稀氨水密封溶解-电感耦合等离子体质谱测定土壤沉积物及生物样品中的碘溴被引量：44

Determination of Total Iodine and Bromine in Soil, Sediment and Biological Samples by Inductively Coupled Plasma Mass Spectrometry with Dilute Ammonia Pressurizing Decomposition

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摘要介绍了一个适合于电感耦合等离子体质谱直接测定土壤、沉积物和生物样品中碘、溴的快速简单的样品前处理方法。样品在φ(NH3·H2O)=10%的水溶液中,于190℃下密封分解18h,溶液适当稀释后放置澄清,用电感耦合等离子体质谱法直接测定溶液中的碘、溴。选用126Te作为内标,补偿基体效应和仪器漂移对分析结果的影响。碘、溴的方法检出限(10σ,DF=100)分别为0.01μg/g、0.04μg/g。用土壤、水系沉积物以及头发等标准物质验证了方法的准确度及精密度,绝大多数样品分析结果在标准值的允许误差范围内。对国家一级标准物质10次测定的RSD为2.0%～8.6%。但方法分析岩石样品结果偏低,不适用于岩石样品的分析。 A simple sample treatment method for accurate and precise determination of total iodine,bromine in soil, sediment and biological samples by inductively coupled plasma mass spectrometry (ICPMS) was described. Iodine,bromine in samples was dissolved in screw top PTFElined stainless steel bombs using a 10% ammonia solution at 190℃ for 18 hours. Sample solution was then directly determined by ICPMS. 126Te was used as the internal standard to compensate for matrix effects and instrument drift. The detection limit of this method, which was based on ten standard deviations of the blank (10σ,DF=100), was 0.04 μg/g for Br and 0.01 μg/g(dry mass) for I. The accuracy and precision of the method were demonstrated by analyzing different Chinese geological certified reference materials (soils, stream sediments and hair). The concentrations found were in a good agreement with the certified values, indicating that the method is unbiased. The precision was 2.0%～8.6% RSD (n=10). For soils and stream sediments, there was no notable difference between the ammonia decomposition method and 'sintering' method, but for biological samples, such as, hair, kelps, tea, the results obtained from sintering method were far lower than those from ammonia decomposition method. Compared with 'sintering' method, ammonia decomposition method has more advantages such as simpler, lower blank, better detection limit and reproducibility. But this method is unsuitable for rock sample analysis. 

作者马新荣李冰韩丽荣

机构地区国家地质实验测试中心

出处《岩矿测试》 CAS CSCD 北大核心 2003年第3期174-178,共5页 Rock and Mineral Analysis

基金国土资源部地质大调查项目(200020190120)

关键词密封溶解氨水电感耦合等离子体质谱土壤沉积物生物样品 pressurizing decomposition inductively coupled plasma mass spectrometry(ICP-MS) iodine bromine soil sediment biological sample ammonia

分类号 O657.63 [理学—分析化学] O613.4 [理学—无机化学]

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