Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais

Detalhes bibliográficos
Ano de defesa: 2017
Autor(a) principal: Ibernom, Ana Carolina dos Santos lattes
Orientador(a): Braga, Neila de Almeida lattes
Banca de defesa: Farias, Marcos Antônio dos Santos, Paschoal, Fabiana Maria Monteiro
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal do Amazonas
Programa de Pós-Graduação: Programa de Pós-graduação em Química
Departamento: Instituto de Ciências Exatas
País: Brasil
Palavras-chave em Português:
Área do conhecimento CNPq:
Link de acesso: https://tede.ufam.edu.br/handle/tede/6474
Resumo: Contamination by potentially toxic metals in aquatic bodies and fuel ethanol has caused significant detrimental changes in the physical, chemical and biological behavior of the recipient bodies, and consequently of the environment. The detection of these metals is generally accomplished by means of spectroscopic techniques which require the use of expensive materials for the industry. Currently, searching for a more cost-effective alternative and having adequate selectivity, sensitivity and reproducibility in the detection of these contaminants, it is necessary that reliable methodologies in the determination of these metallic ions are imposed. This work had the objective of analyzing the redemulsion voltammetries as important techniques in trace metal analysis taking into account the structure of the electrodes used. There are no papers in the literature that perform a correlation on the different forms of microstructures and morphologies of Boron Doped Diamond (DDB) electrodes in the determination of Cu2 + and Fe2 + ions in aqueous and ethanolic environments, using the Anodic Redissolution Voltammetry Technique coupled to Square Wave Voltametry (VRA/VOQ). It was selected as electrolyte support in aqueous medium the 1M KCl and for ethanolic medium 0.04M H2SO4 for Cu and 0.04M HCl for Fe. For the study of the structure and morphology of the electrodes were used the optimized parameters of two works developed in the Laboratory of Inorganic Chemistry Research (LPQI) in relation to the determination of copper and iron in aqueous media (FERREIRA, 2013) and fuel ethanol (PEREIRA, 2015). In this work, the influence of the microstructure and morphology of the DDB electrodes was discussed in more depth, highlighting the importance of these structures for the detection of the metals and their application in real samples. The methodology was submitted to validation, where the figures of the merit were validated: selectivity, linearity, precision (interdia test), accuracy (percentage of recovery) and limits of detection and quantification. The results indicated that the nanocrystalline sample (DNDB) presented the best response for detections in both aqueous and ethanolic environments, presenting the best limits of detection and quantification (LD ranging from 2,44x10-4 to 3,69x10-4; LQ ranging from 3,26x10-4 to 3,84x10-4) due to its morphology and structure when compared to the other electrodes. In addition to presenting a larger window of potential and the voltammogram of the process of reversibility better defined.
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spelling Braga, Neila de Almeida31505520282http://lattes.cnpq.br/8772300241940971Farias, Marcos Antônio dos SantosPaschoal, Fabiana Maria Monteiroppgq@ufam.edu.br96037458200carolibernom@gmail.comDD/UFAM: 298/2018http://lattes.cnpq.br/2444509738014487Ibernom, Ana Carolina dos Santos2018-06-20T15:10:05Z2017-12-07IBERNOM, Ana Carolina dos Santos.Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais. 2017. 111 f. Dissertação (Mestrado em Química) - Universidade Federal do Amazonas, Manaus, 2017.https://tede.ufam.edu.br/handle/tede/6474Contamination by potentially toxic metals in aquatic bodies and fuel ethanol has caused significant detrimental changes in the physical, chemical and biological behavior of the recipient bodies, and consequently of the environment. The detection of these metals is generally accomplished by means of spectroscopic techniques which require the use of expensive materials for the industry. Currently, searching for a more cost-effective alternative and having adequate selectivity, sensitivity and reproducibility in the detection of these contaminants, it is necessary that reliable methodologies in the determination of these metallic ions are imposed. This work had the objective of analyzing the redemulsion voltammetries as important techniques in trace metal analysis taking into account the structure of the electrodes used. There are no papers in the literature that perform a correlation on the different forms of microstructures and morphologies of Boron Doped Diamond (DDB) electrodes in the determination of Cu2 + and Fe2 + ions in aqueous and ethanolic environments, using the Anodic Redissolution Voltammetry Technique coupled to Square Wave Voltametry (VRA/VOQ). It was selected as electrolyte support in aqueous medium the 1M KCl and for ethanolic medium 0.04M H2SO4 for Cu and 0.04M HCl for Fe. For the study of the structure and morphology of the electrodes were used the optimized parameters of two works developed in the Laboratory of Inorganic Chemistry Research (LPQI) in relation to the determination of copper and iron in aqueous media (FERREIRA, 2013) and fuel ethanol (PEREIRA, 2015). In this work, the influence of the microstructure and morphology of the DDB electrodes was discussed in more depth, highlighting the importance of these structures for the detection of the metals and their application in real samples. The methodology was submitted to validation, where the figures of the merit were validated: selectivity, linearity, precision (interdia test), accuracy (percentage of recovery) and limits of detection and quantification. The results indicated that the nanocrystalline sample (DNDB) presented the best response for detections in both aqueous and ethanolic environments, presenting the best limits of detection and quantification (LD ranging from 2,44x10-4 to 3,69x10-4; LQ ranging from 3,26x10-4 to 3,84x10-4) due to its morphology and structure when compared to the other electrodes. In addition to presenting a larger window of potential and the voltammogram of the process of reversibility better defined.contaminação por metais potencialmente tóxicos em corpos aquáticos e etanol combustível tem provocado alterações prejudiciais significativas nos comportamentos físicos, químicos e biológicos dos corpos receptores, e, consequentemente, do meio ambiente. A detecção destes metais é geralmente realizada por meio de técnicas espectroscópicas que requerem a utilização de equipamentos onerosos para a indústria. Atualmente, buscando uma alternativa mais viável quanto ao custo e que possua uma seletividade adequada, sensibilidade e reprodutibilidade na detecção destes contaminantes é necessário que sejam impostas metodologias confiáveis na determinação desses íons metálicos. Este trabalho teve como objetivo analisar as voltametrias de redissolução como técnicas importantes na análise de metais-traço levando em conta a estrutura dos eletrodos utilizados. Não há na literatura trabalhos que realizem uma correlação acerca das diferentes formas de microestruturas e morfologias dos eletrodos de Diamante Dopados com Boro (DDB) na detecção de íons Cu2+ e Fe2+ em meio aquoso e etanólico, empregando a Técnica de Voltametria de Redissolução Anódica acoplada à Voltametria de Onda Quadrada (VRA/VOQ). Foi selecionado como eletrólito suporte em meio aquoso o KCl 1M e para meio etanólico o H2SO4 0,04 M para o Cu e o HCl 0,04 M para o Fe. Para o estudo da estrutura e morfologia dos eletrodos foram utilizados os parâmetros otimizados de dois trabalhos desenvolvidos no Laboratório de Pesquisas em Química Inorgânica (LPQI) com relação à determinação de Cu2+ e Fe2+ em meio aquoso (FERREIRA, 2013) e etanol combustível (PEREIRA, 2015). Neste trabalho foi abordado de forma mais aprofundada a influência da microestrutura e morfologia dos eletrodos DDB, destacando qual a importância destes para a detecção dos metais abordados e aplicação dos mesmos em amostras reais. A metodologia foi submetida a validação, onde foram validadas as figuras do mérito: seletividade, a linearidade, a precisão (ensaio interdia), a exatidão (percentual de recuperação) e os limites de detecção e quantificação. Os resultados indicaram que a amostra nanocristalina (DNDB) apresentou melhor resposta para as detecções tanto em meio aquoso, quanto em meio etanólico, apresentando os melhores limites de detecção e quantificação (LD variando de 2,44x10-4 a 3,69x10-4; LQ variando de 3,26x10-4 a 3,84x10-4) devido a sua morfologia e estrutura quando comparado aos demais eletrodos. Além do fato de apresentar uma maior janela de potencial e o voltamograma do processo de reversibilidade mais bem definido.Submitted by Divisão de Documentação/BC Biblioteca Central (ddbc@ufam.edu.br) on 2018-06-20T15:09:37Z No. of bitstreams: 2 license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Dissertação - versão FINAL.pdf: 4610535 bytes, checksum: 5d31fadc3fa46f36a713a7d60d2dad1e (MD5)Approved for entry into archive by Divisão de Documentação/BC Biblioteca Central (ddbc@ufam.edu.br) on 2018-06-20T15:10:05Z (GMT) No. of bitstreams: 2 license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Dissertação - versão FINAL.pdf: 4610535 bytes, checksum: 5d31fadc3fa46f36a713a7d60d2dad1e (MD5)Made available in DSpace on 2018-06-20T15:10:05Z (GMT). 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dc.title.por.fl_str_mv Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais
title Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais
spellingShingle Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais
Ibernom, Ana Carolina dos Santos
Voltametria
Morfologia - Eletrodos DDB
Detecção de metais
CIÊNCIAS EXATAS E DA TERRA: QUÍMICA
title_short Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais
title_full Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais
title_fullStr Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais
title_full_unstemmed Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais
title_sort Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais
author Ibernom, Ana Carolina dos Santos
author_facet Ibernom, Ana Carolina dos Santos
author_role author
dc.contributor.advisor1email.por.fl_str_mv ppgq@ufam.edu.br
dc.contributor.advisor1.fl_str_mv Braga, Neila de Almeida
dc.contributor.advisor1ID.fl_str_mv 31505520282
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/8772300241940971
dc.contributor.referee1.fl_str_mv Farias, Marcos Antônio dos Santos
dc.contributor.referee2.fl_str_mv Paschoal, Fabiana Maria Monteiro
dc.contributor.authorID.fl_str_mv 96037458200
carolibernom@gmail.com
DD/UFAM: 298/2018
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/2444509738014487
dc.contributor.author.fl_str_mv Ibernom, Ana Carolina dos Santos
contributor_str_mv Braga, Neila de Almeida
Farias, Marcos Antônio dos Santos
Paschoal, Fabiana Maria Monteiro
dc.subject.por.fl_str_mv Voltametria
Morfologia - Eletrodos DDB
Detecção de metais
topic Voltametria
Morfologia - Eletrodos DDB
Detecção de metais
CIÊNCIAS EXATAS E DA TERRA: QUÍMICA
dc.subject.cnpq.fl_str_mv CIÊNCIAS EXATAS E DA TERRA: QUÍMICA
description Contamination by potentially toxic metals in aquatic bodies and fuel ethanol has caused significant detrimental changes in the physical, chemical and biological behavior of the recipient bodies, and consequently of the environment. The detection of these metals is generally accomplished by means of spectroscopic techniques which require the use of expensive materials for the industry. Currently, searching for a more cost-effective alternative and having adequate selectivity, sensitivity and reproducibility in the detection of these contaminants, it is necessary that reliable methodologies in the determination of these metallic ions are imposed. This work had the objective of analyzing the redemulsion voltammetries as important techniques in trace metal analysis taking into account the structure of the electrodes used. There are no papers in the literature that perform a correlation on the different forms of microstructures and morphologies of Boron Doped Diamond (DDB) electrodes in the determination of Cu2 + and Fe2 + ions in aqueous and ethanolic environments, using the Anodic Redissolution Voltammetry Technique coupled to Square Wave Voltametry (VRA/VOQ). It was selected as electrolyte support in aqueous medium the 1M KCl and for ethanolic medium 0.04M H2SO4 for Cu and 0.04M HCl for Fe. For the study of the structure and morphology of the electrodes were used the optimized parameters of two works developed in the Laboratory of Inorganic Chemistry Research (LPQI) in relation to the determination of copper and iron in aqueous media (FERREIRA, 2013) and fuel ethanol (PEREIRA, 2015). In this work, the influence of the microstructure and morphology of the DDB electrodes was discussed in more depth, highlighting the importance of these structures for the detection of the metals and their application in real samples. The methodology was submitted to validation, where the figures of the merit were validated: selectivity, linearity, precision (interdia test), accuracy (percentage of recovery) and limits of detection and quantification. The results indicated that the nanocrystalline sample (DNDB) presented the best response for detections in both aqueous and ethanolic environments, presenting the best limits of detection and quantification (LD ranging from 2,44x10-4 to 3,69x10-4; LQ ranging from 3,26x10-4 to 3,84x10-4) due to its morphology and structure when compared to the other electrodes. In addition to presenting a larger window of potential and the voltammogram of the process of reversibility better defined.
publishDate 2017
dc.date.issued.fl_str_mv 2017-12-07
dc.date.accessioned.fl_str_mv 2018-06-20T15:10:05Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
format masterThesis
status_str publishedVersion
dc.identifier.citation.fl_str_mv IBERNOM, Ana Carolina dos Santos.Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais. 2017. 111 f. Dissertação (Mestrado em Química) - Universidade Federal do Amazonas, Manaus, 2017.
dc.identifier.uri.fl_str_mv https://tede.ufam.edu.br/handle/tede/6474
identifier_str_mv IBERNOM, Ana Carolina dos Santos.Estudo da influência da estrutura e morfologia de eletrodos de diamante dopados com boro na detecção de metais. 2017. 111 f. Dissertação (Mestrado em Química) - Universidade Federal do Amazonas, Manaus, 2017.
url https://tede.ufam.edu.br/handle/tede/6474
dc.language.iso.fl_str_mv por
language por
dc.relation.department.fl_str_mv -8156311678363143599
dc.relation.confidence.fl_str_mv 500
dc.rights.driver.fl_str_mv http://creativecommons.org/licenses/by-nc-nd/4.0/
info:eu-repo/semantics/openAccess
rights_invalid_str_mv http://creativecommons.org/licenses/by-nc-nd/4.0/
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal do Amazonas
dc.publisher.program.fl_str_mv Programa de Pós-graduação em Química
dc.publisher.initials.fl_str_mv UFAM
dc.publisher.country.fl_str_mv Brasil
dc.publisher.department.fl_str_mv Instituto de Ciências Exatas
publisher.none.fl_str_mv Universidade Federal do Amazonas
dc.source.none.fl_str_mv reponame:Biblioteca Digital de Teses e Dissertações da UFAM
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reponame_str Biblioteca Digital de Teses e Dissertações da UFAM
collection Biblioteca Digital de Teses e Dissertações da UFAM
bitstream.url.fl_str_mv http://localhost:8080//bitstream/tede/6474/1/license.txt
http://localhost:8080//bitstream/tede/6474/2/license_url
http://localhost:8080//bitstream/tede/6474/3/license_text
http://localhost:8080//bitstream/tede/6474/4/license_rdf
http://localhost:8080//bitstream/tede/6474/5/Disserta%C3%A7%C3%A3o_Ana+Carolina+Ibernom
http://localhost:8080//bitstream/tede/6474/6/Disserta%C3%A7%C3%A3o_Ana+Carolina+Ibernom.txt
http://localhost:8080//bitstream/tede/6474/7/Disserta%C3%A7%C3%A3o_Ana+Carolina+Ibernom.jpg
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bitstream.checksumAlgorithm.fl_str_mv MD5
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repository.name.fl_str_mv Biblioteca Digital de Teses e Dissertações da UFAM - Universidade Federal do Amazonas (UFAM)
repository.mail.fl_str_mv ddbc@ufam.edu.br
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