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首页> 外文期刊>Analytica chimica acta >Valence properties of tellurium in different chemical systems and its determination in refractory environmental samples using hydride generation - Atomic fluorescence spectroscopy
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Valence properties of tellurium in different chemical systems and its determination in refractory environmental samples using hydride generation - Atomic fluorescence spectroscopy

机译:氢化物发生-不同化学体系中碲的价性质及其在难处理环境样品中的测定-原子荧光光谱法。

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Using HG - AFS as a powerful tool to study valence transformations of Te, we found that, in presence of HCl and at high temperature, Te can form volatile species and be lost during sample digestion and pre-reduction steps. It was also noticed that the chemical valences of Te can be modified under different chemical and digestion conditions and even by samples themselves with certain matrices. KBr can reduce Te(VI) to Te(IV) in 3.0 M HCl at 100 degrees C, but when HNO3 was > 5% (v/v) in solution, Br-2 was formed and caused serious interference to Te measurements. HCl alone can also pre-reduce Te(VI) to Te(IV), only when its concentration was >= 6.0 M (100 degrees C for 15 min). Among 10 studied chemical elements, only Cu2+ caused severe interference. Thiourea is an effective masking agent only when Cu2+ concentration is equal or lower than 10 mg/L. Chemical reagents, chemical composition of sample, as well as the modes of digestion can greatly affect Te valences, reagent blanks and analytical precisions. A protocol of 2-step-digestion followed by an elimination of HF is proposed to minimize reagent blank and increase the signaloise ratios. It is important to perform a preliminary test to confirm whether a pre-reduction step is necessary; this is especially true for samples with complex matrices such as those with high sulfide content. The analytical detection limits of this method in a pure solution and a solid sample were 100 ng/L and 0.10 +/- 0.02 mu g/g, respectively. (C) 2015 Elsevier B.V. All rights reserved.
机译:使用HG-AFS作为研究Te的价态转化的有力工具,我们发现,在HCl存在下和高温下,Te会形成挥发性物质,并在样品消化和预还原步骤中丢失。还应注意的是,Te的化学价可以在不同的化学和消化条件下甚至通过具有某些基质的样品本身进行修饰。 KBr可以在100摄氏度下于3.0 M HCl中将Te(VI)还原为Te(IV),但当溶液中HNO3含量> 5%(v / v)时,会形成Br-2,并严重干扰了Te的测量。仅当浓度大于等于6.0 M(100摄氏度,持续15分钟)时,单独的HCl还能将Te(VI)还原为Te(IV)。在研究的10种化学元素中,只有Cu2 +引起严重干扰。仅当Cu2 +浓度等于或低于10 mg / L时,硫脲才是有效的掩蔽剂。化学试剂,样品的化学成分以及消化方式会极大地影响分析价,试剂空白和分析精度。提出了两步消解并消除HF的方案,以最大程度地减少试剂空白并增加信噪比。进行初步测试以确认是否需要进行还原前的步骤非常重要;对于具有复杂基质(例如高硫化物含量)的样品,尤其如此。该方法在纯溶液和固体样品中的分析检出限分别为100 ng / L和0.10 +/- 0.02μg / g。 (C)2015 Elsevier B.V.保留所有权利。

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