Nanocompósitos híbridos a base de silsesquioxano e nitroprussiato de cobalto e zinco: preparação, caracterização e aplicações eletroanalíticas
Carregando...
Arquivos
Data
2019-04-04
Autores
Magossi, Mariana de Souza
Título da Revista
ISSN da Revista
Título de Volume
Editor
Universidade Estadual Paulista (Unesp)
Resumo
Neste trabalho, novos nanocompósitos híbridos a base de silsesquioxano e nitroprussiato de cobalto e zinco foram preparados, seguindo dois métodos de síntese. Os materiais preparados foram caracterizados empregando diferentes técnicas: Espectroscopia na Região do Infravermelho por transformada de Fourier (FTIR), Espectroscopia Raman, Espectroscopia de Reflectância Difusa UV/Vis, Ressonância Magnética Nuclear (RMN), Difração de Raios-X (DRX), Microscopia Eletrônica de Varredura (MEV), Espectroscopia de Energia Dispersiva de Raios-X (EDX), Microscopia Eletrônica de Transmissão (MET) e Análise Termogravimétrica (TGA). Após a obtenção dos nanocompósitos com complexos metálicos de nitroprussiato (ACCoN e ACZnN), realizou-se um estudo sistemático sobre o comportamento voltamétrico desses materiais, empregando técnicas eletroquímicas, tais como: Voltametria Cíclica (VC) e Voltametria de Pulso Diferencial (VPD), utilizando eletrodos de pasta de grafite. O eletrodo de pasta de grafite contendo ACCoN mostrou-se sensível a concentrações de hidrazina e isoniazida. Já o eletrodo de pasta de grafite contendo ACZnN foi aplicado na detecção de N-acetilcisteína e isoniazida com sucesso. Após os testes de eletro-oxidação catalítica dessas substâncias, realizou-se uma investigação da influência dos principais interferentes, de forma que a interferência observada não se mostrou significativa. Avaliou-se também a recuperação destas substâncias a partir de amostras de água da torneira e urina sintética. Desta maneira, os nanocompósitos híbridos bimetálicos formados (ACCoN e ACZnN) são potenciais candidatos para a construção de sensores eletroquímicos para a detecção de hidrazina, isoniazida e N-acetilcisteína. Por outro lado, as caracterizações espectroscópicas obtidas dos nanocompósitos híbridos ACCoNM e ACZnNM, preparados seguindo uma metodologia alternativa, sugerem que a interação do nitroprussiato com cobalto e zinco na estrutura do silsesquioxano se deram em menor extensão, porém, estes materiais apresentaram uma boa resposta voltamétrica, estimulando futuramente a realizar estudos complementares sobre essas propriedades eletroquímicas, visando suas aplicações na eletro-oxidação catalítica de diferentes substâncias de interesse farmacêutico, biológico e ambiental.
In this work, new nanocomposites based on silsesquioxane and cobalt and zinc nitroprusside were prepared, following two synthetic methods. The prepared materials were characterized by different techniques: Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, UV-Vis Diffuse Reflectance Spectroscopy, Nuclear Magnetic Resonance (NMR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray spectroscopy (EDX), Transmission Electron Microscopy (TEM), Thermogravimetric Analysis (TGA). After obtaining the nanocomposites with metallic nitroprusside complexes, it was carried out a systematic study on the voltammetric behavior of these materials, using electrochemical techniques, such as: Cyclic Voltametry (CV) and Differential Pulse Voltammetry (DPV), using graphite paste electrodes. The graphite paste electrode containing ACCoN was sensitive to concentrations of hydrazine and isoniazid. The graphite paste electrode containing ACZnN was applied to the detection of N-acetylcysteine and isoniazid, with success. After catalytic electrooxidation tests of these substances, it was investigated the influence of the main interferents, so that the noticed interferences were not significant. Also, it was evaluated the recovery of these substances from samples of tap water and synthetic urine. By this way, the binuclear hybrid nanocomposites formed (ACCoN and ACZnN) are potential candidates for the construction of electrochemical sensors in the hydrazine, isoniazid and N-acetylcysteine detection. On the other hand, the spectroscopic characterizations obtained from hybrid nanocomposites ACCoNM and ACZnNM, prepared following an alternative methodology, suggest that the interaction of nitroprusside with cobalt and zinc in the structure of silsesquioxane occurred to a lesser exten, however, these materials presented a good voltammetric response, stimulating in the future to carry out complementary studies on these electrochemical properties, aiming at their applications in the catalytic electro-oxidation of different substances of interest pharmaceutical, biological and environmental.
In this work, new nanocomposites based on silsesquioxane and cobalt and zinc nitroprusside were prepared, following two synthetic methods. The prepared materials were characterized by different techniques: Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, UV-Vis Diffuse Reflectance Spectroscopy, Nuclear Magnetic Resonance (NMR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray spectroscopy (EDX), Transmission Electron Microscopy (TEM), Thermogravimetric Analysis (TGA). After obtaining the nanocomposites with metallic nitroprusside complexes, it was carried out a systematic study on the voltammetric behavior of these materials, using electrochemical techniques, such as: Cyclic Voltametry (CV) and Differential Pulse Voltammetry (DPV), using graphite paste electrodes. The graphite paste electrode containing ACCoN was sensitive to concentrations of hydrazine and isoniazid. The graphite paste electrode containing ACZnN was applied to the detection of N-acetylcysteine and isoniazid, with success. After catalytic electrooxidation tests of these substances, it was investigated the influence of the main interferents, so that the noticed interferences were not significant. Also, it was evaluated the recovery of these substances from samples of tap water and synthetic urine. By this way, the binuclear hybrid nanocomposites formed (ACCoN and ACZnN) are potential candidates for the construction of electrochemical sensors in the hydrazine, isoniazid and N-acetylcysteine detection. On the other hand, the spectroscopic characterizations obtained from hybrid nanocomposites ACCoNM and ACZnNM, prepared following an alternative methodology, suggest that the interaction of nitroprusside with cobalt and zinc in the structure of silsesquioxane occurred to a lesser exten, however, these materials presented a good voltammetric response, stimulating in the future to carry out complementary studies on these electrochemical properties, aiming at their applications in the catalytic electro-oxidation of different substances of interest pharmaceutical, biological and environmental.
Descrição
Palavras-chave
Silsesquioxano, Nanocompósitos, Complexos metálicos, Voltametria, Eletro-oxidação catalítica, Silsesquioxane, Nanocomposites, Metallic complexes, Voltammetry, Catalytic electro-oxidation