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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 被引量:15

Determination of Mercury and Arsenic in Compost by Microwave Digestion-Sequential Injection Hydride Generation-Atomic Fluorescence Spectrometry
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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.
出处 《农业环境科学学报》 CAS CSCD 北大核心 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)
关键词 堆肥 微波消解 氢化物发生 原子荧光光谱法 HG AS compost microwave digestion hydride generation atomic fluorescence spectrometry mercury arsenic
作者简介 王玉军(1972-),男,在读博士,讲师,研究方向为环境化学与土壤污染防治。E-mail:jlndwangyujun@163.com 通讯作者:窦森
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