Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS
Ano de defesa: | 2016 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
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: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/17689 |
Resumo: | In this work, the following methods for yerba mate digestion/extraction for further determination of As, Cd and Pb by graphite furnace atomic absorption spectrometry (GF AAS) and/or inductively coupled plasma mass spectrometry (ICP-MS) were evaluated: i) wet digestion in open systems ii) wet digestion in closed systems iii) microwave-assisted wet digestion (MAWD) using diluted HNO3 and O2 as auxiliary reagent and iv) ultrasound-assisted extraction (UAE). For the wet digestion method using open and closed systems by conventional heating, the digestion efficiency for several sample masses and HNO3 volume were evaluated in the both systems. For methods “i” and “ii”a low digestion efficiency was observed than the open system was used allowing a high throughput and not necessary predigestion step. The GF AAS technique was used for As, Cd and Pb determination due to the low digestion efficiency of open system method and to avoid possible interferences in the determination step. For MAWD using diluted HNO3 with O2 as auxiliary reagent, several sample masses, variable amount of O2 in gaseous phase and different flow-rates during digestion process were evaluated. After the MAWD evaluation using diluted HNO3 with O2 as auxiliary reagent it was possible to use a relatively high yerba mate mass (1500 mg). For high of sample mass the digestion was not observed influences in the efficiency digestion for different amount of O2 in gaseous phase. On the other hand, it was observed an improvement in the digestion efficiency when the maximum flow-rate allowed by equipment was used. However this condition could cause problems in equipment. For the determination step by ICP-MS it was necessary an interference study due to the high carbon content in solution. For the UAE, extractant solution, sonication time, temperature and sample mass were evaluated. Regarding the recovery of As, Cd and Pb, antagonist effects were observed when sample masses higher the 1000 mg were used. The limit of quantification obtained for three methods evaluated were lower than those established in legislation. Therefore, the proposed methods were considered as feasible for yerba mate digestion/extraction for further determination of As, Cd and Pb by GF AAS and/or ICP-MS. |
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2019-08-02T18:52:51Z2019-08-02T18:52:51Z2016-08-04http://repositorio.ufsm.br/handle/1/17689In this work, the following methods for yerba mate digestion/extraction for further determination of As, Cd and Pb by graphite furnace atomic absorption spectrometry (GF AAS) and/or inductively coupled plasma mass spectrometry (ICP-MS) were evaluated: i) wet digestion in open systems ii) wet digestion in closed systems iii) microwave-assisted wet digestion (MAWD) using diluted HNO3 and O2 as auxiliary reagent and iv) ultrasound-assisted extraction (UAE). For the wet digestion method using open and closed systems by conventional heating, the digestion efficiency for several sample masses and HNO3 volume were evaluated in the both systems. For methods “i” and “ii”a low digestion efficiency was observed than the open system was used allowing a high throughput and not necessary predigestion step. The GF AAS technique was used for As, Cd and Pb determination due to the low digestion efficiency of open system method and to avoid possible interferences in the determination step. For MAWD using diluted HNO3 with O2 as auxiliary reagent, several sample masses, variable amount of O2 in gaseous phase and different flow-rates during digestion process were evaluated. After the MAWD evaluation using diluted HNO3 with O2 as auxiliary reagent it was possible to use a relatively high yerba mate mass (1500 mg). For high of sample mass the digestion was not observed influences in the efficiency digestion for different amount of O2 in gaseous phase. On the other hand, it was observed an improvement in the digestion efficiency when the maximum flow-rate allowed by equipment was used. However this condition could cause problems in equipment. For the determination step by ICP-MS it was necessary an interference study due to the high carbon content in solution. For the UAE, extractant solution, sonication time, temperature and sample mass were evaluated. Regarding the recovery of As, Cd and Pb, antagonist effects were observed when sample masses higher the 1000 mg were used. The limit of quantification obtained for three methods evaluated were lower than those established in legislation. Therefore, the proposed methods were considered as feasible for yerba mate digestion/extraction for further determination of As, Cd and Pb by GF AAS and/or ICP-MS.No presente trabalho foram avaliados os seguintes métodos de decomposição/extração de erva-mate: i) decomposição por via úmida em sistema aberto ii) decomposição por via úmida em sistema fechado, iii) decomposição assistida por radiação micro-ondas (MAWD) empregando HNO3 diluído e O2 como reagente auxiliar e iv) extração assistida por ultrassom para a posterior determinação de As, Cd e Pb por espectrometria de absorção atômica com forno de grafite (GF AAS) e/ou espectrometria de massa com plasma indutivamente acoplado (ICP-MS). No primeiro e segundo método foi avaliada a eficiência de decomposição para massas de amostra até 1000 mg e volumes de HNO3 em ambos os métodos. Os digeridos obtidos após esses estudos apresentaram baixa eficiência de decomposição e valores semelhantes entre os métodos. Assim, foi utilizado o sistema aberto, pela possibilidade de obter uma elevada frequência analítica e não apresentar uma etapa de pré-digestão. Devido a essa má eficiência de decomposição e com o intuito de evitar possíveis interferências na etapa de determinação, para este método foi utilizado a técnica de GF AAS para a determinação de As, Cd e Pb. Para o método de MAWD empregando HNO3 diluído com O2 como reagente auxiliar, foi avaliada a decomposição de diferentes massas de amostras, quantidades de O2 na fase gasosa e a influência da circulação de ar em diferentes vazões externamente aos frascos durante o processo de decomposição. Após as avaliações, foi possível utilizar HNO3 diluído com O2 como reagente auxiliar para a decomposição de massas mais elevadas de erva-mate (até 1500 mg). Foi observado que a quantidade de O2 não influenciou a eficiência de decomposição de 1500 mg de amostra. Por outro lado, a utilização da vazão de ar máxima permitida pelo equipamento, melhorou a eficiência de decomposição. Entretanto, esta condição poderia causar problemas ao equipamento optando-se, assim, pela utilização de condições mais brandas de circulação de ar. Devido à massa de amostra relativamente elevada, houve a necessidade de um estudo de interferências dos elementos C, Cl e K na etapa de determinação por ICP-MS. No método de extração assistida por ultrassom foram avaliadas a solução extratora, o tempo de extração, temperatura e a massa de amostra. A melhor solução extratora foi o HNO3, utilizando 30 min de extração. Também foi possível observar um efeito antagônico da massa de amostra com a recuperação de As, Cd e Pb. Os limites de quantificação obtidos para os métodos propostos foram da ordem de ng g-1 e menores que os valores permitidos pela legislação. Portanto, os resultados obtidos nas avaliações no presente trabalho, mostraram-se que a utilização dos métodos propostos são viáveis para a decomposição/extração de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e/ou ICP-MS.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/openAccessQuímicaErva-mateArsênioChumboCádmioQuímica analíticaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Moraes, Diogo Pompéu dehttp://lattes.cnpq.br/3777062632260326Duarte, Fábio Andreihttp://lattes.cnpq.br/3503633944419329http://lattes.cnpq.br/0617212620483345Pardinho, Renan Buque100600000000600a9c2788c-7913-4d7b-92e1-3429800ac028d95fe6ca-aa5d-4323-ba0e-ff6e1407ed3ca24788db-190b-4118-b5c6-084138df6c807b2cc41c-5584-4228-a9bf-b1eb4d91e1e4reponame: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 |
Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS |
title |
Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS |
spellingShingle |
Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS Pardinho, Renan Buque Química Erva-mate Arsênio Chumbo Cádmio Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS |
title_full |
Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS |
title_fullStr |
Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS |
title_full_unstemmed |
Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS |
title_sort |
Desenvolvimento de métodos de preparo de amostras de erva-mate para a posterior determinação de As, Cd e Pb por GF AAS e ICP-MS |
author |
Pardinho, Renan Buque |
author_facet |
Pardinho, Renan Buque |
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 |
Moraes, Diogo Pompéu de |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/3777062632260326 |
dc.contributor.referee2.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/3503633944419329 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/0617212620483345 |
dc.contributor.author.fl_str_mv |
Pardinho, Renan Buque |
contributor_str_mv |
Flores, Érico Marlon de Moraes Moraes, Diogo Pompéu de Duarte, Fábio Andrei |
dc.subject.por.fl_str_mv |
Química Erva-mate Arsênio Chumbo Cádmio Química analítica |
topic |
Química Erva-mate Arsênio Chumbo Cádmio Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, the following methods for yerba mate digestion/extraction for further determination of As, Cd and Pb by graphite furnace atomic absorption spectrometry (GF AAS) and/or inductively coupled plasma mass spectrometry (ICP-MS) were evaluated: i) wet digestion in open systems ii) wet digestion in closed systems iii) microwave-assisted wet digestion (MAWD) using diluted HNO3 and O2 as auxiliary reagent and iv) ultrasound-assisted extraction (UAE). For the wet digestion method using open and closed systems by conventional heating, the digestion efficiency for several sample masses and HNO3 volume were evaluated in the both systems. For methods “i” and “ii”a low digestion efficiency was observed than the open system was used allowing a high throughput and not necessary predigestion step. The GF AAS technique was used for As, Cd and Pb determination due to the low digestion efficiency of open system method and to avoid possible interferences in the determination step. For MAWD using diluted HNO3 with O2 as auxiliary reagent, several sample masses, variable amount of O2 in gaseous phase and different flow-rates during digestion process were evaluated. After the MAWD evaluation using diluted HNO3 with O2 as auxiliary reagent it was possible to use a relatively high yerba mate mass (1500 mg). For high of sample mass the digestion was not observed influences in the efficiency digestion for different amount of O2 in gaseous phase. On the other hand, it was observed an improvement in the digestion efficiency when the maximum flow-rate allowed by equipment was used. However this condition could cause problems in equipment. For the determination step by ICP-MS it was necessary an interference study due to the high carbon content in solution. For the UAE, extractant solution, sonication time, temperature and sample mass were evaluated. Regarding the recovery of As, Cd and Pb, antagonist effects were observed when sample masses higher the 1000 mg were used. The limit of quantification obtained for three methods evaluated were lower than those established in legislation. Therefore, the proposed methods were considered as feasible for yerba mate digestion/extraction for further determination of As, Cd and Pb by GF AAS and/or ICP-MS. |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-08-04 |
dc.date.accessioned.fl_str_mv |
2019-08-02T18:52:51Z |
dc.date.available.fl_str_mv |
2019-08-02T18:52:51Z |
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.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/17689 |
url |
http://repositorio.ufsm.br/handle/1/17689 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
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dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
eu_rights_str_mv |
openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
reponame:Biblioteca Digital de Teses e Dissertações do UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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UFSM |
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UFSM |
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Biblioteca Digital de Teses e Dissertações do UFSM |
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