微波消解—原子荧光光谱法测花椒制品中铅和砷

Determination of Pb and As in Chinese Prickly ash products by microwave digestion-atomic fluorescence spectrometry

采用微波消解-原子荧光光谱法对花椒制品中铅和砷的测定条件（消解条件、酸浓度、硼氢化钾浓度等）进行了研究。结果表明：采用HNO3-H2O2（5∶2）消化体系为消化剂,优化微波消解程序对花椒样品进行微波消解;测铅用载留液为2%HCl,测砷用载留液为5%HCl,还原剂硼氢化钾浓度为10 g/L,在此条件下测定铅和砷的标准曲线的相关系数分别为0.9992和0.9995,方法的加标回收率在95.00%-102.00%,相对标准偏差（RSD）1.26%-3.04%,方法检出限分别为0.1μg/L和0.02μg/L。该检测方法方便、快捷、准确且灵敏度高,为花椒制品的铅和砷含量测定提供了一种较好的方法。

The determination conditions of the Pb and As in chinese prickly ash products by microwave digestion-atomic fl uorescence spectrometry were researched,including the microwave digestion conditions,acid concentration and potassium borohydride concentrations. The result showed that ：The microwave digestion with HNO3-H2O2（5：2）had many advantages such as fast and effi cient. Analyze Pb in digested samples with carrier liquid of 2% hydrochloric acid and As in samples with carrier liquid of 2% hydrochloric acid; the reducing agent concentration of potassium borohydride was 10 g/L. Under the optimized experimental conditions,the content of Pb and As was determined by AFS. The correlation coeffi cient of the standard curve was 0.9992 and 0.9995 respectively. The recoveries of the method were between 95.00% - 102.00%,the relative standard deviations（RSD）were between 1.26% - 3.04%. The detection limits were 0.1 μg/L and 0.02 μg/L respectively. The method is convenient,quickacquired accurate and highly sensitive. The method can be applied to determination of Pb and As in chinese prickly ash products with satisfactory results.