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微波消解-顺序注射氢化物发生-原子荧光光谱法测定堆肥中的Hg和As

Determination of Mercury and Arsenic in Compost by Microwave Digestion-Sequential Injection Hydride Generation-Atomic Fluorescence Spectrometry

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【作者】 王玉军窦森张大军崔俊涛

【Author】 WANG Yu-jun1,DOU Sen1,ZHANG Da-jun2,CUI Jun-tao1(1.College of Resource and Environment Science,Jilin Agricultural University,Changchun 130118,China;2.Institute for Land Surveying and Planning of Jilin Province,Changchun 130061,China)

【机构】 吉林农业大学资源与环境学院吉林省土地勘测规划研究院吉林农业大学资源与环境学院 吉林长春130118吉林长春130118吉林长春130061

【摘要】 采用微波消解技术处理堆肥样品,优化了样品前处理条件和仪器分析条件,建立了微波消解-氢化物发生-原子荧光光谱法测定堆肥中的Hg和As的分析方法。结果表明,该方法在最佳条件下,Hg、As的检出限分别为0.001 2、0.018μg.L-1,校准曲线的相关系数r均大于0.999。样品中待测元素的回收率在(100±8)%范围以内,RSD均小于2%,说明该方法具有简便、快速、灵敏、准确等特点,适合于堆肥样品的测定。通过堆肥产品和堆肥原料中的对比实验发现,堆肥后Hg、As的损失率小于7%,说明堆肥处理对重金属Hg、As的总量减少意义不大。

【Abstract】 The method of microwave digestion-sequential injection hydride generation-atomic fluorescence spectrometry was proposed for determining mercury(Hg) and arsenic(As) in compost by means of optimizing pre-processing and instrumental performance.The digestion temperature and volume of reagent,flow chart of digestion of compost were determined.20 min pre-processing of a sample reduced the release volume of poisonous gas.The pre-processing method of sample had characteristic of low pollution,briefness and rapidity.Disturbing effect of HNO3 was eliminated with 1% ascorbic acid in the course of testing sample.Used Ar as carrier gas and sheath gas,the flow rate was respectively 400 and 800 mL·min-1,the carrier liquid was 0.12 mol·L-1 HCl,the reducer was KHB4(its content was respectively 0.01% and 1% for testing Hg and As).The detection limit of Hg and As was 0.001 2 μg·L-1 and 0.018 μg·L-1 respectively under optimal conditions.The correlation coefficient of standard curve was more than 0.999.The recovery of Hg and As was(100±8)%,with RSD below 2%.The testing method was sensitive and accurate.The loss ratio of Hg and As was below 7% after composting,indicating that the composting had little effect on Hg and As decreasing.

【基金】 国家自然科学基金(40471076、40271069);长春市净月项目(2004C005)
  • 【文献出处】 农业环境科学学报 ,Journal of Agro-Environment Science , 编辑部邮箱 ,2006年05期
  • 【分类号】S141.4
  • 【被引频次】4
  • 【下载频次】153
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