摘要
目的建立微波密闭H2O2鄄HNO3消解、分离测定植物样品中不同形态硒(Se)。方法以氢化物发生原子荧光光谱法直接测定水溶态的无机Se(IV),还原后测定Se(VI)。用XAD鄄2树脂消除可溶有机质对测定的干扰,以差减法获得可溶态硒、不溶态硒、无机Se(IV)和Se(VI)以及有机硒。结果氢化物发生原子荧光光谱法测定Se(IV)的线性范围为0～80μg/L,最低检出限0.05μg/L。微波消解、原子荧光法测定植物样品硒总量的RSD为1.7%(n=5)。标准参考物质的硒总量测定结果与标准值相吻合。结论微波消解法处理植物样品避免了硒的挥发损失;XAD鄄2树脂消除有机基体对荧光法直接测定植物样品中Se(Ⅳ)的干扰,扩大了该方法在形态分析中的应用;建立的硒形态系统分析流程可以分析植物样品中6种形态的Se,操作简便,方法实用。
Objective To develop a method for speciation analysis of selenium in plant samples by H2O2-HNO3 microwave-assisted digestion-HGAFS. Methods Plant samples were prepared using H2O2-HNO3 by microwave-assisted digestion. The contents of soluble inorganic Se(IV)and Se(VI)in the samples were determined by HGAFS after separation most of the soluble organic compounds by XAD-2 resin column in HNO3 medium at pH=3. The contents of soluble Se,insoluble Se,inorganic Se (IV)and Se (VI)and organic Se could be calculated. Results The linear range and detection limit of Se(IV)were 0-80 μg/L and 0.05 μg/L respectively. The RSD for the total Se detection was 1.7%(n=5?雪. The total Se content in the reference standard substance obtained by this method agreed well with the reference value. Conclusion The method for preparation of plant samples using microwave-assisted digestion could avoid the loss of Se through volatilization. The pretreatment using XAD-2 resin could remove the interference of organic compounds on detecting results of Se(Ⅳ)in the plant samples,which could widen the application of the method in the speciation analysis. The analytical scheme of the method could determine the contents of total,soluble,insoluble,soluble inorganic Se(IV?雪?Se(VI?雪,and organic Se in plant samples. The method was simple and practical.
出处
《环境与健康杂志》
CAS
CSCD
北大核心
2004年第3期176-179,共4页
Journal of Environment and Health
基金
国家科委科技攻关项目(96-920-02-03)
原地矿部地勘高新技术研究开发计划项目(95056013)
关键词
分光光度法
硒
微波消解
Spectrophotometry
Selenium
Microwave-assisted digestion
