采用增压消化罐进行样品预处理,HG-AFS法测定了固体样品中的AS和Pb。探讨了酸介质、称样量、还原剂浓度及酸度等因素对测定结果的影响,优选出仪器最佳工作条件,并用此方法对标准物质小麦(GBW08503)和标准参考物质桃叶(82301)进行分析,结果表明,小麦中As和Pb的测定结果均在标准含量范围之内,桃叶中As和Pb的测定值与推荐值之间的相对偏差分别为2.35％和1.04％。 Samples were pre-treated with a pressurized digestion tank and HG-AFS was used to determine AS and Pb in solid samples. The effects of acid medium, sample amount, concentration of reductant and acidity on the determination results were discussed. The optimum working conditions of the instrument were optimized. The standard material wheat (GBW08503) and the standard reference material peach leaf (82301) The results showed that the determination results of As and Pb in wheat were within the standard content, and the relative deviations of As and Pb in peach leaf from the recommended value were 2.35% and 1.04% respectively.