Disposable Voltammetric Sensor Modified with Block Copolymer-Dispersed Graphene for Simultaneous Determination of Dopamine and Ascorbic Acid in Ex Vivo Mouse Brain Tissue

Dopamine (DA) and ascorbic acid (AA) are two important biomarkers with similar oxidation potentials. To facilitate their simultaneous electrochemical detection, a new voltammetric sensor was developed by modifying a screen-printed carbon electrode (SPCE) with a newly synthesized block copolymer (poly(DMAEMA-b-styrene), PDbS) as a dispersant for reduced graphene oxide (rGO). The prepared PDbS–rGO and the modified SPCE were characterized using a range of physical and electrochemical techniques including Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, cyclic voltammetry, electrochemical impedance spectroscopy, and linear sweep voltammetry. Compared to the bare SPCE, the PDbS–rGO-modified SPCE (PDbS–rGO/SPCE) showed better sensitivity and peak-to-peak separation for DA and AA in mixed solutions. Under the optimum conditions, the dynamic linear ranges for DA and AA were 0.1–300 and 10–1100 µM, and the detection limits were 0.134 and 0.88 µM (S/N = 3), respectively. Furthermore, PDbS–rGO/SPCE exhibited considerably enhanced anti-interference capability, high reproducibility, and storage stability for four weeks. The practical potential of the PDbS–rGO/SPCE sensor for measuring DA and AA was demonstrated using ex vivo brain tissues from a Parkinson’s disease mouse model and the control.

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Poly-Phthalocyanine–Doped Graphene Oxide Nanosheet Conjugates for Electrocatalytic Oxidation of Drug Residues

Frontiers in Chemistry ◽

10.3389/fchem.2021.633547 ◽

2021 ◽

Vol 9 ◽

Author(s):

Prince Chundu ◽

Edith Dube ◽

Ngceboyakwethu P. Zinyama ◽

Mambo Moyo ◽

Munyaradzi Shumba

Keyword(s):

Electron Microscopy ◽

Ascorbic Acid ◽

Graphene Oxide ◽

Dynamic Range ◽

Electrochemical Impedance ◽

Cow Milk ◽

Catalytic Rate Constant ◽

Donor And Acceptor ◽

Vis Spectroscopy ◽

Doped Graphene

Donor and acceptor phthalocyanine molecules were copolymerized and linked to graphene oxide nanosheets through amidation to yield electrocatalytic platforms on glassy carbon electrodes. The platforms were characterized using transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy, UV/Vis spectroscopy, cyclic voltammetry, and electrochemical impedance spectroscopy. The fabricated electrochemical catalytic surfaces were then evaluated toward electrocatalytic detection of ascorbic acid and tryptophan. These were characterized by a wide linear dynamic range and low limits of detection and quantification of 2.13 and 7.12 µM for ascorbic acid and 1.65 and 5.5 µM for tryptophan, respectively. The catalytic rate constant was 1.86 × 104 and 1.51 × 104 M−1s−1 for ascorbic acid and tryptophan, respectively. The Gibbs energy for catalytic reactions was −17.45 and −14.83 kJ mol−1 depicting a spontaneous reaction on the electrode surface. The sensor platform showed an impressive recovery when applied in real samples such as fresh cow milk, in the range 91.71–106.73% for both samples. The developed sensor therefore shows high potential for applicability for minute quantities of the analytes in real biological samples.

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Development of one-dimensional titania nanomaterials

10.12681/eadd/38706 ◽

2014 ◽

Author(s):

Ναούμ Βαενάς

Keyword(s):

Electron Microscopy ◽

Electrochemical Impedance ◽

Linear Sweep Voltammetry ◽

Linear Sweep ◽

One Dimensional ◽

Force Microscopy ◽

Photocurrent Spectroscopy ◽

Atomic Force ◽

Transmission Electron ◽

Dye Solar Cells

Σκοπός αυτής της διδακτορικής διατριβής είναι η ανάπτυξη μονοδιάστατων νανοδομών τιτανίας και εν συνεχεία η εφαρμογή τους στην κατασκευή ευαισθητοποιημένων ηλιακών κελιών (Dye Solar Cells - DSCs). Οι νανοσωλήνες τιτανίας αποτελούν την ιδανική επιλογή για τους στόχους αυτής της έρευνας καθώς: α) μπορούν να προετοιμαστούν εύκολα από την ανοδική οξείδωση ενός φύλλου τιτανίου, β) επιτρέπουν τον εύκολο έλεγχο της μορφολογίας τους μέσω της ηλεκτροχημικής νάνο-μηχανικής, γ) εξασφαλίζουν εξαιρετικές ηλεκτρικές ιδιότητες, όπως κατευθυνόμενη κίνηση των ηλεκτρονίων. Οι νανοσωλήνες τιτανίας χρησιμοποιήθηκαν ως ηλεκτρόδια εργασίας (photo-anodes) στα ευαισθητοποιημένα ηλιακά κελιά που κατασκευάστηκαν στη συνέχεια.Τα μορφολογικά και δομικά χαρακτηριστικά των νανοσωλήνων μελετήθηκαν με τις τεχνικές, της μικροσκοπίας ατομικών δυνάμεων (Atomic Force Microscopy - AFM), της μικροσκοπίας ηλεκτρονικής σάρωσης (Scanning Electron Microscopy - SEM), της μικροσκοπίας ηλεκτρονικής διελεύσεως (Transmission Electron Microscopy - TEM), της φασματοσκοπίας υπεριώδους/ορατού (Ultraviolet–Visible - UV-Vis) και της φασματοσκοπίας Ράμαν (Raman spectroscopy). Επιπλέον η αξιολόγηση και ο χαρακτηρισμός των ηλιακών κελιών πραγματοποιήθηκε με τις μεθόδους, της φασματοσκοπίας ηλεκτροχημικής εμπέδησης (Electrochemical Impedance Spectroscopy - EIS), της φασματοσκοπίας φωτοδυναμικού/φωτορεύματος περιοδικά μεταβαλλόμενης έντασης φωτισμού (Intensity Modulated Photovoltage/ Photocurrent Spectroscopy - IMVS/IMPS) και τελικά οι αποδόσεις των φωτοβολταϊκών εξάχθηκαν από την βολταμετρία φωτορεύματος (Linear Sweep Voltammetry - LSV). Κίνητρα για αυτήν την μελέτη αποτέλεσαν η ανάγκη κατανόησης, των βασικών μηχανισμών ανάπτυξης των νανοσωλήνων τιτανίας καθώς και των αρχών λειτουργίας που διέπουν τα ευαισθητοποιημένα ηλιακά κελιά. Στο πρώτο μέρος αυτής της έρευνας πραγματοποιήθηκαν μερικά προκαταρτικά πειράματα, με σκοπό την βελτίωση της μορφολογίας του χρησιμοποιούμενου υποστρώματος τιτανίου, όπως και των νανοσωλήνων τιτανίας που προέκυψαν. Μόλις οι συνθήκες ανοδίωσης σταθεροποιήθηκαν, υψηλής ομοιογένειας και ποιότητας νανοσωλήνες προετοιμάστηκαν και χρησιμοποιήθηκαν σε ευαισθητοποιημένα ηλιακά κελιά με ικανοποιητική απόδοση. Στην δεύτερη φάση αυτού του έργου, οι δομικές ιδιότητες των νανοσωλήνων μελετήθηκαν , με σκοπό να εξασφαλιστεί η ανεμπόδιστη μεταφορά των ηλεκτρονίων. Συγκεκριμένα η επίδραση της διαδικασίας απόπτυσης των νανοσωλήνων διερευνήθηκε συνάρτηση των ηλεκτρικών χαρακτηριστικών των φωτοβολταϊκών συσκευών που τελικά παράχθηκαν. Στο τρίτο στάδιο της διατριβής, προηγμένες δομές νανοσωλήνων προετοιμάσθηκαν μέσω σύνθετων τρόπων ανοδίωσης. Η ποτενσιοστατική και γαλβανοστατική ανοδίωση συνδυάστηκαν για πρώτη φορά στην βιβλιογραφία και οδήγησαν στην εξέλιξη της μεθόδου της ανοδίωσης. Το τελευταίο μέρος της δουλειάς αφιερώθηκε αποκλείστηκα στην αύξηση της απόδοσης των φωτοβολταϊκών που ενσωμάτωναν φωτοηλεκτροδία νανοσωλήνων, μέσω της χρήσης των πιο σύγχρονων ηλεκτρολυτών και χρωστικών. Το οξειδοαναγωγικό ζεύγος κοβαλτίου διαχύθηκε με ευκολία στους πορώδους νανοσωλήνες και σε συνδυασμό με την οργανική χρωστική D35, οδήγησε σε υψηλές φωτοτάσεις και αποδόσεις.

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Electrochemical Corrosion of SAC Alloys: A Review

Metals ◽

10.3390/met10101276 ◽

2020 ◽

Vol 10 (10) ◽

pp. 1276

Author(s):

Ali Gharaibeh ◽

Ilona Felhősi ◽

Zsófia Keresztes ◽

Gábor Harsányi ◽

Balázs Illés ◽

...

Keyword(s):

Electrochemical Impedance ◽

Corrosion Behaviour ◽

Electrochemical Techniques ◽

Electrochemical Corrosion ◽

Linear Sweep Voltammetry ◽

Lead Free ◽

Solder Alloys ◽

Accelerated Corrosion ◽

Manufacturing Technologies ◽

Tin Silver Copper

Tin–silver–copper (SAC) solder alloys are the most promising candidates to replace Sn–Pb solder alloys. However, their application is still facing several challenges; one example is the electrochemical corrosion behaviour, which imposes a risk to electronics reliability. Numerous investigations have been carried out to evaluate the corrosion performance of SAC lead-free alloys, regarding the effect of the corrosive environment, the different manufacturing technologies, the effect of fluxes, the metallic contents within the SAC alloys themselves, and the different alloying elements. In these studies, widely used electrochemical techniques are applied as accelerated corrosion tests, such as linear sweep voltammetry and electrochemical impedance spectroscopy. However, there is lack of studies that try to summarise the various corrosion results in terms of lead-free solder alloys including low-Ag and composite solders. This study aims to review these studies by showing the most important highlights regarding the corrosion processes and the possible future developments.

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Beneficial Effects of Vanadium Additions on the Corrosion of Ti6AlxV Alloys in Chloride Solutions

Metals ◽

10.3390/met10020264 ◽

2020 ◽

Vol 10 (2) ◽

pp. 264 ◽

Cited By ~ 1

Author(s):

El-Sayed M. Sherif ◽

Hany S. Abdo ◽

Nabeel H. Alharthi

Keyword(s):

Electron Microscopy ◽

Immersion Time ◽

Electrochemical Impedance ◽

Electrochemical Techniques ◽

Test Medium ◽

X Ray ◽

Beneficial Effects ◽

Cyclic Potentiodynamic Polarization ◽

Scanning Electron

The beneficial effects of V addition on the corrosion of a newly manufactured Ti6AlxV (x = 2 wt %, 4 wt %, 6 wt %, and 8 wt %) alloys after various exposure periods in 3.5% NaCl solutions were reported. The Ti6AlxV were produced from their raw powders using mechanical alloying. Several electrochemical techniques such as electrochemical impedance spectroscopy, cyclic potentiodynamic polarization, and potentiodynamic current versus time at 300 mV experiments were conducted. The surface morphology and the elemental analysis were performed using scanning electron microscopy and energy dispersive X-ray analyses. All results were consistent with each other revealing that the increase of V content increases the resistance of the alloys against corrosion. The increase of corrosion resistance was achieved by the role of V in decreasing the rate of corrosion as a result of the formation of oxide films on the surface of the alloys. This effect was found to increase with prolonging the immersion time of the Ti6AlxV alloys in the test medium from 1 h to 24 h and further to 48 h.

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Synthesis of a simply modified electrochemical nicotine sensor based on silver nanoparticles

Canadian Journal of Chemistry ◽

10.1139/cjc-2017-0492 ◽

2018 ◽

Vol 96 (8) ◽

pp. 821-827 ◽

Cited By ~ 7

Author(s):

M.A. Ameer ◽

A.M. Fekry ◽

S.M. Azab ◽

M. Shehata

Keyword(s):

Electrochemical Impedance ◽

Electrochemical Techniques ◽

Sodium Dodecyl ◽

Linear Sweep Voltammetry ◽

High Sensitivity ◽

Modified Carbon Paste Electrode ◽

Carbon Paste ◽

Long Term Stability ◽

Ph Range ◽

Modified Sensor

An innovative electrochemical nicotine modified sensor was created by chemically mixing a carbon paste with silver nano powder to prepare an Ag nanoparticle modified carbon paste electrode. Different electrochemical techniques including cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy in both aqueous and micellar media were used. The surface morphology was also detected using scanning electron microscope and energy dispersive X-ray analysis techniques. Nicotine measurements were investigated in Britton–Robinson buffer solutions with a pH range of 2.0–8.0 containing 1.0 mmol/L sodium dodecyl sulfate. The electrode-based NIC sensor exhibited a high sensitivity in quantitative analysis, and its detection limit could be as low as 0.0036 μmol/L with linearity ranging from 0.8 μmol/L to 800 μmol/L. In addition, due to its good reproducibility, anti-interference performance, and long-term stability, the proposed sensor is capable of detecting trace levels of nicotine in urine samples and different brands of commercial cigarettes.

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Water Photo-Electrooxidation Using Mats of TiO2 Nanorods, Surface Sensitized by a Metal–Organic Framework of Nickel and 1,2-Benzene Dicarboxylic Acid

Hydrogen ◽

10.3390/hydrogen2010004 ◽

2021 ◽

Vol 2 (1) ◽

pp. 58-75

Author(s):

Sheng-Mu You ◽

Waleed M. A. El Rouby ◽

Loïc Assaud ◽

Ruey-An Doong ◽

Pierre Millet

Keyword(s):

Dicarboxylic Acid ◽

Electrochemical Impedance ◽

Metal Organic Framework ◽

Linear Sweep Voltammetry ◽

Tio2 Nanorods ◽

Tem Analysis ◽

Vis Spectroscopy ◽

Metal Organic ◽

Benzene Dicarboxylic Acid ◽

Organic Framework

Photoanodes comprising a transparent glass substrate coated with a thin conductive film of fluorine-doped tin oxide (FTO) and a thin layer of a photoactive phase have been fabricated and tested with regard to the photo-electro-oxidation of water into molecular oxygen. The photoactive layer was made of a mat of TiO2 nanorods (TDNRs) of micrometric thickness. Individual nanorods were successfully photosensitized with nanoparticles of a metal–organic framework (MOF) of nickel and 1,2-benzene dicarboxylic acid (BDCA). Detailed microstructural information was obtained from SEM and TEM analysis. The chemical composition of the active layer was determined by XRD, XPS and FTIR analysis. Optical properties were determined by UV–Vis spectroscopy. The water photooxidation activity was evaluated by linear sweep voltammetry and the robustness was assessed by chrono-amperometry. The OER (oxygen evolution reaction) photo-activity of these photoelectrodes was found to be directly related to the amount of MOF deposited on the TiO2 nanorods, and was therefore maximized by adjusting the MOF content. The microscopic reaction mechanism which controls the photoactivity of these photoelectrodes was analyzed by photo-electrochemical impedance spectroscopy. Microscopic rate parameters are reported. These results contribute to the development and characterization of MOF-sensitized OER photoanodes.

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Electro-Oxidation of Ammonia at Novel Ag2O−PrO2/γ-Al2O3 Catalysts

Coatings ◽

10.3390/coatings11020257 ◽

2021 ◽

Vol 11 (2) ◽

pp. 257

Author(s):

Mariam Khan ◽

Naveed Kausar Janjua ◽

Safia Khan ◽

Ibrahim Qazi ◽

Shafaqat Ali ◽

...

Keyword(s):

Electron Microscopy ◽

Electrochemical Impedance ◽

Precipitation Method ◽

Impregnation Method ◽

X Rays ◽

Kinetic And Thermodynamic Parameters ◽

Catalytic Support ◽

Transmission Electron ◽

Electro Oxidation ◽

Oxidation Of Ammonia

An Ag2O(x)−PrO2(y)/γ-Al2O3 electrocatalyst series (X:Y is for Ag:Pr from 0 to 10) was synthesized, to use synthesized samples in electrochemical applications, a step in fuel cells advancements. Ag2O(x)−PrO2(y)/γ-Al2O3/Glassy-Carbon was investigated for electrochemical oxidation of ammonia in alkaline medium and proved to be highly effective, having high potential utility, as compared to commonly used Pt-based electrocatalysts. In this study, gamma alumina as catalytic support was synthesized via precipitation method, and stoichiometric wt/wt.% compositions of Ag2O−PrO2 were loaded on γ-Al2O3 by co-impregnation method. The desired phase of γ-Al2O3 and supported nanocatalysts was obtained after heat treatment at 800 and 600 °C, respectively. The successful loadings of Ag2O−PrO2 nanocatalysts on surface of γ-Al2O3 was determined by X-rays diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), and energy dispersive analysis (EDX). The nano-sized domain of the sample powders sustained with particle sizes was calculated via XRD and scanning electron microscopy (SEM). The surface morphology and elemental compositions were examined by SEM, transmission electron microscopy (TEM) and EDX. The conductive and electron-transferring nature was investigated by cyclic voltammetry and electrochemical impedance (EIS). Cyclic voltammetric profiles were observed, and respective kinetic and thermodynamic parameters were calculated, which showed that these synthesized materials are potential catalysts for ammonia electro-oxidation. Ag2O(6)−PrO2(4)/γ-Al2O3 proved to be the most proficient catalyst among all the members of the series, having greater diffusion coefficient, heterogeneous rate constant and lesser Gibbs free energy for this system. The catalytic activity of these electrocatalysts is revealed from electrochemical studies which reflected their potentiality as electrode material in direct ammonia fuel cell technology for energy production.

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Performance of coatings containing treated silica fume in the corrosion protection of reinforced concrete

Pigment & Resin Technology ◽

10.1108/prt-08-2017-0076 ◽

2018 ◽

Vol 47 (4) ◽

pp. 350-359 ◽

Cited By ~ 4

Author(s):

Nivin M. Ahmed ◽

Mostafa G. Mohamed ◽

Reham H. Tammam ◽

Mohamed R. Mabrouk

Keyword(s):

Reinforced Concrete ◽

Silica Fume ◽

Corrosion Protection ◽

Electrochemical Impedance ◽

Electrochemical Techniques ◽

Dual Function ◽

Core Shell ◽

Protection Efficiency ◽

Content Type ◽

Anticorrosive Pigments

Purpose This study aims to apply novel anticorrosive pigments containing silica fume-phosphates (Si-Ph), which were prepared using core-shell technique by covering 80-90 per cent silica fume (core) with 10-20 per cent phosphates (shell) previously, to play dual functions simultaneously as anticorrosive pigments in coating formulations and as an anticorrosive admixture in concrete even if it is not present in the concrete itself. Two comparisons were held out to show the results of coatings on rebars containing core-shell pigments in concrete, and concrete admixtured with silica fume can perform a dual function as anticorrosive pigment and concrete admixture. The evaluation of corrosion protection efficiency of coatings containing core-shell pigments and those containing phosphates was performed. Design/methodology/approach Simple chemical techniques were used to prepare core-shell pigments, and their characterization was carried out in a previous work. These pigments were incorporated in solvent-based paint formulations based on epoxy resin. Different electrochemical techniques such as open-circuit potential and electrochemical impedance spectroscopy were used to evaluate the anticorrosive efficiency of the new pigments. Findings The electrochemical measurements showed that concrete containing coated rebars with core-shell pigments exhibited almost similar results to that of concrete admixtured with silica fume. Also, the anticorrosive performance of coatings containing Si-Ph pigments offered protection efficiency almost similar to that of phosphates, proving that these new pigments can perform both roles as anticorrosive pigment and concrete admixture. Originality/value Although the new Si-Ph pigments contain more than 80 per cent waste material, its performance can be compared to original phosphate pigments in the reinforced concrete.

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Corrosion of Steel Rebars in Anoxic Environments. Part I: Electrochemical Measurements

Materials ◽

10.3390/ma14102491 ◽

2021 ◽

Vol 14 (10) ◽

pp. 2491

Author(s):

Elena Garcia ◽

Julio Torres ◽

Nuria Rebolledo ◽

Raul Arrabal ◽

Javier Sanchez

Keyword(s):

Corrosion Rate ◽

Electrochemical Impedance ◽

Electrochemical Techniques ◽

Chloride Content ◽

Offshore Platforms ◽

Anoxic Conditions ◽

Current Limit ◽

Anoxic Environments ◽

Corrosion Of Steel ◽

Steel Rebars

The number of reinforced concrete structures subject to anoxic conditions such as offshore platforms and geological storage facilities is growing steadily. This study explored the behaviour of embedded steel reinforcement corrosion under anoxic conditions in the presence of different chloride concentrations. Corrosion rate values were obtained by three electrochemical techniques: Linear polarization resistance, electrochemical impedance spectroscopy, and chronopotenciometry. The corrosion rate ceiling observed was 0.98 µA/cm2, irrespective of the chloride content in the concrete. By means of an Evans diagram, it was possible to estimate the value of the cathodic Tafel constant (bc) to be 180 mV dec−1, and the current limit yielded an ilim value of 0.98 µA/cm2. On the other hand, the corrosion potential would lie most likely in the −900 mVAg/AgCl to −1000 mVAg/AgCl range, whilst the bounds for the most probable corrosion rate were 0.61 µA/cm2 to 0.22 µA/cm2. The experiments conducted revealed clear evidence of corrosion-induced pitting that will be assessed in subsequent research.

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Effect of Mechanical Surface Treatments on the Surface State and Passive Behavior of 304L Stainless Steel

Metals ◽

10.3390/met11010135 ◽

2021 ◽

Vol 11 (1) ◽

pp. 135

Author(s):

Kathleen Jaffré ◽

Benoît Ter-Ovanessian ◽

Hiroshi Abe ◽

Nicolas Mary ◽

Bernard Normand ◽

...

Keyword(s):

Electron Microscopy ◽

Stainless Steel ◽

Surface State ◽

Electrochemical Impedance ◽

Passive Films ◽

Surface Finishing ◽

Ultrafine Grain ◽

304L Stainless Steel ◽

Passive Behavior

The effect of dry grinding on 304L stainless steel’s passive behavior is compared to two other surface finishing (mechanical polishing down to 2400 with SiC emery paper and 1 µm with diamond paste, respectively). The characterization of the surface state was performed using scanning electron microscopy, transmission electron microscopy, 3D optical profilometer, and X-ray diffraction. Results indicate that each surface treatment leads to different surface states. The ground specimens present an ultrafine grain layer and a strong plastic deformation underneath the surface, while an ultrafine grain layer characterizes the subsurface of the polished specimens. Grinding induces high residual compressive stresses and high roughness compared to polishing. The characterization of the passive films was performed by electrochemical impedance spectroscopy and Mott–Schottky analysis. The study shows that the semiconductor properties and the thickness of the passive films are dependent on the surface state of the 304L stainless steel.

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