A simple and convenient solid state microanalytical technique for identification and characterization of the high temperature superconductor YBa2Cu3O7−x

Scholz, Fritz; Nitschke, L.; Kemnitz, Erhard; Olesch, T.; Henrion, Günter; Hass, Dieter; Bagchi, R. N.; Herrmann, R.; Pruss, N.; Wilde, Willy De

doi:10.1007/bf00474252

Cited by 19 publications

(6 citation statements)

References 4 publications

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“…Another example is the determination of the oxidation state of sulfur in different thallium sulfides [174]: That method is based on measuring in a first step the charge consumed for reduction of the thallium sulfide to thallium, and in a following step the determination of the charge of oxidation of the thallium metal. The metal ratios of high-temperature superconductors have also been determined by SSEAC [175]. The ratios of the constituents of alloys can be easily determined based on the oxidation signals of the single constituents [46][47][48][49][50][51][52][53][54].…”

Section: Quantitative Analysismentioning

confidence: 99%

Electroanalytical chemistry for the analysis of solids: Characterization and classification (IUPAC Technical Report)

Doménech‐Carbó

Labuda

Scholz

2012

Pure and Applied Chemistry

155

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Solid state electroanalytical chemistry (SSEAC) deals with studies of the processes, materials, and methods specifically aimed to obtain analytical information (quantitative elemental composition, phase composition, structure information, and reactivity) on solid materials by means of electrochemical methods. The electrochemical characterization of solids is not only crucial for electrochemical applications of materials (e.g., in batteries, fuel cells, corrosion protection, electrochemical machining, etc.) but it lends itself also for providing analytical information on the structure and chemical and mineralogical composition of solid materials of all kinds such as metals and alloys, various films, conducting polymers, and materials used in nanotechnology. The present report concerns the relationships between molecular electrochemistry (i.e., solution electrochemistry) and solid state electrochemistry as applied to analysis. Special attention is focused on a critical evaluation of the different types of analytical information that are accessible by SSEAC.

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Section: Quantitative Analysismentioning

confidence: 99%

Electroanalytical chemistry for the analysis of solids: Characterization and classification (IUPAC Technical Report)

Doménech‐Carbó

Labuda

Scholz

2012

Pure and Applied Chemistry

155

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“…Este fenômeno tem sido demonstrado em numerosos casos de compostos contendo íons metálicos eletroativos em ambientes de coordenação diferentes, como em sítios octaédricos e tetraédricos de óxidos (Ti n+ em amostras de zeólitas), 71 ou íons Cu n+ em óxidos de diversas composições, exibindo vários comportamentos eletroquímicos. 57,58 Outros exemplos de especiação redox em amostras sólidas estão listados na Tabela 1.…”

Section: Análise De Especiação Redox Em Sólidosunclassified

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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“…Remarkable results were achieved by mechanical deposition of extremely low amounts of solid powder substances on to a paraffin-impregnated graphite electrode [8,9,10,11,12,13,14,15,16,17,18]. The current-potential curves recorded by abrasive "stripping" voltammetry of such solid materials can be directly analyzed qualitatively and quantitatively.…”

Section: Introductionmentioning

confidence: 97%

“…Recently it was shown that in the large spectrum of electroanalytical methods [3], anodic dissolution has been used for both qualitative and quantitative analysis of metals and alloys [4,5,6,7,8,9,10,11,12,13,14,15,16,17,18]. A number of these fall into the category of "stripping analysis", implying that only thin surface layers of the samples are dissolved so that the methods could be considered almost as non-destructive.…”

Section: Introductionmentioning

confidence: 99%

Determination of lead in an Sb-Pb alloy by anodic linear scan voltammetry

Vr²,

et al. 2001

Fresenius' Journal of Analytical Chemistry

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Anodic linear scan voltammetry (ALSV) has been used to determine the content of Pb (up to 3.5 wt%) in a eutectic type of binary Sb-Pb alloy. The effect of type of electrolyte and as well as the rate of the potential change on the dissolution of Pb from this alloy were investigated by ALSV. The method can be used for the determination of low concentrations of Pb in the investigated alloy and well-defined current peaks of Pb dissolution can be detected on the voltammograms. Well-defined linear dependencies between the quantities of electricity under the current peak of Pb dissolution (Q Pb ) and the respective contents of Pb (w) in the alloy, so-called "check curves", were found. The smallest ratio of Pb in Sb-Pb alloy which could be detected by ALSV was 0.45 wt%.The dissolution involves only ten atomic layers of the less precious metal (Pb) from the surface of the alloy samples.

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A simple and convenient solid state microanalytical technique for identification and characterization of the high temperature superconductor YBa2Cu3O7−x

Cited by 19 publications

References 4 publications

Electroanalytical chemistry for the analysis of solids: Characterization and classification (IUPAC Technical Report)

Electroanalytical chemistry for the analysis of solids: Characterization and classification (IUPAC Technical Report)

Voltametria de micropartículas imobilizadas: fundamentos e aplicações analíticas

Determination of lead in an Sb-Pb alloy by anodic linear scan voltammetry

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