Experimental Setup of Square-Wave Anodic Stripping Voltammetry Measurement of Lead and Cadmium Using Antimony Impregnated Activated Carbon Electrode
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A Rhodium Centered Supramolecular Complex as a Photoinitiated Electron Collector by Mark Christopher Elvington Dissertation submitted to the faculty of the Virgnia Polytechnic Institute and State University in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Chemistry Karen J. Brewer, Chair Mark R. Anderson Paul A. Deck Brian E. Hanson Gordon T. Yee July 24, 2007 Blacksburg, Virginia Keywords: Supramolecular, photochemistry, photocatalysis, electron transfer A Rhodium Centered Supramolecular Complex as a Photoinitiated Electron Collector Mark Christopher Elvington Abstract The research presented here is focused on photochemical studies of a supramolecular structural motif for photoinitiated electron collection. The complex studied, [{(bpy)2Ru(dpp)}2RhCl2](PF6)5, is of the form LA-BL-EC-BL-LA comprising a Ru(II) polyazine light absorber (LA) bearing two bpy (bpy = 2,2’-bipyridine) ligands, two dpp (dpp = 2,3’-bis(2-pyridyl)pyrazine) bridging ligands (BL), and a central rhodium(III) electron collector (EC). Ruthenium-polyazine light absorbers are commonly used in light to energy conversion systems due to the intense metal to ligand charge transfer (MLCT) absorptions observed in the visible spectrum. Electrochemical methods establish rhodium as the site of localization of the lowest lying unoccupied molecular orbital, while phosphorescence measurements are used to study electron transfer within the supramolecular assembly. Electrochemical and photochemical experiments show that the absorption of light in the rhodium centered supramolecular complex, [{(bpy)2Ru(dpp)}2RhCl2](PF6)5, can initiate the sequential transfer of multiple electrons to the rhodium metal center, i.e. photoinitiated electron collection. A mechanistic study of photoinitiated electron collection, involving a Stern-Volmer analysis of emission quenching and product formation, is also presented, to determine the rate constants of the possible excited state and ground state reactions. -
Electrochemical Behavior of Biologically Important Indole Derivatives
SAGE-Hindawi Access to Research International Journal of Electrochemistry Volume 2011, Article ID 154804, 10 pages doi:10.4061/2011/154804 Review Article Electrochemical Behavior of Biologically Important Indole Derivatives Cigdem Karaaslan and Sibel Suzen Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Ankara University, Tandogan 06100, Ankara, Turkey Correspondence should be addressed to Sibel Suzen, [email protected] Received 11 January 2011; Accepted 21 January 2011 Academic Editor: Bengi Uslu Copyright © 2011 C. Karaaslan and S. Suzen. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. Voltammetric techniques are most suitable to investigate the redox properties of a new drug. Use of electrochemistry is an important approach in drug discovery and research as well as quality control, drug stability, and determination of physiological activity. The indole nucleus is an essential element of a number of natural and synthetic products with significant biological activity. Indole derivatives are the well-known electroactive compounds that are readily oxidized at carbon-based electrodes, and thus analytical procedures, such as electrochemical detection and voltammetry, have been developed for the determination of biologically important indoles. This paper explains some of the relevant and recent achievements in the electrochemistry processes and parameters mainly related to biologically important indole derivatives in view of drug discovery and analysis. 1. Indoles in Medicinal Chemistry of the sulfur containing 2PI derivatives show in vivo anti- neoplastic and antiestrogenic activity [9, 10]. Furthermore, Indole is an aromatic heterocyclic compound that has a some indole derivatives, such as melatonin and serotonin, bicyclic structure. -
Square-Wave Protein-Film Voltammetry: New Insights in the Enzymatic Electrode Processes Coupled with Chemical Reactions
Journal of Solid State Electrochemistry https://doi.org/10.1007/s10008-019-04320-7 ORIGINAL PAPER Square-wave protein-film voltammetry: new insights in the enzymatic electrode processes coupled with chemical reactions Rubin Gulaboski1 & Valentin Mirceski2,3 & Milivoj Lovric4 Received: 4 April 2019 /Revised: 9 June 2019 /Accepted: 9 June 2019 # Springer-Verlag GmbH Germany, part of Springer Nature 2019 Abstract Redox mechanisms in which the redox transformation is coupled to other chemical reactions are of significant interest since they are regarded as relevant models for many physiological systems. Protein-film voltammetry, based on surface confined electro- chemical processes, is a methodology of exceptional importance, which is designed to provide information on enzyme redox chemistry. In this work, we address some theoretical aspects of surface confined electrode mechanisms under conditions of square-wave voltammetry (SWV). Attention is paid to a collection of specific voltammetric features of a surface electrode reaction coupled with a follow-up (ECrev), preceding (CrevE) and regenerative (EC’) chemical reaction. While presenting a collection of numerically calculated square-wave voltammograms, several intriguing and simple features enabling kinetic char- acterization of studied mechanisms in time-independent experiments (i.e., voltammetric experiments at a constant scan rate) are addressed. The aim of the work is to help in designing a suitable experimental set-up for studying surface electrode processes, as well as to provide a means for determination of kinetic and/or thermodynamic parameters of both electrode and chemical steps. Keywords Kinetics of electrode reactions and chemical reactions . Surface EC′ catalytic mechanism . Surface ECrev mechanism . Surface CrevE mechanism . Square-wave voltammetry Introduction modulation applied, however, SWV is seldom explored as a technique for mechanistic evaluations. -
DC Cell Analysis Techniques Pulse Voltammetry John Harper and Brian Sayers Application Guide: AGML11 Solartron Analytical, Farnborough, UK
electrochemistry DC cell analysis techniques Pulse Voltammetry John Harper and Brian Sayers Application Guide: AGML11 Solartron Analytical, Farnborough, UK. Introduction Polarographic techniques were among the first to be developed by electrochemists as a set of standardized methods with analytical solutions of diffusion equations. They are commonly employed in trace analysis applications such as trace metal analysis in water quality and analysis of blood. Historically, mercury electrodes were the substrate of choice. However, due to the toxicity of mercury, many studies now use inert materials such as boron-doped diamond electrodes. This demonstration experiment shows how the ModuLab potentiostat applies and measures the voltage and current for three common polarographic techniques; normal, differential and square wave pulse voltammetry. Key system capabilities used in this demonstration • In addition to conventional forward and reverse current measurements per pulse, ModuLab allows the user to sample current and voltage continuously while using pulse techniques. This allows the user to check the pulse shapes and decide where the “per pulse” type measurements should be made. This is a very useful feature since the timing varies due to the cell time constant and DC scan rates. • This is also a useful feature to check that the correct waveform is being applied to the cell. Equipment required for this demonstration • ModuLab Potentiostat, ModuLab Test Cell Connections • Connect coloured cables to their corresponding connections on the test cell Experiment setup Select "AGML11 Pulse Voltammetry" in the "ModuLab Application Guide" project Either a multiple step experiment as below, or individual experiments for each pulse technique Step # Purpose Step 1 Normal Pulse Voltammetry step Step 2 Differential Pulse Voltammetry Step 3 Squarewave Voltammetry Additional test possibilities: • The low current femto ammeter option may be used for better current resolution if needed. -
Fundamentals of Electrochemistry
Yonsei University Fundamentals of Electrochemistry References Electrochemical Methods : Fundamentals and Applications, 2nd edition. by A. J. Bard and L.R. Faulkner • Makes use of electrochemistry for the purpose of analysis • A voltage (potentiometry) or current (voltammetry) signal originating from an electrochemical cell is related to the activity or concentration of a particular species in the cell. • Excellent detection limit (10-8 ~ 10-3 M): 1959, Nobel Prize (Polarography) • Inexpensive technique. • Easily miniaturized : implantable and/or portable (biosensor, biochip) Electrochemical cells Galvanic cell Digital High input impedance voltmeter A B e- Anode reaction Zn Zn2+ + 2e- : oxidation e- Cathode reaction Cu2+ + 2e- Cu (-)KCl (+) : reduction Zn Cu Salt bridge Zn + Cu2+ Zn2+ + Cu K+ - - 2e Cl 2e- Cell potential : a measure of difference in electron Zn2+ energy between the two electrodes 2- SO4 Zn Cu Open-circuit potential (zero-current potential) Zn2+ Cu2+ 2+ 2+ Zn 2- 2- Cu : can be calculated from thermodynamic data, ie. SO4 SO 4 standard cell potentials of the half-cell reactions. Anode Cathode Fig. 27.1 Electrochemical cell consisting of a zinc electrode in 0.1 M ZnSO4, a copper electrode in 0.1 M CuSO4, and a salt bridge. Galvanic cell. (From Heineman book) Standard Electrode Potential Table 22.1 Standard Electrode Potentials Reaction E0 at 25 ℃, V - - Cl2(g) + 2e 2Cl +1.359 + - O2(g) + 4H +4e 2H2O +1.229 - - Br2(aq) + 2e 2Br +1.087 - - Br2(l) + 2e 2Br +1.065 Ag+ + e- Ag(s) +-.799 Reduction 자발적 Fe3+ + e- Fe2+ +0.771 - - - I3 + 2e 3I +0.536 Cu2+ + 2e- Cu(s) +0.337 - - Hg2Cl2(s) + 2e 2Hg(l) + 2Cl +0.268 AgCl(s) + e- Ag(s) + Cl- +0.222 3- - 2- A quantitative description of the relative driving force Ag(S2O3)2 + e Ag(s) + 2S2O3 +0.010 for a half-cell reaction. -
Computer-Aided Analytical Methods - a Review
COMPUTER-AIDED ANALYTICAL METHODS - A REVIEW Läszlö Kekedy-Nagy Chair of Analytical Chemistry Faculty of Chemistry and Chemical Engineering Babe§-Bolyai University 3400 Cluj-Napoca, Romania INTRODUCTION Digital computers have become integral components of modern methods of analysis, influencing both instrument design and analytical methods. To understand the role of a computer in a specific instrumental method, it is necessary to consider the interaction among instrument, computer and analyst. Computers are being increasingly used in analytical work, but a survey of the literature shows that their potential has not yet been fully utilized. They offer enormous flexibility and sophistication in the execution and control of experiments, and their influence will doubtless be more and more widely felt. The following should be mentioned as main concerns: 1) Determination of the optimum analytical conditions, selecting the values of different parameters (e.g., the input signal) such that the best response is possible. In this respect, in order to avoid excessive experimental work and calculations and simplify operations, the mathematical modeling of the relations investi- gated is necessary. 2) Control of the measurement of analytical signals, used, e.g., to control the timing of different phases of the experiment, to prevent or warn against operator errors. 3) Data acquisition and storage of the analytical information. 4) Processing of analytical data is perhaps the main benefit that computers offer for analytical chemists. The computer makes it possible to qualify and classify the hidden information, using various chemometric methods including application of analytical intelligence, such as pattern recognition or expert control of chemical analysis systems. -
Hydrodynamic Studies of the Electrochemical Oxidation of Organic Fuels
Hydrodynamic Studies of the Electrochemical Oxidation of Organic Fuels by c Azam Sayadi A thesis submitted to the School of Graduate Studies in partial fulfilment of the requirements for the degree of Doctor of Philosophy Department of Chemistry Memorial University of Newfoundland September 2020 St. John's Newfoundland Abstract A clear understanding of small organic molecules (SOM) electrochemical oxidation opens a great opportunity for breakthrough in the development of fuel cell technology. SOM such as formic acid, methanol, and ethanol can produce electrical power through their oxidation in the fuel cell's anode. These molecules are also known as organic fuels and theoretically have the potential to produce close to 100% energy efficiency in a fuel cell. However, fast and complete oxidation of some organic fuels, such as ethanol, has not been achieved at this time, and has led to a dramatic decrease in the level of fuel cell efficiency. Therefore, a comprehensive study of the electrocatalytic oxidation mechanisms of organic fuels as well as a determination of the average number of transferred electrons (nav) are crucial for the enhancement of fuel cell efficiency. Hydrodynamic methods are highly effective approaches for these study purposes, and they have the ability to emulate the hydrodynamic conditions of a fuel cell anode. The main purpose of this project was establishing a simple and novel system for the assessment of various fuel cell catalysts performances in relation to formic acid, methanol and ethanol electrochemical oxidation. For this purpose, we applied two different approaches of hydrodynamic techniques, rotating disk voltammetry (RDV) and flow cell electrolysis. -
Electroanalytical Methods: Guide to Experiments and Applications, 2Nd
Electroanalytical Methods Fritz Scholz Editor Electroanalytical Methods Guide to Experiments and Applications Second, Revised and Extended Edition With contributions by A.M. Bond, R.G. Compton, D.A. Fiedler, G. Inzelt, H. Kahlert, Š. Komorsky-Lovric,´ H. Lohse, M. Lovric,´ F. Marken, A. Neudeck, U. Retter, F. Scholz, Z. Stojek 123 Editor Prof. Dr. Fritz Scholz University of Greifswald Inst. of Biochemistry Felix-Hausdorff-Str. 4 17487 Greifswald Germany [email protected] ISBN 978-3-642-02914-1 e-ISBN 978-3-642-02915-8 DOI 10.1007/978-3-642-02915-8 Springer Heidelberg Dordrecht London New York Library of Congress Control Number: 2009935962 © Springer-Verlag Berlin Heidelberg 2010 This work is subject to copyright. All rights are reserved, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilm or in any other way, and storage in data banks. Duplication of this publication or parts thereof is permitted only under the provisions of the German Copyright Law of September 9, 1965, in its current version, and permission for use must always be obtained from Springer. Violations are liable to prosecution under the German Copyright Law. The use of general descriptive names, registered names, trademarks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. Cover design: WMXDesign GmbH, Heidelberg Printed on acid-free paper Springer is part of Springer Science+Business Media (www.springer.com) Electroanalytical Methods Fritz Scholz dedicates this book to the memory of his late parents Anneliese and Herbert Scholz Preface to the Second Edition The authors are pleased to present here the second edition of the book “Electroanalytical Methods. -
Article an Alternative Method for the Simultaneous Determination of Copper and Lead for Quality Control of Sugar Cane Spirit Using a Nanotube-Based Sensor
J. Braz. Chem. Soc., Vol. 23, No. 9, 1614-1622, 2012. Printed in Brazil - ©2012 Sociedade Brasileira de Química A 0103 - 5053 $6.00+0.00 Article An Alternative Method for the Simultaneous Determination of Copper and Lead for Quality Control of Sugar Cane Spirit using a Nanotube-Based Sensor Elisângela de F. L. Tavares,a Leonardo L. Okumura,*,b Maria das Graças Cardoso,a Marcelo F. de Oliveirac, Zuy Maria Magriotisa and Adelir A. Saczk*,a aUniversidade Federal de Lavras, 37200-000 Lavras-MG, Brazil bUniversidade Federal de Viçosa, 36570-000 Viçosa-MG, Brazil cDepartamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, 14040-901 Ribeirão Preto, Brazil Um método eletroanalítico foi desenvolvido para determinação simultânea de íons cobre e chumbo em cachaça empregando eletrodo de pasta de carbono modificado com ácido ascórbico e nanotubos de carbono (CPE-AaCNT). A técnica de voltametria de onda quadrada (SWV) com redissolução anódica foi empregada e otimizada com relação aos seguintes parâmetros: frequência (50 Hz), amplitude (100 mV) e incremento de varredura (9 mV). As curvas analíticas apresentaram intervalo linear de 0,09 a 7,00 mg L–1 para o chumbo e para o cobre. Os limites de detecção foram de 48,5 e 23,9 µg L–1 para o chumbo e o cobre, respectivamente. O método desenvolvido foi aplicado na determinação simultânea de chumbo e cobre em cinco amostras comerciais de cachaça. Os resultados apresentaram-se concordantes com os obtidos por F AAS/GF AAS (espectrometria de absorção atômica com chama/espectrometria de absorção atômica com forno de grafite) e revelaram que CPE-AaCNT podem ser empregados com êxito na quantificação de cobre e chumbo em amostras comerciais de cachaça. -
Squarewave Voltammetry: a Review on the Recent Progress
Review Square-Wave Voltammetry: A Review on the Recent Progress Valentin Mirceski,*a, b Rubin Gulaboski,a, b Milivoj Lovric,c Ivan Bogeski,d Reinhard Kappl,d Markus Hothd a Institute of Chemistry, University “Ss Cyril and Methodius”, Skopje, Republic of Macedonia b University “Goce Delcev”, Stip, Republic of Macedonia c Medical Faculty, Center for Marine Research Zagreb, “Rud¯er Boskovic” Institute, Zagreb, Croatia d Department of Biophysics, University of Saarland, Homburg, Germany *e-mail: [email protected] Received: July 29, 2013 Accepted: September 20, 2013 Published online: && &&, 2013 Abstract A review on the recent progress of square-wave voltammetry is presented, covering the period of the last five years. The review addresses the new theoretical development of the technique as well as its application for mechanistic purposes, electrode kinetic measurements, biochemical and analytical applications. Besides, a few novel methodo- logical modifications are proposed that might expand the scope and application of the technique. Keywords: Square-wave voltammetry, Theory, Electrode mechanisms, Electrode kinetics DOI: 10.1002/elan.201300369 1 Introduction 2 Basic Features and New Methodological Concepts in SWV Square-wave voltammetry (SWV) is a powerful electro- chemical technique suitable for analytical application, 2.1 Basic Characteristics of SWV mechanistic study of electrode processes and electrokinet- ic measurements [1–6]. Nowadays it is considered as one Typical potential modulation used in SWV consists of of the most advanced voltammetric techniques, which a staircase potential ramp modified with square-shaped unifies the advantages of pulse techniques (enhanced sen- potential pulses (Figure 1A). At each step of the staircase sitivity), cyclic voltammetry (insight into the electrode ramp, two equal in height and oppositely directed poten- mechanism) and impedance techniques (kinetic informa- tial pulses are imposed. -
Présentation Powerpoint
Application Note General Electrochemistry AP-GE05 Staircase Voltammetry This Application Note describes how the Staircase Voltammetry method works by giving an example with Ferri/Ferrate solution. Application Note Introduction The Staircase Voltammetry is a flexible method to investigate and record voltammograms of any electrochemical samples. You can set the potential points versus OCP or reference electrode, define the step potential, step duration, scan rate and then start the test. What makes this method special is that the user can define the number of segment. By defining the segment, the number of sweeping (scanning) potential between two vertexes is defined. When the number of segment is 1, then there will be a single-sweep voltammogram. When the number of segment is even means to have complete cycles. Parameters The Parameters of the staircase voltammetry are shown in figure 1. With the above default settings, the potential 1 is set to -1000 mV versus REF electrode, then scan rate is set at 10 mV/s up to achieve to potential 2 which is defined as 1000 mV. In the segment part, the user can define the number of sweeps. In figure 2, different results corresponding to different number of segments are shown. Figure 1: The parameters 2 Application Note (1) The number of segment is 1 (2) The number of segment is 2 Figure 2: Final result, Potential vs Current When the segment is defined as 1, only single-sweep voltammogram will be gained. When the segment is defined as 2 (or any even number) the result will be a cyclic voltammogram. -
How to Cite Complete Issue More Information About This
Revista Cubana de Química ISSN: 0258-5995 ISSN: 2224-5421 Universidad de Oriente Vilasó-Cadre, Javier Ernesto; Arada-Pérez, María de los Ángeles; Arce-Castro, Jorge; Baeza-Reyes, Dr.C. Study of the potential sweeps in the manual staircase voltammetry Revista Cubana de Química, vol. 32, no. 2, 2020, May-August, pp. 287-298 Universidad de Oriente Available in: http://www.redalyc.org/articulo.oa?id=443564573008 How to cite Complete issue Scientific Information System Redalyc More information about this article Network of Scientific Journals from Latin America and the Caribbean, Spain and Journal's webpage in redalyc.org Portugal Project academic non-profit, developed under the open access initiative Rev. Cubana Quím. Vol.32, no.2 mayo-agosto, 2020, págs. 287-298, e-ISSN: 2224-5421 Artículo original Study of the potential sweeps in the manual staircase voltammetry Estudio de los barridos de potencial en la voltamperometría manual de barrido en escalera MSc. Javier Ernesto Vilasó-Cadre1* https://orcid.org/0000-0001-5172-7136 Dra.C. María de los Ángeles Arada-Pérez2 https://orcid.org/0000-0001-9262-2066 Jorge Arce-Castro2 https://orcid.org/0000-0002-5443-6796 Dr.C. José Alejandro Baeza-Reyes3 https://orcid.org/0000-0001-9621-8175 1Institute of Metallurgy. Universidad Autónoma de San Luis Potosí, México. 2Faculty of Natural and Exact Sciences. Universidad de Oriente, Santiago de Cuba, Cuba. 3Faculty of Chemistry. Universidad Nacional Autónoma de México. *Autor para la correspondencia. correo electrónico: [email protected] ABSTRACT Voltammetry can be developed using manual potentiostats. This study focuses on the potential sweeps and its influence on the voltammograms in the manual staircase voltammetry.