Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS

Detalhes bibliográficos
Ano de defesa: 2020
Autor(a) principal: Alves, Camila Maria Aguiar da Costa lattes
Orientador(a): Flores, Érico Marlon de Moraes lattes
Banca de defesa: Silva, Jussiane Souza da, Mello, Paola de Azevedo
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
Programa de Pós-Graduação: Programa de Pós-Graduação em Química
Departamento: Química
País: Brasil
Palavras-chave em Português:
Mel
MIC
Área do conhecimento CNPq:
Link de acesso: http://repositorio.ufsm.br/handle/1/23059
Resumo: In this work, a microwave-induced combustion (MIC) method was proposed for the decomposition of honey, aiming at As, Cd, Hg and Pb determination by ICP-MS. Parameters such as sample mass (with or without the use of combustion aids), composition and concentration of the absorbing solution and microwave oven irradiation program were evaluated. Mass of 0.8 g of honey (with 0.4 g of microcrystalline cellulose and 100 μL of 6 mol L-1 NH4NO3) was decomposed by MIC, using 6 mL of 1 mol L-1 HNO3 as absorbing solution. The digests presented carbon concentration below 25 mg L-1, allowing the determination by ICP-MS free of interference caused by carbon compounds. The accuracy of the proposed method was evaluated based on recovery tests using standard addition and by comparison using microwave-assisted wet digestion with single reaction chamber (MAWD-SRC). The proposed method allowed recoveries between 99 and 104% for the studied analytes and did not show any significant difference in comparison to the results obtained by MAWD-SRC. The LOD values obtained using the optimized conditions were 1.10, 1.70, 2.90 and 4.60 ng g-1 for As, Cd, Hg and Pb, respectively. In this way, it was possible to develop a suitable method for the decomposition of honey and subsequent determination of these elements in order to meet the current legislation, using diluted reagents. The proposed method was also applied to honey samples from different geographical origins, which presented varying concentrations of analytes.
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spelling 2021-11-30T11:16:52Z2021-11-30T11:16:52Z2020-03-19http://repositorio.ufsm.br/handle/1/23059In this work, a microwave-induced combustion (MIC) method was proposed for the decomposition of honey, aiming at As, Cd, Hg and Pb determination by ICP-MS. Parameters such as sample mass (with or without the use of combustion aids), composition and concentration of the absorbing solution and microwave oven irradiation program were evaluated. Mass of 0.8 g of honey (with 0.4 g of microcrystalline cellulose and 100 μL of 6 mol L-1 NH4NO3) was decomposed by MIC, using 6 mL of 1 mol L-1 HNO3 as absorbing solution. The digests presented carbon concentration below 25 mg L-1, allowing the determination by ICP-MS free of interference caused by carbon compounds. The accuracy of the proposed method was evaluated based on recovery tests using standard addition and by comparison using microwave-assisted wet digestion with single reaction chamber (MAWD-SRC). The proposed method allowed recoveries between 99 and 104% for the studied analytes and did not show any significant difference in comparison to the results obtained by MAWD-SRC. The LOD values obtained using the optimized conditions were 1.10, 1.70, 2.90 and 4.60 ng g-1 for As, Cd, Hg and Pb, respectively. In this way, it was possible to develop a suitable method for the decomposition of honey and subsequent determination of these elements in order to meet the current legislation, using diluted reagents. The proposed method was also applied to honey samples from different geographical origins, which presented varying concentrations of analytes.Neste trabalho foi proposto um método de decomposição de mel por combustão iniciada por micro-ondas (MIC) visando à determinação de As, Cd, Hg e Pb por espectrometria de massa com plasma indutivamente acoplado (ICP-MS). Foram avaliados parâmetros como a massa de amostra (com ou sem a utilização de auxiliares de combustão), a composição e a concentração da solução absorvedora e programa de irradiação do forno de micro-ondas. Massas de até 0,8 g de mel (com a adição de 0,4 g de celulose microcristalina e 100 μL de NH4NO3 6 mol L-1) puderam ser decompostas com o método desenvolvido, utilizando apenas 6 mL de HNO3 1 mol L-1 como solução absorvedora. Os digeridos apresentaram concentração de carbono dissolvido abaixo de 25 mg L-1, possibilitando a determinação por ICP-MS livre de interferências causadas por compostos de carbono. A exatidão foi avaliada com base em ensaios de recuperação com adição de padrão e por comparação utilizando o método de decomposição por via úmida assistida por micro-ondas em câmara única de reação (MAWD-SRC). O método proposto possibilitou recuperações entre 99 e 104% para os analitos estudados e não apresentou diferença significativa em comparação com a MAWD-SRC. Os valores de LOD obtidos para as condições otimizadas foram 1,10, 1,70, 2,90 e 4,60 ng g-1 para As, Cd, Hg e Pb, respectivamente. Dessa forma, foi possível desenvolver um método adequado para a decomposição de mel e posterior determinação desses elementos de modo a atender a legislação vigente, utilizando reagentes diluídos. O método proposto foi, também, aplicado para amostras de mel de diferentes origens geográficas, as quais apresentaram concentrações variadas dos analitos.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessContaminantes inorgânicosMelPreparo de amostrasMICICP-MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MSAs, Cd, Hg and Pb determination in honey using microwave-induced combustion and ICP-MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Silva, Jussiane Souza daMello, Paola de Azevedohttp://lattes.cnpq.br/0406016065111964Alves, Camila Maria Aguiar da Costa100600000000600600600600600a9c2788c-7913-4d7b-92e1-3429800ac02872399cb3-6501-423e-bd16-2644eca6891a3af0f519-51ea-4ebd-a63d-a1560feb47f9a33c2787-11dc-4032-8dda-91a38ea80867reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS
dc.title.alternative.eng.fl_str_mv As, Cd, Hg and Pb determination in honey using microwave-induced combustion and ICP-MS
title Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS
spellingShingle Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS
Alves, Camila Maria Aguiar da Costa
Contaminantes inorgânicos
Mel
Preparo de amostras
MIC
ICP-MS
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS
title_full Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS
title_fullStr Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS
title_full_unstemmed Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS
title_sort Determinação de As, Cd, Hg E Pb em mel empregando combustão iniciada por micro-ondas e ICP-MS
author Alves, Camila Maria Aguiar da Costa
author_facet Alves, Camila Maria Aguiar da Costa
author_role author
dc.contributor.advisor1.fl_str_mv Flores, Érico Marlon de Moraes
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/7167629055579212
dc.contributor.referee1.fl_str_mv Silva, Jussiane Souza da
dc.contributor.referee2.fl_str_mv Mello, Paola de Azevedo
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/0406016065111964
dc.contributor.author.fl_str_mv Alves, Camila Maria Aguiar da Costa
contributor_str_mv Flores, Érico Marlon de Moraes
Silva, Jussiane Souza da
Mello, Paola de Azevedo
dc.subject.por.fl_str_mv Contaminantes inorgânicos
Mel
Preparo de amostras
MIC
ICP-MS
topic Contaminantes inorgânicos
Mel
Preparo de amostras
MIC
ICP-MS
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description In this work, a microwave-induced combustion (MIC) method was proposed for the decomposition of honey, aiming at As, Cd, Hg and Pb determination by ICP-MS. Parameters such as sample mass (with or without the use of combustion aids), composition and concentration of the absorbing solution and microwave oven irradiation program were evaluated. Mass of 0.8 g of honey (with 0.4 g of microcrystalline cellulose and 100 μL of 6 mol L-1 NH4NO3) was decomposed by MIC, using 6 mL of 1 mol L-1 HNO3 as absorbing solution. The digests presented carbon concentration below 25 mg L-1, allowing the determination by ICP-MS free of interference caused by carbon compounds. The accuracy of the proposed method was evaluated based on recovery tests using standard addition and by comparison using microwave-assisted wet digestion with single reaction chamber (MAWD-SRC). The proposed method allowed recoveries between 99 and 104% for the studied analytes and did not show any significant difference in comparison to the results obtained by MAWD-SRC. The LOD values obtained using the optimized conditions were 1.10, 1.70, 2.90 and 4.60 ng g-1 for As, Cd, Hg and Pb, respectively. In this way, it was possible to develop a suitable method for the decomposition of honey and subsequent determination of these elements in order to meet the current legislation, using diluted reagents. The proposed method was also applied to honey samples from different geographical origins, which presented varying concentrations of analytes.
publishDate 2020
dc.date.issued.fl_str_mv 2020-03-19
dc.date.accessioned.fl_str_mv 2021-11-30T11:16:52Z
dc.date.available.fl_str_mv 2021-11-30T11:16:52Z
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Centro de Ciências Naturais e Exatas
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dc.publisher.department.fl_str_mv Química
publisher.none.fl_str_mv Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
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