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发展一种在线温度辅助离子液体分散微萃取系统,用于环境和生物样品中钒的灵敏测定。

Development of an on-line temperature-assisted ionic liquid dispersive microextraction system for sensitive determination of vanadium in environmental and biological samples.

机构信息

Analytical Chemistry Research and Development Group (QUIANID), LISAMEN-CCT-CONICET-Mendoza, Av. Ruiz Leal S/N Parque General San Martín, M 5502 IRA Mendoza, Argentina.

出版信息

J Hazard Mater. 2010 Apr 15;176(1-3):721-8. doi: 10.1016/j.jhazmat.2009.11.094. Epub 2009 Nov 24.

Abstract

An original flow injection (FI) system was developed for on-line microextraction of Vanadium (V) based on room temperature ionic liquid (RTIL). Vanadium was complexed with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) at pH 4.0. A 40 microL-volume of 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]) RTIL was mixed with 5 mL of sample solution containing the V-5-Br-PADAP complex. Then, a fully on-line temperature-assisted dispersion procedure was developed, followed by, analyte microextraction; and final on-line separation of the RTIL phase with a florisil-containing microcolumn. Vanadium was removed from the microcolumn with a 10% (v/v) nitric acid (in acetone) solution, and finally measured by electrothermal atomic absorption spectrometry (ETAAS). The detection limit achieved after preconcentration of 5 mL of sample solution, was 4.8 ng L(-1). The relative standard deviation (RSD) for 10 replicate determinations at 5 microg L(-1) of vanadium level was 4.1%, calculated from the obtained peak heights. The calibration graph was linear, with a correlation coefficient of 0.9982 at levels from the detection limits up to 15 microg L(-1). The method was successfully applied for the determination of vanadium in environmental and biological samples.

摘要

一种基于室温离子液体(RTIL)的在线微萃取钒(V)的原始流动注射(FI)系统被开发出来。在 pH 4.0 时,钒与 2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)络合。将 40 μL 的 1-丁基-3-甲基咪唑六氟磷酸盐([C(4)mim][PF(6)])RTIL 与 5 mL 含有 V-5-Br-PADAP 配合物的样品溶液混合。然后,开发了一种完全在线温度辅助分散程序,接着进行分析物微萃取;最后通过含氟硅土的微柱在线分离 RTIL 相。钒从微柱上用 10%(v/v)硝酸(丙酮)溶液洗脱,最后用电热原子吸收光谱法(ETAAS)测量。在预浓缩 5 mL 样品溶液后,检测限达到 4.8 ng L(-1)。在 5 μg L(-1)的钒水平下,10 次重复测定的相对标准偏差(RSD)为 4.1%,根据得到的峰高计算得出。校准曲线是线性的,在检测限到 15 μg L(-1)的水平上相关系数为 0.9982。该方法成功地应用于环境和生物样品中钒的测定。

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