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铋的测定及干扰研究 - 氢化物发生原子吸收光谱法中的钨阱。

Determination and interference studies of bismuth by tungsten trap hydride generation atomic absorption spectrometry.

机构信息

Department of Chemistry, Muğla University, 48000 Muğla, Turkey.

出版信息

Talanta. 2009 Nov 15;80(1):127-32. doi: 10.1016/j.talanta.2009.06.084. Epub 2009 Aug 6.

Abstract

The determination of bismuth requires sufficiently sensitive procedures for detection at the microg L(-1) level or lower. W-coil was used for on-line trapping of volatile bismuth species using HGAAS (hydride generation atomic absorption spectrometry); atom trapping using a W-coil consists of three steps. Initially BiH(3) gas is formed by hydride generation procedure. The analyte species in vapor form are transported through the W-coil trap held at 289 degrees C where trapping takes place. Following the preconcentration step, the W-coil is heated to 1348 degrees C; analyte species are released and transported to flame-heated quartz atom cell where the atomic signal is formed. In our study, interferences have been investigated in detail during Bi determination by hydride generation, both with and without trap in the same HGAAS system. Interferent/analyte (mass/mass) ratio was kept at 1, 10 and 100. Experiments were designed for carrier solutions having 1.0M HNO(3). Interferents such as Fe, Mn, Zn, Ni, Cu, As, Se, Cd, Pb, Au, Na, Mg, Ca, chloride, sulfate and phosphate were examined. The calibration plot for an 8.0 mL sampling volume was linear between 0.10 microg L(-1) and 10.0 microg L(-1) of Bi. The detection limit (3s/m) was 25 ng L(-1). The enhancement factor for the characteristic concentration (C(o)) was found to be 21 when compared with the regular system without trap, by using peak height values. The validation of the procedure was performed by the analysis of the certified water reference material and the result was found to be in good agreement with the certified values at the 95% confidence level.

摘要

铋的测定需要足够灵敏的检测程序,以达到微升(μg/L)级或更低的水平。使用钨丝线圈(W-coil)通过氢化物发生原子吸收光谱法(HGAAS)在线捕获挥发性铋物种;使用钨丝线圈进行原子捕集包括三个步骤。最初,通过氢化物发生程序形成 BiH3 气体。蒸气形式的分析物物种通过 W 线圈捕集器传输,该捕集器在 289°C 下保持捕集状态。在预浓缩步骤之后,将 W 线圈加热至 1348°C;分析物物种被释放并传输到火焰加热的石英原子室,在那里形成原子信号。在我们的研究中,在使用和不使用同一 HGAAS 系统中的捕集器的情况下,详细研究了氢化物生成法测定铋时的干扰。干扰物/分析物(质量/质量)比保持在 1、10 和 100。实验设计用于含有 1.0M HNO3 的载液。研究了铁、锰、锌、镍、铜、砷、硒、镉、铅、金、钠、镁、钙、氯化物、硫酸盐和磷酸盐等干扰物。对于 8.0mL 采样体积,校准曲线在 0.10μg/L 至 10.0μg/L 的 Bi 范围内呈线性。检测限(3s/m)为 25ng/L。与没有捕集器的常规系统相比,使用峰高值,特征浓度(C(o))的增强因子为 21。通过对认证水参考物质的分析验证了该程序的有效性,结果在 95%置信水平下与认证值吻合良好。

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