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通过硬模板法、双氰胺浸渍和电化学铅颗粒沉积制备的改性介孔碳材料（Pb-N-CMK-3）作为用于超痕量测定U(VI)的电极材料

Modified Mesoporous Carbon Material (Pb-N-CMK-3) Obtained by a Hard-Templating Route, Dicyandiamide Impregnation and Electrochemical Lead Particles Deposition as an Electrode Material for the U(VI) Ultratrace Determination.

作者信息

Tyszczuk-Rotko Katarzyna, Olchowski Rafał, Kozak Jędrzej, Sekerzh-Zenkovich Olga, Dobrowolski Ryszard

机构信息

Faculty of Chemistry, Institute of Chemical Sciences, Maria Curie-Skłodowska University, 20-031 Lublin, Poland.

出版信息

Materials (Basel). 2021 Oct 29;14(21):6490. doi: 10.3390/ma14216490.

DOI:10.3390/ma14216490
PMID:34772017
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8585121/
Abstract

In this paper, a dicyandiamide-impregnated mesoporous carbon (N-CMK-3), electrochemically modified in situ with lead film (Pb-N-CMK-3), was tested as an electrode material for U(VI) ultratrace determination. The prepared carbon material was characterized by XRD, SEM-EDX, Raman, FT-IR, XPS analysis and nitrogen sorption measurements. The changes of electrochemical properties of glassy carbon electrodes (GCE) after the N-CMK-3 and Pb-N-CMK-3 modification were studied using CV and EIS methods. The modification of the GCE surface by the N-CMK-3 material and Pb film increases the electroactive area of the electrode and decreases the charge transfer residence and is likely responsible for the electrochemical improvement of the U(VI) analytical signal. Using square-wave adsorptive stripping voltammetry (SWAdSV), two linear calibration ranges extending from 0.05 to 1.0 nM and from 1.0 to 10.0 nM were observed, coupled with the detection and quantification limits of 0.014 and 0.047 nM, respectively. The Pb-N-CMK-3/GCE was successfully applied for U(VI) determination in reference materials (estuarine water SLEW-3 and trace elements in natural water SRM 1640a).

摘要

在本文中，对一种用双氰胺浸渍的介孔碳（N-CMK-3）进行原位电化学铅膜修饰（Pb-N-CMK-3），并将其作为用于超痕量测定U(VI)的电极材料进行测试。通过X射线衍射（XRD）、扫描电子显微镜-能谱分析（SEM-EDX）、拉曼光谱、傅里叶变换红外光谱（FT-IR）、X射线光电子能谱（XPS）分析以及氮吸附测量对制备的碳材料进行表征。使用循环伏安法（CV）和电化学阻抗谱（EIS）方法研究了N-CMK-3和Pb-N-CMK-3修饰后玻碳电极（GCE）的电化学性质变化。N-CMK-3材料和铅膜对GCE表面的修饰增加了电极的电活性面积，减少了电荷转移电阻，这可能是U(VI)分析信号电化学性能改善的原因。使用方波吸附溶出伏安法（SWAdSV），观察到两个线性校准范围，分别从0.05到1.0 nM以及从1.0到10.0 nM，检测限和定量限分别为0.014和0.047 nM。Pb-N-CMK-3/GCE成功应用于参考物质（河口水样SLEW-3和天然水标准参考物质SRM 1640a中的痕量元素）中U(VI)的测定。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef9a/8585121/6705996a5ebb/materials-14-06490-g011.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef9a/8585121/6705996a5ebb/materials-14-06490-g011.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef9a/8585121/6705996a5ebb/materials-14-06490-g011.jpg

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