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吴峥, 熊英, 王龙山. 自制氢化物发生系统与电感耦合等离子体发射光谱法联用测定土壤和水系沉积物中的砷锑铋[J]. 岩矿测试, 2015, 34(5): 533-538. DOI: 10.15898/j.cnki.11-2131/td.2015.05.006
引用本文: 吴峥, 熊英, 王龙山. 自制氢化物发生系统与电感耦合等离子体发射光谱法联用测定土壤和水系沉积物中的砷锑铋[J]. 岩矿测试, 2015, 34(5): 533-538. DOI: 10.15898/j.cnki.11-2131/td.2015.05.006
Zheng WU, Ying XIONG, Long-shan WANG. Determination of As, Sb and Bi in Soil and Stream Sediment by a Self-developed Hydride Generation System Coupled with Inductively Coupled Plasma-Optical Emission Spectrometry[J]. Rock and Mineral Analysis, 2015, 34(5): 533-538. DOI: 10.15898/j.cnki.11-2131/td.2015.05.006
Citation: Zheng WU, Ying XIONG, Long-shan WANG. Determination of As, Sb and Bi in Soil and Stream Sediment by a Self-developed Hydride Generation System Coupled with Inductively Coupled Plasma-Optical Emission Spectrometry[J]. Rock and Mineral Analysis, 2015, 34(5): 533-538. DOI: 10.15898/j.cnki.11-2131/td.2015.05.006

自制氢化物发生系统与电感耦合等离子体发射光谱法联用测定土壤和水系沉积物中的砷锑铋

Determination of As, Sb and Bi in Soil and Stream Sediment by a Self-developed Hydride Generation System Coupled with Inductively Coupled Plasma-Optical Emission Spectrometry

  • 摘要: 氢化物发生法-电感耦合等离子体发射光谱(ICP-OES)联用可以提高仪器测定的灵敏度, 但氢化物发生的化学反应过程不稳定, 导致检测精密度变差。本文设计了一套简易氢化物发生系统, 将样品进样管内径由0.32 mm扩大为0.76 mm, 与还原剂(硼氢化钾)管路通过三通混合, 混合后反应管路内径由0.76 mm扩大为1.14 mm, 反应管长度由30 cm延长至50 cm, 显著增加了待测元素氢化反应的空间和时间, 使氢化反应达到平衡态从而提高了氢化物的稳定性。土壤和水系沉积物样品用盐酸-硝酸水浴浸提、硫脲-抗坏血酸预还原后利用此套系统与ICP-OES联用测定了砷锑铋的含量。砷锑铋的检出限分别为0.35 μg/g、0.33 μg/g、0.25 μg/g, 测定范围分别为1.1~300 μg/g、1.0~100 μg/g、0.75~100 μg/g, 均满足了相关分析要求。

     

    Abstract: Hydride Generation (HG) combined with Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) has excellent analytical sensitivity. However, the instable chemical reactions of HG may cause unsatisfactory analytical precision. In this study, a novel and self-made HG system coupled with ICP-OES was developed for measurement of As, Sb and Bi in geological samples. Inner diameter (i.d.) of introduction tubing changed from 0.32 mm to 0.76 mm. Reaction tubing i.d. changed from 0.76 mm to 1.14 mm and length increased from 30 cm to 50 cm. These changes significantly improve the stability of HG reaction by increasing space and time of chemical reactions to reach reaction equilibrium. Arsenic, Sb and Bi were firstly leached from soil and stream sediment using HCl-HNO3 water bath, pre-reduced by thiocarbamide-ascorbic acid mixture, and were finally determined by the modified HG-ICP-OES. The detection limits of this method are 0.35 μg/g, 0.33 μg/g and 0.25 μg/g for As, Sb and Bi, respectively. The linear ranges are 1.1-300 μg/g for As, 1.0-100 μg/g for Sb and 0.75-100 μg/g for Bi, which is sufficient for the measurement of As, Sb and Bi in geological samples.

     

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