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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Determination of vanadium in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry using permanent modifiers
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Determination of vanadium in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry using permanent modifiers

机译:永久改性剂进样石墨炉原子吸收光谱法测定土壤和沉积物中的钒。

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摘要

A new analytical procedure for vanadium (V) determination in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry (slurry sampling GFAAS) using the mixed permanent modifiers is described. Moreover, the comparison of action of the modifiers based on the iridium (Ir) and carbide-forming elements: tungsten (W) and niobium (Nb) deposited on the graphite tubes is studied, especially in terms of their analytical utility and determination sensitivity. The mechanism of their action was investigated using an X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray detector (EDX). Finally, the mixture of 0.3 μg of Ir and 0.04 μg of Nb was used for the graphite tube permanent modification. The analytical procedure was optimized on the basis of the data from pyrolysis and atomization temperature curves studies. The results obtained for the four certified reference materials (marine sediments: PACS-1 and MESS-1, lake sediment: SL-1, soil: San Joaquin Soil SRM 2709), using the slurry sampling GFAAS and the standard calibration method, were in good agreement with the certified values. The detection and quantification limits and characteristic mass calculated for the proposed procedure were 0.04 μg/g, 0.16 μg/g and 11.9 pg, respectively. The precision (RSD% less than 8%) and the accuracy of vanadium determination in the soil and sediment samples were acceptable.
机译:描述了一种通过使用混合永久性改性剂的浆液采样石墨炉原子吸收光谱法(浆液采样GFAAS)测定土壤和沉积物中钒(V)的新分析程序。此外,还研究了基于铱(Ir)和碳化物形成元素:沉积在石墨管上的钨(W)和铌(Nb)的改性剂的作用比较,尤其是从其分析实用性和测定灵敏度的角度出发。使用配备了能量色散X射线检测器(EDX)的X射线衍射技术(XRD)和扫描电子显微镜(SEM)研究了它们的作用机理。最后,将0.3μgIr和0.04μgNb的混合物用于石墨管的永久改性。根据热解和雾化温度曲线研究的数据对分析程序进行了优化。使用泥浆采样GFAAS和标准校准方法获得了四种认证参考物质(海洋沉积物:PACS-1和MESS-1,湖沉积物:SL-1,土壤:圣华金土壤SRM 2709)的结果。与认证值一致。拟议程序的检测限和定量限以及特征量分别为0.04μg/ g,0.16μg/ g和11.9 pg。在土壤和沉积物样品中的精密度(RSD%小于8%)和钒的测定准确性是可以接受的。

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