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电热蒸发电感耦合等离子体原子发射光谱法测定环境样品中的磷和硫

Determination of phosphorous and sulfur in environmental samples by electrothermal vaporization inductively coupled plasma atomic emission spectrometry.

作者信息

Okamoto Yasuaki, Kanda Kouichirou, Kishiwada Satoru, Fujiwara Terufumi

机构信息

Department of Chemistry, Graduate School of Science, Hiroshima University, Kagamnivama, Higashihiroshima, 739-8526, Japan.

出版信息

Appl Spectrosc. 2004 Jan;58(1):105-10. doi: 10.1366/000370204322729531.

DOI:10.1366/000370204322729531
PMID:14727727
Abstract

From the viewpoint of selective introduction of the analyte from its solvent and matrices, electrothermal vaporization (ETV) is useful for the sample introduction into the inductively coupled plasma (ICP). By using a tungsten boat furnace (TBF) vaporizer system, the loss of analyte phosphorus, which normally occurs during the drying and ashing stages, is suppressed. The phosphate ion is reacted with the tungsten supplied from the surface of the TBF to form stable tungsten phosphate species. Regarding the determination of sulfur, additional chemical modifiers such as copper(II), lead(II), etc., are necessary to retain the analyte on the TBF. The furnace-fusion (FF) method or wet-digestion technique on the TBF is applied to unify the chemical forms of the analytes. Various oxidative and reductive inorganic compounds as well as organic compounds of phosphorus and sulfur show the same sensitivities after the FF digestion with hydrogen peroxide. The detection limits are 1.5 ng and 0.12 ng for phosphorous and sulfur, respectively. The repeatabilities in terms of the relative standard deviations of 10 replicate measurements of phosphorus and sulfur are 4.2% and 2.0%, respectively. Finally, the established method is applied to the determination of several environmental waters.

摘要

从选择性地将分析物从其溶剂和基质中引入的角度来看,电热蒸发(ETV)对于将样品引入电感耦合等离子体(ICP)很有用。通过使用钨舟炉(TBF)蒸发器系统,通常在干燥和灰化阶段发生的分析物磷的损失得到了抑制。磷酸根离子与从TBF表面供应的钨反应形成稳定的磷酸钨物种。关于硫的测定,需要额外的化学改性剂,如铜(II)、铅(II)等,以将分析物保留在TBF上。采用炉熔合(FF)法或TBF上的湿消化技术来统一分析物的化学形态。在用过氧化氢进行FF消化后,各种氧化和还原无机化合物以及磷和硫的有机化合物显示出相同的灵敏度。磷和硫的检测限分别为1.5 ng和0.12 ng。磷和硫10次重复测量的相对标准偏差方面的重复性分别为4.2%和2.0%。最后,将所建立的方法应用于几种环境水样的测定。

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