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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Main Authors: Katarzyna Tyszczuk-Rotko, Rafał Olchowski, Jędrzej Kozak, Olga Sekerzh-Zenkovich, Ryszard Dobrowolski
Format: Article
Language:English
Published: MDPI AG 2021-10-01
Series:Materials
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Online Access:https://www.mdpi.com/1996-1944/14/21/6490
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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
collection DOAJ
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).
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spelling doaj.art-2080ab03a7254b5faf5d2cca701f49172023-11-22T21:12:58ZengMDPI AGMaterials1996-19442021-10-011421649010.3390/ma14216490Modified 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 DeterminationKatarzyna Tyszczuk-Rotko0Rafał Olchowski1Jędrzej Kozak2Olga Sekerzh-Zenkovich3Ryszard Dobrowolski4Faculty of Chemistry, Institute of Chemical Sciences, Maria Curie-Skłodowska University, 20-031 Lublin, PolandFaculty of Chemistry, Institute of Chemical Sciences, Maria Curie-Skłodowska University, 20-031 Lublin, PolandFaculty of Chemistry, Institute of Chemical Sciences, Maria Curie-Skłodowska University, 20-031 Lublin, PolandFaculty of Chemistry, Institute of Chemical Sciences, Maria Curie-Skłodowska University, 20-031 Lublin, PolandFaculty of Chemistry, Institute of Chemical Sciences, Maria Curie-Skłodowska University, 20-031 Lublin, PolandIn 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).https://www.mdpi.com/1996-1944/14/21/6490dicyandiamide-impregnated mesoporous carbonelectrochemically lead film depositedvoltammetric sensorultratrace U(V) determination
spellingShingle 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
Materials
dicyandiamide-impregnated mesoporous carbon
electrochemically lead film deposited
voltammetric sensor
ultratrace U(V) determination
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_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_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_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
topic dicyandiamide-impregnated mesoporous carbon
electrochemically lead film deposited
voltammetric sensor
ultratrace U(V) determination
url https://www.mdpi.com/1996-1944/14/21/6490
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