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

作　　者：王玉军[1] 窦森[1] 张大军[2] 崔俊涛[1] 

机构地区：[1]吉林农业大学资源与环境学院,吉林长春130118 [2]吉林省土地勘测规划研究院,吉林长春130061

出　　处：《农业环境科学学报》2006年第5期1375-1378,共4页Journal of Agro-Environment Science

基　　金：国家自然科学基金(40471076;40271069);长春市净月项目(2004C005)

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。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.

关 键 词：堆肥 微波消解 氢化物发生 原子荧光光谱法 HG AS 

分 类 号：S141.4[农业科学—肥料学]