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石墨烯/Fe3O4@聚噻吩纳米复合材料的制备及其在环境水样中多环芳烃磁性固相萃取中的应用。

Fabrication of graphene/Fe3O4@polythiophene nanocomposite and its application in the magnetic solid-phase extraction of polycyclic aromatic hydrocarbons from environmental water samples.

作者信息

Mehdinia Ali, Khodaee Nader, Jabbari Ali

机构信息

Department of Marine Science, Iranian National Institute for Oceanography and Atmospheric Science, Tehran, Iran.

Department of Chemistry, Faculty of Science, K. N. Toosi University of Technology, Tehran, Iran.

出版信息

Anal Chim Acta. 2015 Apr 8;868:1-9. doi: 10.1016/j.aca.2014.12.022. Epub 2014 Dec 17.

DOI:10.1016/j.aca.2014.12.022
PMID:25813229
Abstract

Polythiophene (PT) was used as a surface modifier of graphene/Fe3O4 (G/Fe3O4) composite to increase merit of it, and also overcome some limitations and disadvantages of using G/Fe3O4 alone as solid phase extraction (SPE) sorbent. An in-situ chemical polymerization method was employed to prepare G/Fe3O4@PT nanocomposites. Application of this newly designed material in the magnetic SPE (MSPE) of polycyclic aromatic hydrocarbons (PAHs), as model analytes, in the environmental water samples was investigated. The characterization of the hybrid material was performed using transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray analysis, Fourier transform-infrared (FT-IR) spectroscopy and vibrating sample magnetometry. Seven important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent, initial sample volume and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 4 min for extraction time, 20 mg for sorbent amount, 100mL for initial sample volume, toluene as desorption solvent, 0.6 mL for desorption solvent volume, 6 min for desorption time and 30% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. Detection limits were in the range of 0.009-0.020 μg L(-1) in the real matrix. The calibration curves were linear over the concentration ranges from 0.03 to 80 μg L(-1) with correlation coefficients (R(2)) between 0.995 and 0.998 for all the analytes. Relative standard deviations were ranged from 4.3 to 6.3%. Appropriate recovery values, in the range of 83-107%, were also obtained for the real sample analysis.

摘要

聚噻吩(PT)被用作石墨烯/四氧化三铁(G/Fe3O4)复合材料的表面改性剂,以提高其性能,同时克服单独使用G/Fe3O4作为固相萃取(SPE)吸附剂的一些局限性和缺点。采用原位化学聚合法制备了G/Fe3O4@PT纳米复合材料。研究了这种新设计的材料在环境水样中作为多环芳烃(PAHs)模型分析物的磁性固相萃取(MSPE)中的应用。使用透射电子显微镜、扫描电子显微镜、能量色散X射线分析、傅里叶变换红外(FT-IR)光谱和振动样品磁强计对杂化材料进行了表征。评估了影响PAHs萃取效率的七个重要参数,包括:吸附剂用量、吸附和解吸时间、洗脱溶剂的类型和体积、初始样品体积和样品的盐含量。获得的最佳萃取条件为:萃取时间4分钟,吸附剂用量20毫克,初始样品体积100毫升,甲苯作为解吸溶剂,解吸溶剂体积0.6毫升,解吸时间6分钟,NaCl浓度30%(w/v)。在优化条件下获得了良好的性能数据。在实际基质中的检测限为0.009-0.020μg L(-1)。校准曲线在0.03至80μg L(-1)的浓度范围内呈线性,所有分析物的相关系数(R(2))在0.995至0.998之间。相对标准偏差范围为4.3至6.3%。实际样品分析也获得了83-107%范围内的适当回收率值。

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