An innovative pretreatment protocol to eliminate silver contamination-induced voltammetric interference on graphite-glass working electrode

In the last decades, a significant amount of research has been focused on the development of miniaturized and portable electrochemical sensors in the form of screen-printed electrodes (SPEs). When performing voltammetric measurements using SPEs, especially in the case of carbon-based electrodes, add...

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Main Authors: Maksimiljan Dekleva, Marija Kovačević, Ema Gričar, Mitja Kolar, Boštjan Genorio, Barbara Repič, Danjela Kuščer, Helena Prosen, Gregor Marolt
Format: Article
Language:English
Published: Elsevier 2024-05-01
Series:Electrochemistry Communications
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S138824812400050X
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author Maksimiljan Dekleva
Marija Kovačević
Ema Gričar
Mitja Kolar
Boštjan Genorio
Barbara Repič
Danjela Kuščer
Helena Prosen
Gregor Marolt
author_facet Maksimiljan Dekleva
Marija Kovačević
Ema Gričar
Mitja Kolar
Boštjan Genorio
Barbara Repič
Danjela Kuščer
Helena Prosen
Gregor Marolt
author_sort Maksimiljan Dekleva
collection DOAJ
description In the last decades, a significant amount of research has been focused on the development of miniaturized and portable electrochemical sensors in the form of screen-printed electrodes (SPEs). When performing voltammetric measurements using SPEs, especially in the case of carbon-based electrodes, additional peaks can appear and overlap with analytes’ signals or otherwise interfere with results. Therefore, the development of pretreatment methods that enable the removal of interferences is of great importance for SPEs utilization, e.g. for sensor applications. Moreover, electrode pretreatment can also be used to improve electron transfer kinetics, including reversibility of the studied redox processes. In this work, we present the evaluation of different pretreatment methods using cyclic voltammetry and potentiostatic anodization, applied on an in-house graphite-glass composite working electrodes. With the use of X-ray photoelectron spectroscopy and scanning electron microscopy it was confirmed that the surface of working electrode was contaminated by sub-micrometer sized silver particles, which resulted in two interference peaks. Several strong acids, including H2SO4, HNO3, and HCl, as well as phosphate buffer solution, were evaluated as electrolytes for electrochemical pretreatment. A rapid, simple, and low-cost pretreatment protocol that enables the removal of the interference peaks, as well as improved voltammetric signals for [Fe(CN)6]3−/4− redox probe was developed. We propose the optimal pretreatment method in H2SO4 as a protocol that could be universally applied for carbon, carbon-glass, or similar types of SPEs before performing voltammetric experiments and/or further modifications of SPEs.
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spelling doaj.art-e745849587db44fc825384a65e40b5f92024-04-06T04:39:38ZengElsevierElectrochemistry Communications1388-24812024-05-01162107707An innovative pretreatment protocol to eliminate silver contamination-induced voltammetric interference on graphite-glass working electrodeMaksimiljan Dekleva0Marija Kovačević1Ema Gričar2Mitja Kolar3Boštjan Genorio4Barbara Repič5Danjela Kuščer6Helena Prosen7Gregor Marolt8University of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna pot 113, Ljubljana, SloveniaUniversity of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna pot 113, Ljubljana, SloveniaUniversity of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna pot 113, Ljubljana, SloveniaUniversity of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna pot 113, Ljubljana, SloveniaUniversity of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna pot 113, Ljubljana, SloveniaJožef Stefan Institute, Electronic Ceramics Department, Jamova cesta 39, Ljubljana, Slovenia; Jožef Stefan International Postgraduate School, Jamova cesta 39, Ljubljana, SloveniaJožef Stefan Institute, Electronic Ceramics Department, Jamova cesta 39, Ljubljana, Slovenia; Jožef Stefan International Postgraduate School, Jamova cesta 39, Ljubljana, SloveniaUniversity of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna pot 113, Ljubljana, SloveniaUniversity of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna pot 113, Ljubljana, Slovenia; Corresponding author.In the last decades, a significant amount of research has been focused on the development of miniaturized and portable electrochemical sensors in the form of screen-printed electrodes (SPEs). When performing voltammetric measurements using SPEs, especially in the case of carbon-based electrodes, additional peaks can appear and overlap with analytes’ signals or otherwise interfere with results. Therefore, the development of pretreatment methods that enable the removal of interferences is of great importance for SPEs utilization, e.g. for sensor applications. Moreover, electrode pretreatment can also be used to improve electron transfer kinetics, including reversibility of the studied redox processes. In this work, we present the evaluation of different pretreatment methods using cyclic voltammetry and potentiostatic anodization, applied on an in-house graphite-glass composite working electrodes. With the use of X-ray photoelectron spectroscopy and scanning electron microscopy it was confirmed that the surface of working electrode was contaminated by sub-micrometer sized silver particles, which resulted in two interference peaks. Several strong acids, including H2SO4, HNO3, and HCl, as well as phosphate buffer solution, were evaluated as electrolytes for electrochemical pretreatment. A rapid, simple, and low-cost pretreatment protocol that enables the removal of the interference peaks, as well as improved voltammetric signals for [Fe(CN)6]3−/4− redox probe was developed. We propose the optimal pretreatment method in H2SO4 as a protocol that could be universally applied for carbon, carbon-glass, or similar types of SPEs before performing voltammetric experiments and/or further modifications of SPEs.http://www.sciencedirect.com/science/article/pii/S138824812400050XScreen-printed electrodeGraphite-glass compositeElectrochemical pretreatmentSilver contamination
spellingShingle Maksimiljan Dekleva
Marija Kovačević
Ema Gričar
Mitja Kolar
Boštjan Genorio
Barbara Repič
Danjela Kuščer
Helena Prosen
Gregor Marolt
An innovative pretreatment protocol to eliminate silver contamination-induced voltammetric interference on graphite-glass working electrode
Electrochemistry Communications
Screen-printed electrode
Graphite-glass composite
Electrochemical pretreatment
Silver contamination
title An innovative pretreatment protocol to eliminate silver contamination-induced voltammetric interference on graphite-glass working electrode
title_full An innovative pretreatment protocol to eliminate silver contamination-induced voltammetric interference on graphite-glass working electrode
title_fullStr An innovative pretreatment protocol to eliminate silver contamination-induced voltammetric interference on graphite-glass working electrode
title_full_unstemmed An innovative pretreatment protocol to eliminate silver contamination-induced voltammetric interference on graphite-glass working electrode
title_short An innovative pretreatment protocol to eliminate silver contamination-induced voltammetric interference on graphite-glass working electrode
title_sort innovative pretreatment protocol to eliminate silver contamination induced voltammetric interference on graphite glass working electrode
topic Screen-printed electrode
Graphite-glass composite
Electrochemical pretreatment
Silver contamination
url http://www.sciencedirect.com/science/article/pii/S138824812400050X
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