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Determination of Bismuth by Dielectric Barrier Discharge Atomic Absorption Spectrometry Coupled with Hydride Generation: Method Optimization and Evaluation of Analytical Performance

机译:介质阻挡放电原子吸收光谱-氢化物发生法测定铋的方法优化与分析性能评价

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摘要

Atomization of bismuth hydride in a 17 W planar quartz dielectric barrier discharge (DBD) atomizer was optimized and the performance of this device compared to that of a conventional quartz tube atomizer (QTA) for atomic absorption spectrometry (AAS). Modification of the inner surface of the DBD atomizer using dimethyldichlorsilane (DMDCS) was essential since it improved sensitivity by a factor of 2-4. Argon, at a flow rate of 125 mL min~(-1), was the best DBD discharge gas. Free Bi atoms were also observed in the DBD with nitrogen, hydrogen, and helium discharge gases but not in air. The detection limit for Bi (1.1 ng mL~(-1)) is worse than with the QTA (0.16 ng mL~(-1) Bi). A poorer detection limit compared to a QTA is a consequence of the shorter optical path of the DBD. Moreover, the lower atomization efficiency and/or faster decay of free atoms in the DBD has to be considered. The performance of the DBD as an atomizer reflects both effects, i.e., atomization efficiency and free atom decay, was estimated to be 65% of that of the externally heated quartz tube atomizer. Nevertheless, this hydride generation DBD-AAS approach can be used for the routine determination of Bi, providing repeatability and accuracy comparable to that reached with a QTA, as demonstrated by analysis of NIST SRM 1643e (trace elements in water). The potential of in-atomizer preconcentration in a DBD atomizer is outlined.
机译:优化了17 W平面石英介电势垒放电(DBD)雾化器中氢化铋的雾化,并且与用于原子吸收光谱(AAS)的常规石英管雾化器(QTA)相比,该设备的性能更高。使用二甲基二氯硅烷(DMDCS)修改DBD雾化器内表面至关重要,因为它可以将灵敏度提高2-4倍。氩气流速为125 mL min〜(-1),是最佳的DBD排放气体。在含氮,氢和氦放电气体的DBD中也观察到了游离Bi原子,但在空气中没有。 Bi(1.1 ng mL〜(-1)Bi)的检出限差于QTA(0.16 ng mL〜(-1)Bi)的检出限。与QTA相比,检测限较差是DBD光路较短的结果。此外,必须考虑DBD中较低的雾化效率和/或自由原子更快的衰减。 DBD作为雾化器的性能反映了两种效果,即雾化效率和自由原子衰减,估计为外部加热的石英管雾化器的65%。尽管如此,这种氢化物生成DBD-AAS方法仍可用于Bi的常规测定,其可重复性和准确性与QTA相当,如NIST SRM 1643e(水中痕量元素)的分析所证明的。概述了DBD雾化器中雾化器内预浓缩的潜力。

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