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Advanced Electrode Materials Dedicated for Electroanalysis

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A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Materials Chemistry".

Deadline for manuscript submissions: closed (10 August 2023) | Viewed by 18765

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Prof. Dr. Sławomira Skrzypek

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Department of Inorganic and Analytical Chemistry, University of Lodz, Faculty of Chemistry, Tamka 12, 91-403 Łódź, Poland
Interests: electrochemistry; electroanalysis; chemical sensing and biosensing solid state electrodes; carbon-based electrodes; ceramic electrodes; electrode materials modification; nanomaterials; conducting polymers, PEDOT; biomaterials, corrosion; interface between two immiscible electrolyte solutions (ITIES)

Dr. Mariola Brycht

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Department of Inorganic and Analytical Chemistry, Faculty of Chemistry, University of Lodz, Tamka 12, 91-403 Łódź, Poland
Interests: carbon-based electrode materials; solid state electrodes; nanomaterials; electrode materials modification; materials characterization; electrochemistry; electroanalysis; chemical sensing and biosensing

Dr. Barbara Burnat

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Department of Inorganic and Analytical Chemistry, Faculty of Chemistry, University of Lodz, Tamka 12, 91-403 Łódź, Poland
Interests: electrochemistry; carbon-based electrode materials; ceramic electrodes; solid state electrodes; nanomaterials; sol-gel materials; materials modification; materials characterization; electroanalysis; corrosion; biomaterials

Special Issue Information

Dear Colleagues,

We would like to invite you to contribute original research manuscripts, comprehensive review articles, or short communications to the Special Issue titled “Advanced Electrode Materials Dedicated for Electroanalysis”.

The electrochemical tools provide simple, inexpensive, and highly sensitive procedures and can be integrated into miniaturized measuring platforms. Numerous types of electrode materials thus far have been developed and successfully applied in electroanalysis. They find an application in many areas including environmental, healthcare, and pharmaceutical analyses, as electrochemical detectors, micro-/nano-electrochemical devices, and chemical and biochemical sensors. Constantly, there is a very high requirement for innovative, advanced electrode materials offering a high selectivity and sensitivity, operation simplicity, and low production cost.

The forthcoming Special Issue seeks high-quality feature papers that provide insight into and highlight the latest progress and innovative developments in advanced electrode materials dedicated for electroanalysis. The topics covered in this Special Issue include the fabrication and processing of the electrode materials based on carbon allotropes; conductive polymers; metal or metal oxide nanoparticles, as well as their characterization; and potential electroanalytical applications. However, other related topics are also welcome.

Prof. Dr. Sławomira Skrzypek
Dr. Mariola Brycht
Dr. Barbara Burnat
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Materials is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

carbon-based electrode materials
conducting polymer-based electrode materials
electrode materials modifications
nanomaterials
enzymes
membranes
miniaturization
materials fabrication
materials characterization
electrochemical properties
synthesis of organic/inorganic materials
electrochemical detection
(bio)electroanalytical applications
chemical (bio)sensing

Published Papers (11 papers)

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Research

13 pages, 3072 KiB

Open AccessEditor’s ChoiceArticle

Fabrication and Characterization of an Electrochemical Platform for Formaldehyde Oxidation, Based on Glassy Carbon Modified with Multi-Walled Carbon Nanotubes and Electrochemically Generated Palladium Nanoparticles

by Andrzej Leniart, Barbara Burnat, Mariola Brycht, Maryia-Mazhena Dzemidovich and Sławomira Skrzypek

Materials 2024, 17(4), 841; https://doi.org/10.3390/ma17040841 - 09 Feb 2024

Viewed by 666

Abstract

This study outlines the fabrication process of an electrochemical platform utilizing glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes (MWCNTs) and palladium nanoparticles (PdNPs). The MWCNTs were applied on the GCE surface using the drop-casting method and PdNPs were produced electrochemically by a potentiostatic method employing various programmed charges from an ammonium tetrachloropalladate(II) solution. The resulting GCEs modified with MWCNTs and PdNPs underwent comprehensive characterization for topographical and morphological attributes, utilizing atomic force microscopy and scanning electron microscopy along with energy-dispersive X-ray spectrometry. Electrochemical assessment of the GCE/MWCNTs/PdNPs involved cyclic voltammetry (CV) and electrochemical impedance spectroscopy conducted in perchloric acid solution. The findings revealed even dispersion of PdNPs, and depending on the electrodeposition parameters, PdNPs were produced within four size ranges, i.e., 10–30 nm, 20–40 nm, 50–60 nm, and 70–90 nm. Additionally, the electrocatalytic activity toward formaldehyde oxidation was assessed through CV. It was observed that an increase in the size of the PdNPs corresponded to enhanced catalytic activity in the formaldehyde oxidation reaction on the GCE/MWCNTs/PdNPs. Furthermore, satisfactory long-term stability over a period of 42 days was noticed for the GCE/MWCNTs/PDNPs(100) material which demonstrated the best electrocatalytic properties in the electrooxidation reaction of formaldehyde. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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16 pages, 6835 KiB

Open AccessArticle

Incorporation of Bismuth(III) Oxide Nanoparticles into Carbon Ceramic Composite: Electrode Material with Improved Electroanalytical Performance in 4-Chloro-3-Methylphenol Determination

by Mariola Brycht, Andrzej Leniart, Sławomira Skrzypek and Barbara Burnat

Materials 2024, 17(3), 665; https://doi.org/10.3390/ma17030665 - 29 Jan 2024

Viewed by 610

Abstract

In this study, a carbon ceramic electrode (CCE) with improved electroanalytical performance was developed by bulk-modifying it with bismuth(III) oxide nanoparticles (Bi-CCE). Characterization of the Bi-CCE was conducted employing atomic force microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy, cyclic voltammetry (CV), and electrochemical impedance spectroscopy. Comparative analysis was conducted using an unmodified CCE. The findings proved that the incorporation of Bi₂O₃ nanoparticles into the CCE significantly altered the morphology and topography of the ceramic composite, and it improved the electrochemical properties of CCE. Notably, the Bi-CCE demonstrated a prolonged operational lifespan of at least three months, and there was a high reproducibility of the electrode preparation procedure. The developed Bi-CCE was effectively employed to explore the electrochemical behavior and quantify the priority environmental pollutant 4-chloro-3-methylphenol (PCMC) using CV and square-wave voltammetry (SWV), respectively. Notably, the developed SWV procedure utilizing Bi-CCE exhibited significantly enhanced sensitivity (0.115 µA L mol⁻¹), an extended linearity (0.5–58.0 µmol L⁻¹), and a lower limit of detection (0.17 µmol L⁻¹) in comparison with the unmodified electrode. Furthermore, the Bi-CCE was utilized effectively for the detection of PCMC in a river water sample intentionally spiked with the compound. The selectivity toward PCMC determination was also successfully assessed. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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18 pages, 5013 KiB

Open AccessArticle

The Composite Material of (PEDOT-Polystyrene Sulfonate)/Chitosan-AuNPS-Glutaraldehyde/as the Base to a Sensor with Laccase for the Determination of Polyphenols

by Paweł Krzyczmonik, Marta Klisowska, Andrzej Leniart, Katarzyna Ranoszek-Soliwoda, Jakub Surmacki, Karolina Beton-Mysur and Beata Brożek-Płuska

Materials 2023, 16(14), 5113; https://doi.org/10.3390/ma16145113 - 20 Jul 2023

Cited by 2 | Viewed by 927

Abstract

The described research aimed to develop the properties of the conductive composite /poly(3,4-ethylenedioxy-thiophene-poly(4-lithium styrenesulfonic acid)/chitosan-AuNPs-glutaraldehyde/ (/PEDOT-PSSLi/chit-AuNPs-GA/) and to develop an electrochemical enzyme sensor based on this composite material and glassy carbon electrodes (GCEs). The composite was created via electrochemical production of an /EDOT-PSSLi/ layer on a glassy carbon electrode (GCE). This layer was covered with a glutaraldehyde cross-linked chitosan and doped with AuNPs. The influence of AuNPs on the increase in the electrical conductivity of the chitosan layers and on facilitating the oxidation of polyphenols in these layers was demonstrated. The enzymatic sensor was obtained via immobilization of the laccase on the surface of the composite, with glutaraldehyde as the linker. The investigation of the surface morphology of the GCE/PEDOT-PSSLi/chit-AuNPs-GA/Laccase sensor was carried out using SEM and AFM microscopy. Using EDS and Raman spectroscopy, AuNPs were detected in the chitosan layer and in the laccase on the surface of the sensor. Polyphenols were determined using differential pulse voltammetry. The biosensor exhibited catalytic activity toward the oxidation of polyphenols. It has been shown that laccase is regenerated through direct electron transfer between the sensor and the enzyme. The results of the DPV tests showed that the developed sensor can be used for the determination of polyphenols. The peak current was linearly proportional to the concentrations of catechol in the range of 2–90 μM, with a limit of detection (LOD) of 1.7 μM; to those of caffeic acid in the range of 2–90 μM, LOD = 1.9 μM; and to those of gallic acid in the range 2–18 μM, LOD = 1.7 μM. Finally, the research conducted in order to determine gallic acid in a natural sample, for which white wine was used, was described. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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14 pages, 2719 KiB

Open AccessArticle

Probing the Use of Homemade Carbon Fiber Microsensor for Quantifying Caffeine in Soft Beverages

by Karla Caroline de Freitas Araújo, Emily Cintia Tossi de Araújo Costa, Danyelle Medeiros de Araújo, Elisama V. Santos, Carlos A. Martínez-Huitle and Pollyana Souza Castro

Materials 2023, 16(5), 1928; https://doi.org/10.3390/ma16051928 - 25 Feb 2023

Viewed by 1359

Abstract

In the development of electrochemical sensors, carbon micro-structured or micro-materials have been widely used as supports/modifiers to improve the performance of bare electrodes. In the case of carbon fibers (CFs), these carbonaceous materials have received extensive attention and their use has been proposed in a variety of fields. However, to the best of our knowledge, no attempts for electroanalytical determination of caffeine with CF microelectrode (µE) have been reported in the literature. Therefore, a homemade CF-µE was fabricated, characterized, and used to determine caffeine in soft beverage samples. From the electrochemical characterization of the CF-µE in K₃Fe(CN)₆ 10 mmol L⁻¹ plus KCl 100 mmol L⁻¹, a radius of about 6 µm was estimated, registering a sigmoidal voltammetric profile that distinguishes a µE indicating that the mass-transport conditions were improved. Voltammetric analysis of the electrochemical response of caffeine at the CF-µE clearly showed that no effects were attained due to the mass transport in solution. Differential pulse voltammetric analysis using the CF-µE was able to determine the detection sensitivity, concentration range (0.3 to 4.5 µmol L⁻¹), limit of detection (0.13 μmol L⁻¹) and linear relationship (I (µA) = (11.6 ± 0.09) × 10⁻³ [caffeine, μmol L⁻¹] − (0.37 ± 0.24) × 10⁻³), aiming at the quantification applicability in concentration quality-control for the beverages industry. When the homemade CF-µE was used to quantify the caffeine concentration in the soft beverage samples, the values obtained were satisfactory in comparison with the concentrations reported in the literature. Additionally, the concentrations were analytically determined by high-performance liquid chromatography (HPLC). These results show that these electrodes may be an alternative to the development of new and portable reliable analytical tools at low cost with high efficiency. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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12 pages, 1972 KiB

Open AccessArticle

Ratiometric Electrochemical Sensor for Butralin Determination Using a Quinazoline-Engineered Prussian Blue Analogue

by Marcio Cristiano Monteiro, João Paulo Winiarski, Edson Roberto Santana, Bruno Szpoganicz and Iolanda Cruz Vieira

Materials 2023, 16(3), 1024; https://doi.org/10.3390/ma16031024 - 23 Jan 2023

Cited by 16 | Viewed by 1701

Abstract

A ratiometric electrochemical sensor based on a carbon paste electrode modified with quinazoline-engineered ZnFe Prussian blue analogue (PBA-qnz) was developed for the determination of herbicide butralin. The PBA-qnz was synthesized by mixing an excess aqueous solution of zinc chloride with an aqueous solution of precursor sodium pentacyanido(quinazoline)ferrate. The PBA-qnz was characterized by spectroscopic and electrochemical techniques. The stable signal of PBA-qnz at +0.15 V vs. Ag/AgCl, referring to the reduction of iron ions, was used as an internal reference for the ratiometric sensor, which minimized deviations among multiple assays and improved the precision of the method. Furthermore, the PBA-qnz-based sensor provided higher current responses for butralin compared to the bare carbon paste electrode. The calibration plot for butralin was obtained by square wave voltammetry in the range of 0.5 to 30.0 µmol L⁻¹, with a limit of detection of 0.17 µmol L⁻¹. The ratiometric sensor showed excellent precision and accuracy and was applied to determine butralin in lettuce and potato samples. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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15 pages, 4203 KiB

Open AccessArticle

Controlled Silanization of Transparent Conductive Oxides as a Precursor of Molecular Recognition Systems

by Anna Domaros, Dorota Zarzeczańska, Tadeusz Ossowski and Anna Wcisło

Materials 2023, 16(1), 309; https://doi.org/10.3390/ma16010309 - 29 Dec 2022

Cited by 1 | Viewed by 2118

Abstract

The search for new molecular recognition systems has become the goal of modern electrochemistry. Creating a matrix in which properties can be controlled to obtain a desired analytical signal is an essential part of creating such tools. The aim of this work was to modify the surface of electrodes based on transparent conductive oxides with the use of selected alkoxysilanes (3-aminopropyltrimethoxysilane, trimethoxy(propyl)silane, and trimethoxy(octyl)silane). Electrochemical impedance spectroscopy and cyclic voltammetry techniques, as well as contact angle measurements, were used to determine the properties of the obtained layers. Here, we prove that not only was the structure of alkoxysilanes taken into account but also the conditions of the modification process—reaction conditions (time and temperature), double alkoxysilane modification, and mono- and binary component modification. Our results enabled the identification of the parameters that are important to ensure the effectiveness of the modification process. Moreover, we confirmed that the selection of the correct alkoxysilane allows the surface properties of the electrode material to be controlled and, consequently, the charge transfer process at the electrode/solution interface, hence enabling the creation of selective molecular recognition systems. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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13 pages, 2557 KiB

Open AccessArticle

The Influence of Graphene Oxide Composition on Properties of Surface-Modified Metal Electrodes

by Natalia Festinger, Aneta Kisielewska, Barbara Burnat, Katarzyna Ranoszek-Soliwoda, Jarosław Grobelny, Kamila Koszelska, Dariusz Guziejewski and Sylwia Smarzewska

Materials 2022, 15(21), 7684; https://doi.org/10.3390/ma15217684 - 01 Nov 2022

Cited by 6 | Viewed by 1595

Abstract

The present paper describes the effect of the concentration of two graphene oxides (with different oxygen content) in the modifier layer on the electrochemical and structural properties of noble metal disk electrodes used as working electrodes in voltammetry. The chemistry of graphene oxides was tested using EDS, FTIR, UV–Vis spectroscopy, and combustion analysis. The structural properties of the obtained modifier layers were examined by means of scanning electron and atomic force microscopy. Cyclic voltammetry was employed for comparative electrochemical studies. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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12 pages, 1389 KiB

Open AccessArticle

The Use of an Acylhydrazone-Based Metal-Organic Framework in Solid-Contact Potassium-Selective Electrode for Water Analysis

by Paweł Kościelniak, Marek Dębosz, Marcin Wieczorek, Jan Migdalski, Monika Szufla, Dariusz Matoga and Jolanta Kochana

Materials 2022, 15(2), 579; https://doi.org/10.3390/ma15020579 - 13 Jan 2022

Cited by 1 | Viewed by 1715

Abstract

A solid-contact ion-selective electrode was developed for detecting potassium in environmental water. Two versions of a stable cadmium acylhydrazone-based metal organic framework, i.e., JUK-13 and JUK-13_H2O, were used for the construction of the mediation layer. The potentiometric and electrochemical characterizations of the proposed electrodes were carried out. The implementation of the JUK-13_H2O interlayer is shown to improve the potentiometric response and stability of measured potential. The electrode exhibits a good Nernstian slope (56.30 mV/decade) in the concentration range from 10⁻⁵ to 10⁻¹ mol L⁻¹ with a detection limit of 2.1 µmol L⁻¹. The long-term potential stability shows a small drift of 0.32 mV h⁻¹ over 67 h. The electrode displays a good selectivity comparable to ion-selective electrodes with the same membrane. The K-JUK-13_H2O-ISE was successfully applied for the determination of potassium in three certified reference materials of environmental water with great precision (RSD < 3.00%) and accuracy (RE < 3.00%). Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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13 pages, 1746 KiB

Open AccessArticle

A Novel Voltametric Measurements of Beta Blocker Drug Propranolol on Glassy Carbon Electrode Modified with Carbon Black Nanoparticles

by Izabela Bargiel, Joanna Smajdor, Anna Górska, Beata Paczosa-Bator and Robert Piech

Materials 2021, 14(24), 7582; https://doi.org/10.3390/ma14247582 - 09 Dec 2021

Cited by 6 | Viewed by 1842

Abstract

A new voltametric method for highly sensitive propranolol (PROP) determination was developed. A glassy carbon electrode modified with a hybrid material made of carbon black (CB) and Nafion was used as the working electrode. The preconcentration potential and time were optimized (550 mV and 15 s), as well as the supporting electrolyte (0.1 mol L⁻¹ H₂SO₄). For 15 s preconcentration time, linearity was achieved in the range 0.5–3.5 μmol L⁻¹ and for 120 s in 0.02–0.14 μmol L⁻¹. Based on the conducted calibration (120 s preconcentration time) limit of detection (LOD) was calculated and was equal to 7 nmol L⁻¹. To verify the usefulness of the developed method, propranolol determination was carried out in real samples (tablets and freeze-dried urine). Recoveries were calculated and were in the range 92–102%, suggesting that the method might be considered as accurate. The repeatability of the signal expressed as relative standard deviation (RSD) was equal to 1.5% (n = 9, PROP concentration 2.5 µmol L⁻¹). The obtained results proved that the developed method for propranolol determination might be successfully applied in routine laboratory practice. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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20 pages, 4172 KiB

Open AccessFeature PaperArticle

Copper Film Modified Glassy Carbon Electrode and Copper Film with Carbon Nanotubes Modified Screen-Printed Electrode for the Cd(II) Determination

by Joanna Wasąg and Malgorzata Grabarczyk

Materials 2021, 14(18), 5148; https://doi.org/10.3390/ma14185148 - 08 Sep 2021

Cited by 9 | Viewed by 1530

Abstract

A copper film modified glassy carbon electrode (CuF/GCE) and a novel copper film with carbon nanotubes modified screen-printed electrode (CuF/CN/SPE) for anodic stripping voltammetric measurement of ultratrace levels of Cd(II) are presented. During the development of the research procedure, several main parameters were investigated and optimized. The optimal electroanalytical performance of the working electrodes was achieved in electrolyte 0.1 M HCl and 2 × 10⁻⁴ M Cu(II). The copper film modified glassy carbon electrode exhibited operation in the presence of dissolved oxygen with a calculated limit of detection of 1.7 × 10⁻¹⁰ M and 210 s accumulation time, repeatability with RSD of 4.2% (n = 5). In the case of copper film with carbon nanotubes modified screen-printed electrode limit of detection amounted 1.3 × 10⁻¹⁰ M for accumulation time of 210 s and with RSD of 4.5% (n = 5). The calibration curve has a linear range in the tested concentration of 5 × 10⁻¹⁰–5 × 10⁻⁷ M (r = 0.999) for CuF/GCE and 3 × 10⁻¹⁰–3 × 10⁻⁷ M (r = 0.999) for CuF/CN/SPE with 210 s accumulation time in both cases. The used electrodes enable trace determination of cadmium in different environmental water samples containing organic matrix. The validation of the proposed procedures was carried out through analysis certified reference materials: TM-25.5, SPS-SW1, and SPS-WW1. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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16 pages, 4069 KiB

Open AccessArticle

Good Choice of Electrode Material as the Key to Creating Electrochemical Sensors—Characteristics of Carbon Materials and Transparent Conductive Oxides (TCO)

by Anna Cirocka, Dorota Zarzeczańska and Anna Wcisło

Materials 2021, 14(16), 4743; https://doi.org/10.3390/ma14164743 - 22 Aug 2021

Cited by 12 | Viewed by 3334

Abstract

The search for new electrode materials has become one of the goals of modern electrochemistry. Obtaining electrodes with optimal properties gives a product with a wide application potential, both in analytics and various industries. The aim of this study was to select, from among the presented electrode materials (carbon and oxide), the one whose parameters will be optimal in the context of using them to create sensors. Electrochemical impedance spectroscopy and cyclic voltammetry techniques were used to determine the electrochemical properties of the materials. On the other hand, properties such as hydrophilicity/hydrophobicity and their topological structure were determined using contact angle measurements and confocal microscopy, respectively. Based on the research carried out on a wide group of electrode materials, it was found that transparent conductive oxides of the FTO (fluorine doped tin oxide) type exhibit optimal electrochemical parameters and offer great modification possibilities. These electrodes are characterized by a wide range of work and high chemical stability. In addition, the presence of a transparent oxide layer allows for the preservation of valuable optoelectronic properties. An important feature is also the high sensitivity of these electrodes compared to other tested materials. The combination of these properties made FTO electrodes selected for further research. Full article

(This article belongs to the Special Issue Advanced Electrode Materials Dedicated for Electroanalysis)

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