A new procedure for fast electrochemical analysis of solid materials

Scholz, Fritz; Nitschke, L.; Henrion, Günter

doi:10.1007/bf00396709

Cited by 135 publications

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“…A method which does not place very high demands on instrumentation, is well suited to routine phase analysis, and moreover, can be used on a micro scale, has been suggested by Scholz and coworkers 1,2 . The method is based on voltammetric measurement with a carbon electrode to which analyte particles are fixed by rubbing against sample, the authors named the technique "abrasive stripping voltammetry" (henceforth AbrSV).…”

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confidence: 99%

“…The method is based on voltammetric measurement with a carbon electrode to which analyte particles are fixed by rubbing against sample, the authors named the technique "abrasive stripping voltammetry" (henceforth AbrSV). The method is useful for the analysis and characterization of metal alloys 1 , minerals 2 , various inorganic binary mixtures 3 , pigments 4 , for the study of high-temperature superconductors 5 , for the calculation of thermodynamic constants of low soluble compounds 6,7 , etc. (a survey of applications has been presented in ref.…”

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Electrochemical Dissolution of Goethite by Abrasive Stripping Voltammetry

Grygar

Šubrt

Boháček

1995

Collect. Czech. Chem. Commun.

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Abrasive stripping voltammetry was applied to the investigation of the reductive dissolution of some iron(III) oxides and hydroxy-oxides, particularly goethite (α-FeOOH), in acid media. The electrode reaction directly involves the solid phase, and the reaction pathway depends on the phase composition and particle shape. This can be used for a qualitative and quantitative characterization of goethite. The results of a quantitative analysis of a mixture of goethite (α-FeOOH) and lepidocrocite (γ-FeOOH) are compared with those of IR and Moessbauer spectroscopic examination. The effects of the particle appearance (shape, crystal intergrowth) on the results of the voltammetric and chronoamperometric measurements are discussed.Direct analysis of powdered solids by electrochemical methods complements nicely conventional phase analysis methods such as powder X-ray analysis, IR spectroscopy and, for iron compounds, Moessbauer spectroscopy. In fact, each of the methods places some specific requirements on the phase crystallinity and particle size and the procedures are instrumentally demanding and time consuming and so that the possibility of resorting to alternative analytical methods is very appealing.A method which does not place very high demands on instrumentation, is well suited to routine phase analysis, and moreover, can be used on a micro scale, has been suggested by Scholz and coworkers 1,2 . The method is based on voltammetric measurement with a carbon electrode to which analyte particles are fixed by rubbing against sample, the authors named the technique "abrasive stripping voltammetry" (henceforth AbrSV). The method is useful for the analysis and characterization of metal alloys 1 , minerals 2 , various inorganic binary mixtures 3 , pigments 4 , for the study of high-temperature superconductors 5 , for the calculation of thermodynamic constants of low soluble compounds 6,7 , etc. (a survey of applications has been presented in ref. 8 ). Since electrode processes can generally involve higher order electrochemical reactions, diffusion, adsorption, and chemical reactions of the substance in the surroundings of the electrode, the overall reaction pathway is very complex 8 and interpretation of the voltammograms requires prior understanding of the conversion mechanism of the substance on the electrode and/or in its surroundings. 950Grygar, Subrt, Bohacek:

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confidence: 99%

Electrochemical Dissolution of Goethite by Abrasive Stripping Voltammetry

Grygar

Šubrt

Boháček

1995

Collect. Czech. Chem. Commun.

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“…A primeira publicação baseada nesta ideia reportou a análise de ligas de chumbo-antimônio. 2 A transferência foi realizada através da fricção da superfície inferior circular do PIGE sobre a superfície das ligas. Uma vez que a quantidade absoluta dos traços de liga transferidos por fricção não pode ser controlada e varia em alguma extensão de experimento para experimento, a avaliação dos voltamogramas foi baseada na porcentagem de corrente de cada pico em relação à soma das correntes de pico.…”

Section: Análise Elementarunclassified

“…Determinaram a estequiometria completa ou, ao menos, a proporção entre os constituintes metálicos nas amostras. Por exemplo, foi determinada a estequiometria completa para os compostos Tl 2 Outros trabalhos envolvendo o estudo da estequiometria de óxidos metálicos e calcogenetos empregando VIM são mostrados na Tabela 1.…”

Section: Análise Da Estequiometria De óXidos Metálicos E Calcogenetosunclassified

Voltametria de micropartículas imobilizadas: fundamentos e aplicações analíticas

Carvalho¹,

Hilgemann²,

Spengler³

et al. 2010

Quím. Nova

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Recebido em 9/11/09; aceito em 17/4/10; publicado na web em 1/9/10 VOLTAMMETRY OF IMMOBILIZED MICROPARTICLES: FUNDAMENTALS AND ANALYTICAL APPLICATIONS. The theoretical aspects of Voltammetry of Immobilized Microparticles (VIM) were discussed. The immobilization of microparticles on electrode surface, the electrode cleaning processes and the electrode materials were analyzed. The three-phase electrode model and the possible reactions between the immobilized particle and the electrolytic solution were discussed. In addition, this work discusses some selected applications of VIM published in the last years.Keywords: voltammetry of immobilized microparticles; solid materials; three-phase electrode. INTRODUÇÃOTradicionalmente, a eletroanalítica está associada aos estudos de substâncias dissolvidas em fases líquidas. Desde a descrição da voltametria por Kolthoff e Laitinen, em 1940, 1 este método analítico tornou-se o mais importante no campo da eletroquímica. Entretanto, para que estudos eletroanalíticos de substâncias sólidas fossem possíveis, novas estratégias experimentais e conceitos teóricos tiveram que ser aprimorados a fim de superar os problemas associados com a preparação da amostra e a eletroquímica de fases sólidas.Em 1989, as dificuldades experimentais puderam ser superadas com o surgimento de uma nova técnica desenvolvida por Scholz e colaboradores, 2,3 chamada inicialmente de voltametria abrasiva de redissolução (AbrSV -Abrasive Stripping Voltammetry) e, posteriormente, de voltametria de micropartículas imobilizadas (VIM -Voltammetry of Immobilized Microparticles).4 Esta técnica eletroanalítica baseia-se na imobilização de micropartículas de uma amostra sólida (menos de 1 μg) sobre a superfície de um eletrodo sólido adequado, o qual é imerso em um eletrólito líquido, e no subsequente registro de um sinal de corrente em função do potencial aplicado. 5,6 Os voltamogramas obtidos revelam informações sobre a composição química da amostra sólida.A imobilização de micropartículas tem se tornado um método bastante utilizado para ensaios diretos de sólidos devido à facilidade de preparação do eletrodo, evitando a dissolução da amostra, além de possibilitar uma análise rápida e de baixo custo.7 Além de ser um método indicado para determinações qualitativas e semiquantitativas, 8,9 também fornece informações sobre a cinética das reações redox de materiais sólidos. 4,10 Encontram-se, na literatura, textos dedicados exclusivamente à VIM, a exemplo de capítulos em livros-texto, 4,11 de alguns artigos de revisão publicados em periódicos especializados, 7,9,12 e um livro-texto dedicado aos seus fundamentos e aplicações, publicado por Scholz, Schröder e Gulaboski intitulado "Electrochemistry of Immobilized Particles and Droplets". 13Este artigo apresenta uma revisão sobre os fundamentos que envolvem a determinação voltamétrica de materiais sólidos e suas principais aplicações analíticas. Os principais tipos de eletrodos utilizados são descritos, assim como a sua limpeza e a imobilização mecânica de micropartículas à su...

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“…Abrasive stripping voltammetry (AbSV), also known as voltammetry of immobilized microparticles (VMP) is a simple, fast and cheap electrochemical technique first described by F. Scholz in the late 1980's [1,2]. It is a very versatile tool used for solid-state characterization [3,4].…”

Section: Introductionmentioning

confidence: 99%

Quantification of Tin and Lead in Binary Alloys Using Voltammetry of Immobilized Microparticles

Arjmand

Adriaens

2011

Electroanalysis

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Voltammetry of immobilized microparticles (VMP) has been used in this work for the quantitative determination of tin and lead particles in their binary alloys. Carbon paste electrodes, which contained small amounts of tin and lead or their mixtures, were used as working electrodes and square wave voltammograms of each electrode were recorded.Quantification was performed using optimum experimental conditions, obtained by an experimental design technique.The calibration was made by measuring the percentage peak height of each metal taking the sum of peak currents of the both metals as 100 %. The results were compared with quantitative results of X-ray fluorescence (XRF) technique to evaluate the capability of VMP method in its quantitative determination of solid samples.

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A new procedure for fast electrochemical analysis of solid materials

Cited by 135 publications

References 0 publications

Electrochemical Dissolution of Goethite by Abrasive Stripping Voltammetry

Electrochemical Dissolution of Goethite by Abrasive Stripping Voltammetry

Voltametria de micropartículas imobilizadas: fundamentos e aplicações analíticas

Quantification of Tin and Lead in Binary Alloys Using Voltammetry of Immobilized Microparticles

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