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

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 a...

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Autores principales: Katarzyna Tyszczuk-Rotko, Rafał Olchowski, Jędrzej Kozak, Olga Sekerzh-Zenkovich, Ryszard Dobrowolski
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Publicado: MDPI AG 2021
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spelling oai:doaj.org-article:2080ab03a7254b5faf5d2cca701f49172021-11-11T18:03:59ZModified 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 Determination10.3390/ma142164901996-1944https://doaj.org/article/2080ab03a7254b5faf5d2cca701f49172021-10-01T00:00:00Zhttps://www.mdpi.com/1996-1944/14/21/6490https://doaj.org/toc/1996-1944In 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).Katarzyna Tyszczuk-RotkoRafał OlchowskiJędrzej KozakOlga Sekerzh-ZenkovichRyszard DobrowolskiMDPI AGarticledicyandiamide-impregnated mesoporous carbonelectrochemically lead film depositedvoltammetric sensorultratrace U(V) determinationTechnologyTElectrical engineering. Electronics. Nuclear engineeringTK1-9971Engineering (General). Civil engineering (General)TA1-2040MicroscopyQH201-278.5Descriptive and experimental mechanicsQC120-168.85ENMaterials, Vol 14, Iss 6490, p 6490 (2021)
institution DOAJ
collection DOAJ
language EN
topic dicyandiamide-impregnated mesoporous carbon
electrochemically lead film deposited
voltammetric sensor
ultratrace U(V) determination
Technology
T
Electrical engineering. Electronics. Nuclear engineering
TK1-9971
Engineering (General). Civil engineering (General)
TA1-2040
Microscopy
QH201-278.5
Descriptive and experimental mechanics
QC120-168.85
spellingShingle dicyandiamide-impregnated mesoporous carbon
electrochemically lead film deposited
voltammetric sensor
ultratrace U(V) determination
Technology
T
Electrical engineering. Electronics. Nuclear engineering
TK1-9971
Engineering (General). Civil engineering (General)
TA1-2040
Microscopy
QH201-278.5
Descriptive and experimental mechanics
QC120-168.85
Katarzyna Tyszczuk-Rotko
Rafał Olchowski
Jędrzej Kozak
Olga Sekerzh-Zenkovich
Ryszard Dobrowolski
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
description 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).
format article
author Katarzyna Tyszczuk-Rotko
Rafał Olchowski
Jędrzej Kozak
Olga Sekerzh-Zenkovich
Ryszard Dobrowolski
author_facet Katarzyna Tyszczuk-Rotko
Rafał Olchowski
Jędrzej Kozak
Olga Sekerzh-Zenkovich
Ryszard Dobrowolski
author_sort Katarzyna Tyszczuk-Rotko
title 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
title_short 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
title_full 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
title_fullStr 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
title_full_unstemmed 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
title_sort 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
publisher MDPI AG
publishDate 2021
url https://doaj.org/article/2080ab03a7254b5faf5d2cca701f4917
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