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超声辅助分散磁固相萃取法预富集和测定食品样品及水溶液中痕量汞(II)离子:基于中心复合设计优化的磁性氧化石墨烯(FeO@GO/2-PTSC)。

Ultrasound-assisted dispersive magnetic solid phase extraction for preconcentration and determination of trace amount of Hg (II) ions from food samples and aqueous solution by magnetic graphene oxide (FeO@GO/2-PTSC): Central composite design optimization.

机构信息

Research Laboratory of Spectrometry & Micro and Nano Extraction, Department of Chemistry, Iran University of Science and Technology, Tehran 16846-13114, Iran.

Research Laboratory of Spectrometry & Micro and Nano Extraction, Department of Chemistry, Iran University of Science and Technology, Tehran 16846-13114, Iran.

出版信息

Ultrason Sonochem. 2017 Sep;38:421-429. doi: 10.1016/j.ultsonch.2017.03.039. Epub 2017 Mar 23.

Abstract

In this work, the synthesis of the magnetic graphene oxide modified by 2-pyridinecarboxaldehyde thiosemicarbazone groups (FeO@GO/2-PTSC) was utilized for preconcentration and determination of mercuric ions in a trace amount by inductively coupled plasma-optical emission spectrometry (ICP-OES). Characterization of the adsorbent was performed using various techniques, such as FT-IR, VSM, SEM and XRD analysis. Central composite design (CCD) under response surface methodology (RSM) was used for obtaining the most important parameters and probable interactions in variables. The variables such as adsorbent dosage, pH, desorption time, and eluent volume was optimized. These values were 8mg, 5.4min, 0.5mL (HCl, 0.1M), respectively. Sonication had an important role in shortening the adsorption time of Hg (II) ions by enhancing the dispersion of adsorbent in solution. Under the optimal conditions, the proposed method presented high enrichment factor of 193, an extraction percentage of 96.5, a detection limit of 0.0079µgL and a relative standard deviation (RSD %) of 1.63%. Finally, the application of the synthesized material was evaluated for preconcentration and determination of mercuric ions from foods and environmental waters samples.

摘要

在这项工作中,利用 2-吡啶甲酰基缩氨硫脲修饰的磁性氧化石墨烯(FeO@GO/2-PTSC)合成物,通过电感耦合等离子体-光学发射光谱法(ICP-OES)对痕量汞离子进行预浓缩和测定。采用傅里叶变换红外光谱(FT-IR)、振动样品磁强计(VSM)、扫描电子显微镜(SEM)和 X 射线衍射(XRD)分析等多种技术对吸附剂进行了表征。在响应面法(RSM)下,采用中心复合设计(CCD)来获取变量中最重要的参数和可能的相互作用。优化了吸附剂用量、pH 值、解吸时间和洗脱体积等变量。这些值分别为 8mg、5.4min、0.5mL(HCl,0.1M)。超声在增强吸附剂在溶液中的分散性方面对缩短 Hg(II)离子的吸附时间起着重要作用。在最佳条件下,该方法的富集因子高达 193,提取率为 96.5%,检测限为 0.0079µgL,相对标准偏差(RSD%)为 1.63%。最后,评估了合成材料在食品和环境水样中预浓缩和测定汞离子的应用。

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