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基于固相萃取-流动注射在线衍生荧光法测定水样中 Cr(III)和 Cr(VI)

Flow injection microfluidic device with on-line fluorescent derivatization for the determination of Cr(III) and Cr(VI) in water samples after solid phase extraction.

机构信息

Key Laboratory of Eco-Environment of Three Gorges Region of Ministry of Education, Chongqing University, Chongqing, 400045, China; Department of Chemistry, Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Tsinghua University, Beijing, 100084, China.

Key Laboratory of Eco-Environment of Three Gorges Region of Ministry of Education, Chongqing University, Chongqing, 400045, China.

出版信息

Anal Chim Acta. 2017 Feb 22;955:58-66. doi: 10.1016/j.aca.2016.11.057. Epub 2016 Dec 2.

Abstract

In this paper, a rapid and simple method using magnetic multi-walled carbon nanotubes (MWCNTS), as a solid-phase extraction (SPE) sorbent, was successfully developed for extraction and preconcentration trace amounts of Cr(III) in water samples. The synthesized magnetic-MWCNTs nanocomposite was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). A rhodamine derivative (R1) was synthesized and characterized as a highly selective and sensitive fluorescent derivatizing agent for Cr(III). After SPE procedure, Cr(III) analysis was performed by flow injection microfluidic chip with on-line fluorescent derivatization and laser-induced fluorescence (LIF) spectroscopy detection. The parameters, which affected the efficiency of the developed method were investigated and optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 0-10.0 nM, with a detection limit of 0.094 nM and an enrichment factor of 38. Furthermore, real water samples were analyzed and good recoveries were obtained from 91.0 to 101.6%.

摘要

本文采用磁性多壁碳纳米管(MWCNTs)作为固相萃取(SPE)吸附剂,成功开发了一种快速、简单的方法,用于萃取和预浓缩水样中痕量的 Cr(III)。合成的磁性 MWCNTs 纳米复合材料通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、X 射线光电子能谱(XPS)和 X 射线衍射(XRD)进行了表征。合成了一种罗丹明衍生物(R1),并将其作为一种高选择性和高灵敏度的荧光衍生化剂用于 Cr(III)分析。在 SPE 程序之后,通过流动注射微流控芯片与在线荧光衍生化和激光诱导荧光(LIF)光谱检测进行 Cr(III)分析。研究并优化了影响开发方法效率的参数。在优化条件下,该方法的线性动态范围为 0-10.0 nM,检测限为 0.094 nM,富集因子为 38。此外,还对实际水样进行了分析,回收率在 91.0%至 101.6%之间。

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