Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS
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/1/17652 |
Resumo: | In this work, a sample preparation method using microwave-induced combustion (MIC) using a single absorbing solution was applied for further determination of both halogens and metals in biological samples. A whole milk powder sample was used for method evaluation. Fluorine was determined by potentiometry with ion selective electrode (ISE), Cl, Br, I, Ag, Cd, Co, Pb e Sr by inductively coupled plasma mass spectrometry (ICP-MS) and Ca, K, Mg and Na by flame atomic absorption spectroscopy (F AAS). The following parameters were evaluated for MIC: sample mass, nitric acid concentration used as absorbing solution and time of reflux step. According to the results, it was possible to observe that sample masses up to 700 mg were efficiently digested by MIC using 5 mol L-1 HNO3 as absorbing solution an 5 min of reflux. For F determination by ISE, standard solutions were prepared using nitric acid, and the digests, as well standard solutions, were adjusted to pH 5 previous the determination step. For Cl, Br and I determination by ICP-MS, calibration was carried out using 10 mmol L-1 NH4OH solution. Digests were diluted and the pH was adjusted (pH 10), in order to avoid memory effects for I. Losses of I were observed when reflux step was higher than 5 min (10 and 15 min). Digested solutions obtained by using MIC can be stored up to 7 days at 4 °C since no losses of F, Cl, Br and I were observed in this period. It is important to mention that these experiments were not carried out for metals determination. The results obtained by the proposed method (MIC) were in agreement with those obtained by MIC using 25 mmol L-1 NH4OH as absorbing solution for halogens and by microwave-assisted wet digestion (MAWD) using concentrated HNO3 for metals. The accuracy was also evaluated using reference materials (NIST 8435, whole milk powder and NIST 1566a, oyster tissue) and obtained results were in agreement with the reference values. Limits of quantification (LOQs) were lower than 19.2 and 1.8 μg g-1 for halogens and metals determination, respectively. The proposed method was applied to bovine liver and crustaceans samples (Penaeus subtilis and Callichirus major). |
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2019-07-31T17:57:41Z2019-07-31T17:57:41Z2016-03-05http://repositorio.ufsm.br/handle/1/17652In this work, a sample preparation method using microwave-induced combustion (MIC) using a single absorbing solution was applied for further determination of both halogens and metals in biological samples. A whole milk powder sample was used for method evaluation. Fluorine was determined by potentiometry with ion selective electrode (ISE), Cl, Br, I, Ag, Cd, Co, Pb e Sr by inductively coupled plasma mass spectrometry (ICP-MS) and Ca, K, Mg and Na by flame atomic absorption spectroscopy (F AAS). The following parameters were evaluated for MIC: sample mass, nitric acid concentration used as absorbing solution and time of reflux step. According to the results, it was possible to observe that sample masses up to 700 mg were efficiently digested by MIC using 5 mol L-1 HNO3 as absorbing solution an 5 min of reflux. For F determination by ISE, standard solutions were prepared using nitric acid, and the digests, as well standard solutions, were adjusted to pH 5 previous the determination step. For Cl, Br and I determination by ICP-MS, calibration was carried out using 10 mmol L-1 NH4OH solution. Digests were diluted and the pH was adjusted (pH 10), in order to avoid memory effects for I. Losses of I were observed when reflux step was higher than 5 min (10 and 15 min). Digested solutions obtained by using MIC can be stored up to 7 days at 4 °C since no losses of F, Cl, Br and I were observed in this period. It is important to mention that these experiments were not carried out for metals determination. The results obtained by the proposed method (MIC) were in agreement with those obtained by MIC using 25 mmol L-1 NH4OH as absorbing solution for halogens and by microwave-assisted wet digestion (MAWD) using concentrated HNO3 for metals. The accuracy was also evaluated using reference materials (NIST 8435, whole milk powder and NIST 1566a, oyster tissue) and obtained results were in agreement with the reference values. Limits of quantification (LOQs) were lower than 19.2 and 1.8 μg g-1 for halogens and metals determination, respectively. The proposed method was applied to bovine liver and crustaceans samples (Penaeus subtilis and Callichirus major).Neste trabalho foi proposto um método de decomposição por combustão iniciada por micro-ondas (MIC), usando solução absorvedora única para a posterior determinação de metais e halogênios em materiais biológicos. Para demonstração do princípio, foram utilizadas amostras de leite em pó integral e a determinação de F foi feita por potenciometria com eletrodo íon seletivo (ISE); Cl, Br, I, Ag, Cd, Co, Pb e Sr por espectrometria de massa com plasma indutivamente acoplado (ICP-MS) e Ca, K, Mg e Na por espectrometria de absorção atômica com chama (F AAS). Para MIC, os seguintes parâmetros foram avaliados: massa de amostra, concentração de HNO3 da solução absorvedora e o tempo de refluxo empregado. Massas de amostra de até 700 mg foram decompostas por MIC, utilizando HNO3 5 mol L-1 como solução absorvedora e 5 min de refluxo. Para a determinação de F, as soluções de calibração foram preparadas em HNO3 e as amostras digeridas, assim como as soluções de calibração, foram ajustadas quanto ao pH (pH 5) previamente às medidas por ISE. A determinação de Cl, Br e I por ICP-MS foi feita empregando-se curvas de calibração preparadas em NH4OH 10 mmol L-1, sendo necessária a prévia diluição e ajuste do pH (pH 10) das amostras digeridas, para contornar efeitos de memória em meio ácido. Perdas de iodo foram observadas quando foram empregados tempos de refluxo maiores que 5 min (10 e 15 min). Após decomposição por MIC, as soluções podem ser armazenadas por até 7 dias sob refrigeração (4 °C), sem que perdas sejam observadas para F, Cl, Br e I. Cabe destacar que estes experimentos de estabilidade não foram feitos para metais. Os resultados obtidos pelo método proposto foram concordantes com os resultados obtidos por MIC usando NH4OH 25 mmol L-1 como solução absorvedora para os halogênios e com os resultados obtidos por decomposição por via úmida assistida por radiação micro-ondas (MAWD) usando HNO3 14,4 mol L-1, para metais. A exatidão foi avaliada empregando materiais de referência de leite em pó integral (NIST 8435) e tecido de ostra (NIST 1566a) e os valores encontrados foram concordantes com os valores de referência. Os limites de quantificação (LOQs) obtidos foram menores que 19,2 e 1,8 μg g-1 para os halogênios e metais, respectivamente. O método proposto foi, também, aplicado para amostras de fígado bovino e crustáceos (camarão, Penaeus subtilis, e corrupto, Callichirus major).Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade 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/openAccessQuímicaCombustãoMicroondasMetaisHalogêniosAbsorçãoQuímica analíticaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICACombustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AASinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Mortari, Sergio Robertohttp://lattes.cnpq.br/7784609477475171Mello, Paola de Azevedohttp://lattes.cnpq.br/2189500441942469http://lattes.cnpq.br/3567238209864913Doneda, Morgana100600000000600a9c2788c-7913-4d7b-92e1-3429800ac028900319df-c13b-4f5c-9c66-1acf16dc6b0ab4d0ba10-19c4-43bb-8e88-bb2ae6aa3e1ba33c2787-11dc-4032-8dda-91a38ea80867reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS |
title |
Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS |
spellingShingle |
Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS Doneda, Morgana Química Combustão Microondas Metais Halogênios Absorção Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS |
title_full |
Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS |
title_fullStr |
Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS |
title_full_unstemmed |
Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS |
title_sort |
Combustão iniciada por micro-ondas para a absorção simultânea de metais e halogênios e determinação por ICP-MS, ISE e F AAS |
author |
Doneda, Morgana |
author_facet |
Doneda, Morgana |
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 |
Mortari, Sergio Roberto |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/7784609477475171 |
dc.contributor.referee2.fl_str_mv |
Mello, Paola de Azevedo |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/2189500441942469 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3567238209864913 |
dc.contributor.author.fl_str_mv |
Doneda, Morgana |
contributor_str_mv |
Flores, Érico Marlon de Moraes Mortari, Sergio Roberto Mello, Paola de Azevedo |
dc.subject.por.fl_str_mv |
Química Combustão Microondas Metais Halogênios Absorção Química analítica |
topic |
Química Combustão Microondas Metais Halogênios Absorção 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, a sample preparation method using microwave-induced combustion (MIC) using a single absorbing solution was applied for further determination of both halogens and metals in biological samples. A whole milk powder sample was used for method evaluation. Fluorine was determined by potentiometry with ion selective electrode (ISE), Cl, Br, I, Ag, Cd, Co, Pb e Sr by inductively coupled plasma mass spectrometry (ICP-MS) and Ca, K, Mg and Na by flame atomic absorption spectroscopy (F AAS). The following parameters were evaluated for MIC: sample mass, nitric acid concentration used as absorbing solution and time of reflux step. According to the results, it was possible to observe that sample masses up to 700 mg were efficiently digested by MIC using 5 mol L-1 HNO3 as absorbing solution an 5 min of reflux. For F determination by ISE, standard solutions were prepared using nitric acid, and the digests, as well standard solutions, were adjusted to pH 5 previous the determination step. For Cl, Br and I determination by ICP-MS, calibration was carried out using 10 mmol L-1 NH4OH solution. Digests were diluted and the pH was adjusted (pH 10), in order to avoid memory effects for I. Losses of I were observed when reflux step was higher than 5 min (10 and 15 min). Digested solutions obtained by using MIC can be stored up to 7 days at 4 °C since no losses of F, Cl, Br and I were observed in this period. It is important to mention that these experiments were not carried out for metals determination. The results obtained by the proposed method (MIC) were in agreement with those obtained by MIC using 25 mmol L-1 NH4OH as absorbing solution for halogens and by microwave-assisted wet digestion (MAWD) using concentrated HNO3 for metals. The accuracy was also evaluated using reference materials (NIST 8435, whole milk powder and NIST 1566a, oyster tissue) and obtained results were in agreement with the reference values. Limits of quantification (LOQs) were lower than 19.2 and 1.8 μg g-1 for halogens and metals determination, respectively. The proposed method was applied to bovine liver and crustaceans samples (Penaeus subtilis and Callichirus major). |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-03-05 |
dc.date.accessioned.fl_str_mv |
2019-07-31T17:57:41Z |
dc.date.available.fl_str_mv |
2019-07-31T17:57:41Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
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masterThesis |
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publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/17652 |
url |
http://repositorio.ufsm.br/handle/1/17652 |
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por |
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por |
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100600000000 |
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600 |
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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 |
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