了氢化物发生原子荧光光谱法(HG-AFS)测定铅锭中砷和汞的简单方法.研究了溶样方法和PESA用量对测定结果的影响,优化了氢化物发生条件及仪器的工作参数,考察了共存元素可能引起的干扰.实验表明,0.1g铅锭溶解后加入2.0 mL PESA可以有效地掩蔽基体元素Pb,铅锭中的Ca、Cu、Sb和Sn不干扰As和Hg的测定.砷和汞的方法检出限分别为0.070μg/L和0.011 μg/L.将方法应用于实际样品分析,砷和汞的相对标准偏差(RSD,n=5)分别在1.0％～2.0％和1.3％～1.9％之间,加标回收率分别为96％～102％和99％～103％.
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