Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas

Detalhes bibliográficos
Ano de defesa: 2023
Autor(a) principal: Martins, Matheus Henrique lattes
Orientador(a): Pissetti, Fábio Luiz lattes
Banca de defesa: Ribeiro, Emerson Schwingel, Cordeiro, Márcia Regina
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Alfenas
Programa de Pós-Graduação: Programa de Pós-Graduação em Química
Departamento: Instituto de Química
País: Brasil
Palavras-chave em Português:
Área do conhecimento CNPq:
Link de acesso: https://repositorio.unifal-mg.edu.br/handle/123456789/2242
Resumo: Functionalized materials have been the target of study in several areas of interest, among them, the manufacture of chemically modified electrodes for application as electrochemical sensors. In this work, a polymeric network of poly (dimethylsiloxane) (PDMS) functionalized with sulphonic group containing metallic nanoparticles was prepared to obtain an electrode material for use as electrochemical sensor. For this porpouse, a functionalized polymeric network was prepared with PDMS and 3-mercaptopropyltrimethoxysilane (3- MPTMS), then hydrogen peroxide was added to promote oxidation of the thiol group, obtaining the functionalized material with sulphonic group (PSO). Materials containing metallic nanoparticles silver (PSOAg) and gold (PSOAu) were also prepared, adding these species during the preparation of the networks. The prepared materials were characterized by thermogravimetric analysis (TG) and Fourier Transform Infrared Spectroscopy (FTIR). Results indicate the formation of the proposed polymeric network. Then, working electrodes were prepared: Graphite was added to PSO, PSOAg and PSOAu, in the proportion 1:0.5, network:graphite, m:m. The electrochemical behavior of the material was evaluated by cyclic voltametry (CV) and electrochemical impedance spectroscopy (EIS). The electrodes containing the metallic nanoparticles (PSOAg/Graphite and PSOAu/Graphite) presented the best responses in the study with the probe molecule ([Fe(CN) 6 ] 3-/4 . Among them, a smaller difference in anodic and cathode potential, ratio of anodic/cathodic current density near to one and also higher intensities of peak current densities. In order to evaluate the applicability of the electrode as a sensor, CV measurements were performed to determine copper, where oxidation potentials of -0.05 V were obtained for the PSOAg/Graphite electrode and 0.06 for the PSOAu/Graphite electrode. With square wave voltametry, oxidation potentials of -0.27 V were obtained for the electrode containing silver nanoparticles and -0.25 V for the electrode containing gold nanoparticles, while the detection limits were 0.13 μmol.L -1 and 0.04 μmol.L - 1 , respectively.
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spelling Martins, Matheus Henriquehttp://lattes.cnpq.br/4560803280050919Lucho, Alzira Maria SerpaRibeiro, Emerson SchwingelCordeiro, Márcia ReginaPissetti, Fábio Luizhttp://lattes.cnpq.br/05570079647705602023-05-25T12:27:09Z2024-02-292023-02-27MARTINS, Matheus Henrique. Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas. 2023. 97 f. Dissertação (Mestrado em Química) - Universidade Federal de Alfenas, Alfenas, MG, 2023.https://repositorio.unifal-mg.edu.br/handle/123456789/2242Functionalized materials have been the target of study in several areas of interest, among them, the manufacture of chemically modified electrodes for application as electrochemical sensors. In this work, a polymeric network of poly (dimethylsiloxane) (PDMS) functionalized with sulphonic group containing metallic nanoparticles was prepared to obtain an electrode material for use as electrochemical sensor. For this porpouse, a functionalized polymeric network was prepared with PDMS and 3-mercaptopropyltrimethoxysilane (3- MPTMS), then hydrogen peroxide was added to promote oxidation of the thiol group, obtaining the functionalized material with sulphonic group (PSO). Materials containing metallic nanoparticles silver (PSOAg) and gold (PSOAu) were also prepared, adding these species during the preparation of the networks. The prepared materials were characterized by thermogravimetric analysis (TG) and Fourier Transform Infrared Spectroscopy (FTIR). Results indicate the formation of the proposed polymeric network. Then, working electrodes were prepared: Graphite was added to PSO, PSOAg and PSOAu, in the proportion 1:0.5, network:graphite, m:m. The electrochemical behavior of the material was evaluated by cyclic voltametry (CV) and electrochemical impedance spectroscopy (EIS). The electrodes containing the metallic nanoparticles (PSOAg/Graphite and PSOAu/Graphite) presented the best responses in the study with the probe molecule ([Fe(CN) 6 ] 3-/4 . Among them, a smaller difference in anodic and cathode potential, ratio of anodic/cathodic current density near to one and also higher intensities of peak current densities. In order to evaluate the applicability of the electrode as a sensor, CV measurements were performed to determine copper, where oxidation potentials of -0.05 V were obtained for the PSOAg/Graphite electrode and 0.06 for the PSOAu/Graphite electrode. With square wave voltametry, oxidation potentials of -0.27 V were obtained for the electrode containing silver nanoparticles and -0.25 V for the electrode containing gold nanoparticles, while the detection limits were 0.13 μmol.L -1 and 0.04 μmol.L - 1 , respectively.Os materiais funcionalizados têm sido alvo de estudo em diversas áreas de interesse, dentre elas, a confecção de eletrodos quimicamente modificados para aplicação como sensores eletroquímicos. Neste trabalho foi preparada uma rede polimérica de poli(dimetilsiloxano) (PDMS) funcionalizada com grupo sulfônico contendo nanopartículas metálicas visando a obtenção de um material eletródico para utilização como sensor eletroquímico para determinação de cobre. Para tal, uma rede polimérica funcionalizada foi preparada com PDMS, 3-mercaptopropiltrimetoxisilano, em seguida, foi adicionado peróxido de hidrogênio no ambiente reacional para promover a oxidação do grupo tiol, obtendo o material funcionalizado com grupo sulfônico (PSO). Também foram preparados materiais contendo nanopartículas metálicas, de prata (PSOAg) e de ouro (PSOAu), adicionando essas espécies durante a preparação das redes. Os materiais preparados foram caracterizados por análise termogravimétrica (TG) e espectroscopia na região do infravermelho com transformada de Fourier (FTIR), indicando a formação da rede polimérica proposta. Em seguida, foram confeccionados eletrodos de trabalho, pela adição de grafite ao PSO, PSOAg e PSOAu, na proporção 1:0,5, rede:grafite, m:m. O comportamento eletroquímico do material foi avaliado por voltametria cíclica (VC) e espectroscopia de impedância eletroquímica (EIE). Os eletrodos contendo as nanopartículas metálicas (PSOAg/Grafite e PSOAu/Grafite) apresentaram as melhores respostas no estudo com a molécula sonda (K 3 Fe(CN) 6 ). Dentre estas, uma menor diferença de potencial anódico e catódico, razão de densidade de corrente anódica/catódica próxima a um e também maiores intensidades de densidades de correntes de pico. Com o intuito de avaliar a aplicabilidade do eletrodo como sensor foram realizadas medidas de VC para determinação do cobre, onde se obteve potenciais de oxidação de -0,05 V para o eletrodo PSOAg/Grafite e 0,06 para o eletrodo PSOAu/Grafite. Com a voltametria de onda quadrada, obteve-se os potenciais de oxidação de -0,27 V para o eletrodo contendo nanopartículas de prata e -0,25 V para o eletrodo contendo nanopartículas de ouro, enquanto os limites de detecção foram de 0,13 μmol.L -1 e 0,04 μmol.L -1 , respectivamente.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESapplication/pdfporUniversidade Federal de AlfenasPrograma de Pós-Graduação em QuímicaUNIFAL-MGBrasilInstituto de Químicainfo:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by-nc-nd/4.0/PolidimetilsiloxanoGrupo SulfônicoNanopartículas MetálicasEletrodo Quimicamente ModificadoCobreQUIMICA::QUIMICA INORGANICACaracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicasinfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/publishedVersion132825307882678230660060060031391270652389310962075167498588264571reponame:Repositório Institucional da Universidade Federal de Alfenas - RiUnifalinstname:Universidade Federal de Alfenas (UNIFAL)instacron:UNIFALMartins, Matheus HenriqueLICENSElicense.txtlicense.txttext/plain; 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dc.title.pt-BR.fl_str_mv Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas
title Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas
spellingShingle Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas
Martins, Matheus Henrique
Polidimetilsiloxano
Grupo Sulfônico
Nanopartículas Metálicas
Eletrodo Quimicamente Modificado
Cobre
QUIMICA::QUIMICA INORGANICA
title_short Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas
title_full Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas
title_fullStr Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas
title_full_unstemmed Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas
title_sort Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas
author Martins, Matheus Henrique
author_facet Martins, Matheus Henrique
author_role author
dc.contributor.author.fl_str_mv Martins, Matheus Henrique
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/4560803280050919
dc.contributor.advisor-co1.fl_str_mv Lucho, Alzira Maria Serpa
dc.contributor.referee1.fl_str_mv Ribeiro, Emerson Schwingel
dc.contributor.referee2.fl_str_mv Cordeiro, Márcia Regina
dc.contributor.advisor1.fl_str_mv Pissetti, Fábio Luiz
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/0557007964770560
contributor_str_mv Lucho, Alzira Maria Serpa
Ribeiro, Emerson Schwingel
Cordeiro, Márcia Regina
Pissetti, Fábio Luiz
dc.subject.por.fl_str_mv Polidimetilsiloxano
Grupo Sulfônico
Nanopartículas Metálicas
Eletrodo Quimicamente Modificado
Cobre
topic Polidimetilsiloxano
Grupo Sulfônico
Nanopartículas Metálicas
Eletrodo Quimicamente Modificado
Cobre
QUIMICA::QUIMICA INORGANICA
dc.subject.cnpq.fl_str_mv QUIMICA::QUIMICA INORGANICA
description Functionalized materials have been the target of study in several areas of interest, among them, the manufacture of chemically modified electrodes for application as electrochemical sensors. In this work, a polymeric network of poly (dimethylsiloxane) (PDMS) functionalized with sulphonic group containing metallic nanoparticles was prepared to obtain an electrode material for use as electrochemical sensor. For this porpouse, a functionalized polymeric network was prepared with PDMS and 3-mercaptopropyltrimethoxysilane (3- MPTMS), then hydrogen peroxide was added to promote oxidation of the thiol group, obtaining the functionalized material with sulphonic group (PSO). Materials containing metallic nanoparticles silver (PSOAg) and gold (PSOAu) were also prepared, adding these species during the preparation of the networks. The prepared materials were characterized by thermogravimetric analysis (TG) and Fourier Transform Infrared Spectroscopy (FTIR). Results indicate the formation of the proposed polymeric network. Then, working electrodes were prepared: Graphite was added to PSO, PSOAg and PSOAu, in the proportion 1:0.5, network:graphite, m:m. The electrochemical behavior of the material was evaluated by cyclic voltametry (CV) and electrochemical impedance spectroscopy (EIS). The electrodes containing the metallic nanoparticles (PSOAg/Graphite and PSOAu/Graphite) presented the best responses in the study with the probe molecule ([Fe(CN) 6 ] 3-/4 . Among them, a smaller difference in anodic and cathode potential, ratio of anodic/cathodic current density near to one and also higher intensities of peak current densities. In order to evaluate the applicability of the electrode as a sensor, CV measurements were performed to determine copper, where oxidation potentials of -0.05 V were obtained for the PSOAg/Graphite electrode and 0.06 for the PSOAu/Graphite electrode. With square wave voltametry, oxidation potentials of -0.27 V were obtained for the electrode containing silver nanoparticles and -0.25 V for the electrode containing gold nanoparticles, while the detection limits were 0.13 μmol.L -1 and 0.04 μmol.L - 1 , respectively.
publishDate 2023
dc.date.accessioned.fl_str_mv 2023-05-25T12:27:09Z
dc.date.issued.fl_str_mv 2023-02-27
dc.date.available.fl_str_mv 2024-02-29
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
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dc.identifier.citation.fl_str_mv MARTINS, Matheus Henrique. Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas. 2023. 97 f. Dissertação (Mestrado em Química) - Universidade Federal de Alfenas, Alfenas, MG, 2023.
dc.identifier.uri.fl_str_mv https://repositorio.unifal-mg.edu.br/handle/123456789/2242
identifier_str_mv MARTINS, Matheus Henrique. Caracterização eletroquímica de poli(dimetilsiloxano) funcionalizado com grupo sulfônico contendo nanopartículas metálicas. 2023. 97 f. Dissertação (Mestrado em Química) - Universidade Federal de Alfenas, Alfenas, MG, 2023.
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dc.publisher.country.fl_str_mv Brasil
dc.publisher.department.fl_str_mv Instituto de Química
publisher.none.fl_str_mv Universidade Federal de Alfenas
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repository.name.fl_str_mv Repositório Institucional da Universidade Federal de Alfenas - RiUnifal - Universidade Federal de Alfenas (UNIFAL)
repository.mail.fl_str_mv repositorio@unifal-mg.edu.br
_version_ 1859830899944718336