Electrochemical Sensing of Pb<sup>2+</sup> and Cd<sup>2+</sup> Ions with the Use of Electrode Modified with Carbon-Covered Halloysite and Carbon Nanotubes

A novel voltammetric method for the sensitive and selective determination of cadmium and lead ions using screen-printed carbon electrodes (SPCEs) modified with carbon-deposited natural halloysite (C_Hal) and multi-walled carbon nanotubes (MWCNTs) was developed. The electrochemical properties of the...

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Main Authors: Paweł Knihnicki, Aleksandra Skrzypek, Małgorzata Jakubowska, Radosław Porada, Anna Rokicińska, Piotr Kuśtrowski, Paweł Kościelniak, Jolanta Kochana
Format: Article
Language:English
Published: MDPI AG 2022-07-01
Series:Molecules
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Online Access:https://www.mdpi.com/1420-3049/27/14/4608
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author Paweł Knihnicki
Aleksandra Skrzypek
Małgorzata Jakubowska
Radosław Porada
Anna Rokicińska
Piotr Kuśtrowski
Paweł Kościelniak
Jolanta Kochana
author_facet Paweł Knihnicki
Aleksandra Skrzypek
Małgorzata Jakubowska
Radosław Porada
Anna Rokicińska
Piotr Kuśtrowski
Paweł Kościelniak
Jolanta Kochana
author_sort Paweł Knihnicki
collection DOAJ
description A novel voltammetric method for the sensitive and selective determination of cadmium and lead ions using screen-printed carbon electrodes (SPCEs) modified with carbon-deposited natural halloysite (C_Hal) and multi-walled carbon nanotubes (MWCNTs) was developed. The electrochemical properties of the proposed sensor were investigated by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV), while the morphology and structure were established by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). A two-factorial central composite design (CCD) was employed to select the composition of the nanocomposite modifying the electrode surface. The optimal measuring parameters of differential pulse anodic stripping voltammetry (DPASV) used for quantitative analysis were established with the Nelder–Mead simplex method. In the analytical investigation of Cd(II) and Pb(II) ions by DPASV, the MWCNTs/C_Hal/Nafion/SPCE exhibited a linear response in the concentration range of 0.1–10.0 µmol L<sup>−1</sup> (for both ions) with a detection limit of 0.0051 and 0.0106 µmol L<sup>−1</sup> for Pb(II) and Cd(II), respectively. The proposed sensor was successfully applied for the determination of metal ions in different natural water and honey samples with recovery values of 96.4–101.6%.
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spelling doaj.art-42199cde7c6a418a9f9857f8de42c1f72023-12-03T12:02:19ZengMDPI AGMolecules1420-30492022-07-012714460810.3390/molecules27144608Electrochemical Sensing of Pb<sup>2+</sup> and Cd<sup>2+</sup> Ions with the Use of Electrode Modified with Carbon-Covered Halloysite and Carbon NanotubesPaweł Knihnicki0Aleksandra Skrzypek1Małgorzata Jakubowska2Radosław Porada3Anna Rokicińska4Piotr Kuśtrowski5Paweł Kościelniak6Jolanta Kochana7Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Gronostajowa 2, 30-387 Krakow, PolandDepartment of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Gronostajowa 2, 30-387 Krakow, PolandFaculty of Materials and Ceramics, AGH University of Science and Technology, A. Mickiewicza 30, 30-059 Krakow, PolandFaculty of Materials and Ceramics, AGH University of Science and Technology, A. Mickiewicza 30, 30-059 Krakow, PolandDepartment of Chemical Technology, Faculty of Chemistry, Jagiellonian University, Gronostajowa 2, 30-387 Krakow, PolandDepartment of Chemical Technology, Faculty of Chemistry, Jagiellonian University, Gronostajowa 2, 30-387 Krakow, PolandDepartment of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Gronostajowa 2, 30-387 Krakow, PolandDepartment of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Gronostajowa 2, 30-387 Krakow, PolandA novel voltammetric method for the sensitive and selective determination of cadmium and lead ions using screen-printed carbon electrodes (SPCEs) modified with carbon-deposited natural halloysite (C_Hal) and multi-walled carbon nanotubes (MWCNTs) was developed. The electrochemical properties of the proposed sensor were investigated by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV), while the morphology and structure were established by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). A two-factorial central composite design (CCD) was employed to select the composition of the nanocomposite modifying the electrode surface. The optimal measuring parameters of differential pulse anodic stripping voltammetry (DPASV) used for quantitative analysis were established with the Nelder–Mead simplex method. In the analytical investigation of Cd(II) and Pb(II) ions by DPASV, the MWCNTs/C_Hal/Nafion/SPCE exhibited a linear response in the concentration range of 0.1–10.0 µmol L<sup>−1</sup> (for both ions) with a detection limit of 0.0051 and 0.0106 µmol L<sup>−1</sup> for Pb(II) and Cd(II), respectively. The proposed sensor was successfully applied for the determination of metal ions in different natural water and honey samples with recovery values of 96.4–101.6%.https://www.mdpi.com/1420-3049/27/14/4608halloysitesensorcadmiumlead
spellingShingle Paweł Knihnicki
Aleksandra Skrzypek
Małgorzata Jakubowska
Radosław Porada
Anna Rokicińska
Piotr Kuśtrowski
Paweł Kościelniak
Jolanta Kochana
Electrochemical Sensing of Pb<sup>2+</sup> and Cd<sup>2+</sup> Ions with the Use of Electrode Modified with Carbon-Covered Halloysite and Carbon Nanotubes
Molecules
halloysite
sensor
cadmium
lead
title Electrochemical Sensing of Pb<sup>2+</sup> and Cd<sup>2+</sup> Ions with the Use of Electrode Modified with Carbon-Covered Halloysite and Carbon Nanotubes
title_full Electrochemical Sensing of Pb<sup>2+</sup> and Cd<sup>2+</sup> Ions with the Use of Electrode Modified with Carbon-Covered Halloysite and Carbon Nanotubes
title_fullStr Electrochemical Sensing of Pb<sup>2+</sup> and Cd<sup>2+</sup> Ions with the Use of Electrode Modified with Carbon-Covered Halloysite and Carbon Nanotubes
title_full_unstemmed Electrochemical Sensing of Pb<sup>2+</sup> and Cd<sup>2+</sup> Ions with the Use of Electrode Modified with Carbon-Covered Halloysite and Carbon Nanotubes
title_short Electrochemical Sensing of Pb<sup>2+</sup> and Cd<sup>2+</sup> Ions with the Use of Electrode Modified with Carbon-Covered Halloysite and Carbon Nanotubes
title_sort electrochemical sensing of pb sup 2 sup and cd sup 2 sup ions with the use of electrode modified with carbon covered halloysite and carbon nanotubes
topic halloysite
sensor
cadmium
lead
url https://www.mdpi.com/1420-3049/27/14/4608
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AT aleksandraskrzypek electrochemicalsensingofpbsup2supandcdsup2supionswiththeuseofelectrodemodifiedwithcarboncoveredhalloysiteandcarbonnanotubes
AT małgorzatajakubowska electrochemicalsensingofpbsup2supandcdsup2supionswiththeuseofelectrodemodifiedwithcarboncoveredhalloysiteandcarbonnanotubes
AT radosławporada electrochemicalsensingofpbsup2supandcdsup2supionswiththeuseofelectrodemodifiedwithcarboncoveredhalloysiteandcarbonnanotubes
AT annarokicinska electrochemicalsensingofpbsup2supandcdsup2supionswiththeuseofelectrodemodifiedwithcarboncoveredhalloysiteandcarbonnanotubes
AT piotrkustrowski electrochemicalsensingofpbsup2supandcdsup2supionswiththeuseofelectrodemodifiedwithcarboncoveredhalloysiteandcarbonnanotubes
AT pawełkoscielniak electrochemicalsensingofpbsup2supandcdsup2supionswiththeuseofelectrodemodifiedwithcarboncoveredhalloysiteandcarbonnanotubes
AT jolantakochana electrochemicalsensingofpbsup2supandcdsup2supionswiththeuseofelectrodemodifiedwithcarboncoveredhalloysiteandcarbonnanotubes