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电化学制备的三维还原氧化石墨烯-聚苯胺纳米复合材料作为固相微萃取涂层用于测定硫丹。

Electrochemically prepared three-dimensional reduced graphene oxide-polyaniline nanocomposite as a solid-phase microextraction coating for ethion determination.

机构信息

Department of Chemistry, Isfahan University of Technology, Isfahan, 84156-83111, Iran.

Department of Chemistry, Isfahan University of Technology, Isfahan, 84156-83111, Iran.

出版信息

Talanta. 2020 Mar 1;209:120576. doi: 10.1016/j.talanta.2019.120576. Epub 2019 Nov 21.

Abstract

Here, a three-dimensional reduced graphene oxide-polyaniline nanocomposite was synthesized and applied as a sorbent for solid-phase microextraction of ethion from water samples followed by negative corona discharge ionization ion mobility spectrometry. The nanocomposite was synthesized via a fast and facile two-step electrochemical method. The prepared sorbent was characterized by Fourier transform infrared spectroscopy, field emission scanning electron microscopy and thermogravimetric analysis. The main experimental parameters in the preparation of the fiber including concentration of graphene oxide, electrodeposition time, aniline concentration, and electropolymerization time were investigated. Also, parameters affecting the extraction process (i.e., salt addition, sample stirring rate, solution pH, extraction temperature and extraction time) were studied. Under the optimal conditions, the linearity and limit of detection were found to be 1.0-70 and 0.4 μg L, respectively. The method presented good precision (intra-day and inter-day, n = 3), ranged from 1.7 to 4.7%. The analyte recovery obtained using spiked real water samples were in the range of 84-98%.

摘要

在这里,合成了一种三维还原氧化石墨烯-聚苯胺纳米复合材料,并将其用作固相微萃取的吸附剂,从水样中萃取乙硫磷,然后采用负电晕放电电离离子迁移谱法进行分析。该纳米复合材料是通过快速简便的两步电化学方法合成的。采用傅里叶变换红外光谱、场发射扫描电子显微镜和热重分析对制备的吸附剂进行了表征。还研究了纤维制备过程中的主要实验参数(氧化石墨烯浓度、电沉积时间、苯胺浓度和电聚合时间)。此外,还研究了影响萃取过程的参数(加盐量、样品搅拌速度、溶液 pH 值、萃取温度和萃取时间)。在最佳条件下,发现线性范围和检测限分别为 1.0-70 和 0.4μg/L。该方法具有良好的精密度(日内和日间,n=3),范围为 1.7-4.7%。使用加标实际水样进行分析,得到的分析物回收率在 84-98%范围内。

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