Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito

Detalhes bibliográficos
Autor(a) principal: PAULA, Nattany Tayany Gomes de
Data de Publicação: 2015
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Biblioteca Digital de Teses e Dissertações da UFRPE
Texto Completo: http://www.tede2.ufrpe.br:8080/tede2/handle/tede2/6368
Resumo: Sulfites are considered food additives that after chemical reaction releasing sulfur dioxide (SO2), sulfite ion (SO32-), or bisulfite ion (HSO3-). These additives act as antioxidants in food, in the control of bacterial growth and enzymatic and non-enzymatic browning reactions during processing and storage. Although widely used in the food industry, the use of sulfite as a preservative causes some problems, reducing the nutritional quality of foods processed and in some cases are caused adverse effects to human health. In this work it is proposed to determine sulfite in samples of processed juices and wines through an analytical flow system with biamperometric detection. The system was built employing a peristaltic pump, proportional injector, a Gas Diffusion Cell (GDC) and Reagent Generation Cell (RGC) and polyethylene tubes with an internal diameter of 0.8 mm for making the analytical path. The RGC was coupled to a potentiostat for applying current to the electrochemical generation of triiodide ions. For detection it was used a biamperometric detector, adapted to a coulometer for applying the constant potential. For the data acquisition and processing was performed using a software developed in Lab View® language. The analysis method was based on a redox reaction between the I3- ions SO32- and providing a decrease of the generated current by the pair and this decrease in the signal is proportional to the concentration of SO32- ions. After the system optimization, the proposed procedure was operated with KI concentrations of 0.25 mol L-1, HCl 1.0 mol L-1, Na2SO4 and 0.1 mol L-1, with 0.25 mA current applied in RGC and the length of the sampling loop was of 20 cm. In the proposed procedure, a linear response was obtained between 1 and 12 mg L-1 of sulfite E = - (0,2371 ± 0,0028) C + (6,7097 ± 0,0182), R = -0,9997), LD = 0,26 mg L-1 and LQ = 0,86 mg L-1, relative standard deviation less than 2% (n = 10), with sampling frequency of 40 h−1. Potential interfering studies demonstrated the selectivity of the proposed method. Addition and recovery tests with samples of juices and wines were performed to give results of recovery between 91.63 and 110.34%, demonstrating the possibility of operation of the proposed procedure in real samples.
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spelling LAVORANTE, André FernandoNASCIMENTO, Valberes Bernardo doOLIVEIRA, Severino Carlos Bezerra dePAIM, Ana Paula Silveirahttp://lattes.cnpq.br/7064933045758285PAULA, Nattany Tayany Gomes de2017-02-15T14:00:25Z2015-03-12PAULA, Nattany Tayany Gomes de. Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito. 2015. 77 f. Dissertação (Programa de Pós-Graduação em Química) - Universidade Federal Rural de Pernambuco, Recife.http://www.tede2.ufrpe.br:8080/tede2/handle/tede2/6368Sulfites are considered food additives that after chemical reaction releasing sulfur dioxide (SO2), sulfite ion (SO32-), or bisulfite ion (HSO3-). These additives act as antioxidants in food, in the control of bacterial growth and enzymatic and non-enzymatic browning reactions during processing and storage. Although widely used in the food industry, the use of sulfite as a preservative causes some problems, reducing the nutritional quality of foods processed and in some cases are caused adverse effects to human health. In this work it is proposed to determine sulfite in samples of processed juices and wines through an analytical flow system with biamperometric detection. The system was built employing a peristaltic pump, proportional injector, a Gas Diffusion Cell (GDC) and Reagent Generation Cell (RGC) and polyethylene tubes with an internal diameter of 0.8 mm for making the analytical path. The RGC was coupled to a potentiostat for applying current to the electrochemical generation of triiodide ions. For detection it was used a biamperometric detector, adapted to a coulometer for applying the constant potential. For the data acquisition and processing was performed using a software developed in Lab View® language. The analysis method was based on a redox reaction between the I3- ions SO32- and providing a decrease of the generated current by the pair and this decrease in the signal is proportional to the concentration of SO32- ions. After the system optimization, the proposed procedure was operated with KI concentrations of 0.25 mol L-1, HCl 1.0 mol L-1, Na2SO4 and 0.1 mol L-1, with 0.25 mA current applied in RGC and the length of the sampling loop was of 20 cm. In the proposed procedure, a linear response was obtained between 1 and 12 mg L-1 of sulfite E = - (0,2371 ± 0,0028) C + (6,7097 ± 0,0182), R = -0,9997), LD = 0,26 mg L-1 and LQ = 0,86 mg L-1, relative standard deviation less than 2% (n = 10), with sampling frequency of 40 h−1. Potential interfering studies demonstrated the selectivity of the proposed method. Addition and recovery tests with samples of juices and wines were performed to give results of recovery between 91.63 and 110.34%, demonstrating the possibility of operation of the proposed procedure in real samples.Os agentes sulfitantes ou sulfitos são considerados aditivos alimentares que, após reação química, liberam dióxido de enxofre (SO2), íon sulfito (SO32-) ou íon bissulfito (HSO3-). Estes aditivos são agentes multifuncionais e atuam como antioxidantes em alimentos, no controle do crescimento bacteriano e de reações (enzimáticas e não enzimáticas) de escurecimento durante o processamento e estocagem. Mesmo sendo muito utilizado na indústria de alimentos, o emprego de sulfitos como conservantes provoca alguns problemas, reduzindo a qualidade nutricional dos alimentos tratados e em alguns casos são provocados efeitos adversos à saúde humana. Neste trabalho propõe-se determinar sulfitos em amostras de sucos industrializados e vinhos empregando um sistema de análise em fluxo com detecção biamperométrica. O sistema foi construído empregando-se uma Bomba Peristáltica, um Injetor Proporcional, uma Câmara de Difusão Gasosa (CDG) e uma Câmara de Geração de Reagente (CGR). A CGR foi acoplada a um potenciostato para a aplicação de corrente necessária para a geração eletroquímica de íons triiodeto. Para detecção foi utilizado um detector biamperométrico. Para o tratamento e aquisição de dados, foi utilizado um software desenvolvido em linguagem Lab View®. A metodologia de análise foi baseada em uma reação de oxirredução entre os íons SO32- e I3-, que proporciona uma diminuição da corrente biamperométrica gerada pelo par redox I3-/I-, sendo essa diminuição de corrente proporcional a concentração de íons SO32-. Após a otimização do procedimento proposto obteve-se as melhores condições: 0,25 mol L-1 de KI, 1,0 mol L-1 de HCl, 0,1 mol L-1 de Na2SO4, corrente de 0,25 mA aplicada na CGR e volume de amostra de 100 μL. Nestas condições, obteve-se uma resposta linear entre 1 e 12 mg L-1 de sulfito (I = - (0,2371 ± 0,0028) C + (6,7097 ± 0,0182), R = -0,9997), LD = 0,26 mg L-1 e LQ = 0,86 mg L-1, desvio padrão relativo menor que 2% (n = 10), com frequência de amostragem de 40 determinações por hora. Estudos de potenciais interferentes demonstraram a seletividade do método proposto. Testes de adição e recuperação com amostras de sucos e vinhos foram realizados, obtendo-se resultados de recuperação entre 91,63 e 110,34%, demonstrando a possibilidade de operação do procedimento proposto em amostras reais.Submitted by (lucia.rodrigues@ufrpe.br) on 2017-02-15T14:00:25Z No. of bitstreams: 1 Nattany Tayany Gomes de Paula.pdf: 885461 bytes, checksum: 787ab63496a1306c113ee5c12e2dac92 (MD5)Made available in DSpace on 2017-02-15T14:00:25Z (GMT). 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dc.title.por.fl_str_mv Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito
title Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito
spellingShingle Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito
PAULA, Nattany Tayany Gomes de
Agentes sulfitantes
Sulfito
Análise por injeção em fluxo
Difusão gasosa
Biamperometria
Química
Sulfite
Flow injection analysis
Gas diffusion
Biamperometry
CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito
title_full Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito
title_fullStr Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito
title_full_unstemmed Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito
title_sort Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito
author PAULA, Nattany Tayany Gomes de
author_facet PAULA, Nattany Tayany Gomes de
author_role author
dc.contributor.advisor1.fl_str_mv LAVORANTE, André Fernando
dc.contributor.advisor-co1.fl_str_mv NASCIMENTO, Valberes Bernardo do
dc.contributor.referee1.fl_str_mv OLIVEIRA, Severino Carlos Bezerra de
dc.contributor.referee2.fl_str_mv PAIM, Ana Paula Silveira
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/7064933045758285
dc.contributor.author.fl_str_mv PAULA, Nattany Tayany Gomes de
contributor_str_mv LAVORANTE, André Fernando
NASCIMENTO, Valberes Bernardo do
OLIVEIRA, Severino Carlos Bezerra de
PAIM, Ana Paula Silveira
dc.subject.por.fl_str_mv Agentes sulfitantes
Sulfito
Análise por injeção em fluxo
Difusão gasosa
Biamperometria
Química
topic Agentes sulfitantes
Sulfito
Análise por injeção em fluxo
Difusão gasosa
Biamperometria
Química
Sulfite
Flow injection analysis
Gas diffusion
Biamperometry
CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Sulfite
Flow injection analysis
Gas diffusion
Biamperometry
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::QUIMICA
description Sulfites are considered food additives that after chemical reaction releasing sulfur dioxide (SO2), sulfite ion (SO32-), or bisulfite ion (HSO3-). These additives act as antioxidants in food, in the control of bacterial growth and enzymatic and non-enzymatic browning reactions during processing and storage. Although widely used in the food industry, the use of sulfite as a preservative causes some problems, reducing the nutritional quality of foods processed and in some cases are caused adverse effects to human health. In this work it is proposed to determine sulfite in samples of processed juices and wines through an analytical flow system with biamperometric detection. The system was built employing a peristaltic pump, proportional injector, a Gas Diffusion Cell (GDC) and Reagent Generation Cell (RGC) and polyethylene tubes with an internal diameter of 0.8 mm for making the analytical path. The RGC was coupled to a potentiostat for applying current to the electrochemical generation of triiodide ions. For detection it was used a biamperometric detector, adapted to a coulometer for applying the constant potential. For the data acquisition and processing was performed using a software developed in Lab View® language. The analysis method was based on a redox reaction between the I3- ions SO32- and providing a decrease of the generated current by the pair and this decrease in the signal is proportional to the concentration of SO32- ions. After the system optimization, the proposed procedure was operated with KI concentrations of 0.25 mol L-1, HCl 1.0 mol L-1, Na2SO4 and 0.1 mol L-1, with 0.25 mA current applied in RGC and the length of the sampling loop was of 20 cm. In the proposed procedure, a linear response was obtained between 1 and 12 mg L-1 of sulfite E = - (0,2371 ± 0,0028) C + (6,7097 ± 0,0182), R = -0,9997), LD = 0,26 mg L-1 and LQ = 0,86 mg L-1, relative standard deviation less than 2% (n = 10), with sampling frequency of 40 h−1. Potential interfering studies demonstrated the selectivity of the proposed method. Addition and recovery tests with samples of juices and wines were performed to give results of recovery between 91.63 and 110.34%, demonstrating the possibility of operation of the proposed procedure in real samples.
publishDate 2015
dc.date.issued.fl_str_mv 2015-03-12
dc.date.accessioned.fl_str_mv 2017-02-15T14:00:25Z
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 PAULA, Nattany Tayany Gomes de. Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito. 2015. 77 f. Dissertação (Programa de Pós-Graduação em Química) - Universidade Federal Rural de Pernambuco, Recife.
dc.identifier.uri.fl_str_mv http://www.tede2.ufrpe.br:8080/tede2/handle/tede2/6368
identifier_str_mv PAULA, Nattany Tayany Gomes de. Sistema de análise em fluxo empregando geração eletroquímica de reagente e detecção biamperométrica para a determinação de sulfito. 2015. 77 f. Dissertação (Programa de Pós-Graduação em Química) - Universidade Federal Rural de Pernambuco, Recife.
url http://www.tede2.ufrpe.br:8080/tede2/handle/tede2/6368
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dc.publisher.program.fl_str_mv Programa de Pós-Graduação em Química
dc.publisher.initials.fl_str_mv UFRPE
dc.publisher.country.fl_str_mv Brasil
dc.publisher.department.fl_str_mv Departamento de Química
publisher.none.fl_str_mv Universidade Federal Rural de Pernambuco
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