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Application of a novel poly(SMAm)-Tris-Fe3O4 nanocomposite for selective extraction and enrichment of Cu(I) /Cu(II) from beer, soft drinks and wine samples, and speciation analysis by micro-volume UV–Vis spectrophotometry
Talanta ( IF 6.1 ) Pub Date : 2020-10-19 , DOI: 10.1016/j.talanta.2020.121789
H.B. Zengin , R. Gürkan

In this study, a novel functional nanocomposite was synthesized, characterized and selectively used in pH-controlled separation, pre-concentration and speciation analysis of Cu(I) and Cu(II) from sample matrices where extraction is assisted, facilitated and greatly enhanced by ultrasound energy. The hydrophilic composite material functionalized with tris(2-hydroxymethyl)aminomethane (Tris) and Fe3O4 NPs was characterized in detail by ATR-FT-IR, 1H NMR, XRD, EDX peaks and SEM images. After optimization of the main variables influencing extraction efficiency such as pH, volumes of buffer, modified copolymer in acetone, CTAB and Triton X-114 at fixed concentrations including sonication conditions, the Cu(I) and Cu(II) were monitored against a blank at 347 nm by micro-volume UV–vis spectrophotometer. A good linearity was obtained in the range of 2–140 and 5–150 μg L−1 for Cu(II) and Cu(I) with r2 ≥ 0.993. The limits of detection (LODs) of 0.66 and 1.60 μg L−1 for each analyte, were obtained from a pre-concentration of 70-fold. After validation, the method was applied to speciation of Cu(I), Cu(II), and total Cu in the pre-treated and diluted beverage samples before and after pre-oxidation of Cu(I) to Cu(II) due to be more sensitive of extraction process to Cu(II) at pH 6.0. The results were also compared with those obtained by FAAS analysis to ensure the reliability of the results. It was observed that there was a statistically good agreement between the results of both methods.



中文翻译:

新型聚(SMAm)-Tris-Fe 3 O 4纳米复合材料在啤酒,软饮料和葡萄酒样品中选择性提取和富集Cu(I)/ Cu(II)的应用以及通过微量UV-Vis进行形态分析分光光度法

在这项研究中,合成了一种新型的功能性纳米复合材料,对其进行了表征和选择,可用于从样品基质中辅助,促进和促进萃取的样品基质中的Cu(I)和Cu(II)的pH控制分离,预浓缩和形态分析。超声能量。用ATR-FT-IR,1表征了被三(2-羟甲基)氨基甲烷(Tris)和Fe 3 O 4 NPs功能化的亲水性复合材料。1 H NMR,XRD,EDX峰和SEM图像。优化影响萃取效率的主要变量(例如pH,缓冲液体积,丙酮中的改性共聚物,CTAB和Triton X-114)在固定浓度(包括超声处理条件)后,针对空白条件对Cu(I)和Cu(II)进行监测微型紫外可见分光光度计在347 nm下检测。在2-140和5-150微克L的范围内进行,得到良好的线性-1的Cu(I)对Cu(II)和随r 2  ≥0.993。检测限(LOD)为0.66和1.60μgL -1对于每种分析物,均从70倍的预浓缩中获得。验证后,该方法适用于在预处理和稀释饮料样品中将Cu(I)预氧化为Cu(II)之前和之后的Cu(I),Cu(II)和总Cu的形态。在pH 6.0时对铜(II)的提取过程更敏感。还将结果与通过FAAS分析获得的结果进行比较,以确保结果的可靠性。据观察,两种方法的结果在统计学上都很好地吻合。

更新日期:2020-10-30
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