Imobilização de íons ferricianeto sobre eletrodo de ouro e desenvolvimento de um sistema dip-coating para elaboração de eletrodos modificados

Detalhes bibliográficos
Ano de defesa: 2014
Autor(a) principal: ALMEIDA JÚNIOR, Pedro Lemos de lattes
Orientador(a): NASCIMENTO, Valberes Bernardo do
Banca de defesa: Não Informado pela instituição
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal Rural de Pernambuco
Programa de Pós-Graduação: Programa de Pós-Graduação em Química
Departamento: Departamento de Química
País: Brasil
Palavras-chave em Português:
Área do conhecimento CNPq:
Link de acesso: http://www.tede2.ufrpe.br:8080/tede2/handle/tede2/7045
Resumo: The development of multilayer self-assembled films using the Layer Layer (LbL) approach has showed a high efficiency on the fabrication o ultrathin films. The LbL technique have been successfully and increasingly employed on developing new arquitectures for immobilization of enzymes, catalysts, electron mediators and other chemicals on conventional solid electrode surfaces for the development of electrochemical sensors and biosensors. This work followed two main paths: it was proposed the development and application of a new miniaturized dip-coating equipment, named LbL System, for the preparation of multilayers thin films on solid electrodes, and also a new method for the modification of gold electrodes for the immobilization of ferricyanide ions into a silica network, with application for the determination of nitrite ions. The proposed LbL System is automatic and has an embedded microcontroller that simplifies its hardware and software, and also favors its miniaturization. The system makes it possible all the modification process of being carried out automatically without attendance during the operation, only requiring the definition of some parameters by the user. The development of the equipment was based on a new concept of dip-coating, where, the solution flows to a fixed electrode instead of dipping the electrode in the solution, as it happens at all the commercial equipments, making possible to work with microvolumes of reagents and solutions keeping a high reproducibility of the modification process. The proposed new method for immobilization of ferricyanide ions on gold electrodes was based on its affinity with a silica network modified with a spacer containing amine terminal groups, anchored on the surface via silanol groups of the opposite terminal bound to other silanol groups of a self-assembled monolayer previously deposited on the metal. The gold modified electrode presents the voltammetric characteristic reversible signal of the redox pair Fe((III)/Fe(II), showing the maintenance of the Fe(III)/Fe(II) in the molecular arquitecture mounted on the metal surface. The modified electrode presented electrocatalytic activity for the reduction of nitrite ions and was successfully applied on a flow injection analysis system for analyses of natural waters, presenting a linear response range of 1x10-6 to 4x10-5 mol L-1 (r = 0.9995), with a detection limit of 0,53x10-6 mol L-1.