Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica
Ano de defesa: | 2016 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
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/1/17721 |
Resumo: | In this work, four sample preparation methods were evaluated for further determination of F and Cl by ion chromatography (IC) and Br and I by inductively coupled plasma mass spectrometry (ICP-MS) in soils with variable organic matter content (in the range of 8 to 96%). The following sample preparation methods were evaluated: microwave-induced combustion (MIC), quartz combustion tube followed by pyrohydrolysis (QTC-P), microwave-assisted acid wet digestion using a single reaction chamber (MAWD-SRC) and microwave-assisted extraction using a single reaction chamber (MAE-SRC). All the methods were applied for three soil groups based on the organic matter content: i organic matter content lower than 10%; ii) organic matter content about 50% and iii organic matter content higher than 95%. The results obtained after soils digestion by MIC were used as reference values for optimization of other sample preparation methods evaluated. According to the obtained results, it was possible to observe that for combustion methods (MIC and QTC- P), the use of cellulose was necessary for soils containing organic matter lower or about 50% for quantitative recoveries of F, Cl, Br and I. On the other hand, for soils containing higher organic matter content ( , the use of cellulose was not necessary and quantitative results were obtained for all the halogens for both combustion methods. Regarding to the MAWD-SRC and MAE-SRC methods, the determination of F in all groups of soils was not possible due to the interferences observed using IC. The application of MAWD-SRC method using only H2O2 as decomposition solution allowed Cl, Br and I determination in soils with high content of organic matter However, the determination of Cl was not possible for soils containing low organic content soils extraction by MAE-SRC, it was possible to observe that quantitative results were only obtained for Cl, Br and I in soil used for method optimization (organic matter higher than 95%). When MAE-SRC was applied for the extraction of other soils in the same group (group “C”), lower agreement (in the range of 70 to 80%) were obtained for analytes in comparison to those obtained by the reference method (MIC). |
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2019-08-06T21:33:49Z2019-08-06T21:33:49Z2016-08-11http://repositorio.ufsm.br/handle/1/17721In this work, four sample preparation methods were evaluated for further determination of F and Cl by ion chromatography (IC) and Br and I by inductively coupled plasma mass spectrometry (ICP-MS) in soils with variable organic matter content (in the range of 8 to 96%). The following sample preparation methods were evaluated: microwave-induced combustion (MIC), quartz combustion tube followed by pyrohydrolysis (QTC-P), microwave-assisted acid wet digestion using a single reaction chamber (MAWD-SRC) and microwave-assisted extraction using a single reaction chamber (MAE-SRC). All the methods were applied for three soil groups based on the organic matter content: i organic matter content lower than 10%; ii) organic matter content about 50% and iii organic matter content higher than 95%. The results obtained after soils digestion by MIC were used as reference values for optimization of other sample preparation methods evaluated. According to the obtained results, it was possible to observe that for combustion methods (MIC and QTC- P), the use of cellulose was necessary for soils containing organic matter lower or about 50% for quantitative recoveries of F, Cl, Br and I. On the other hand, for soils containing higher organic matter content ( , the use of cellulose was not necessary and quantitative results were obtained for all the halogens for both combustion methods. Regarding to the MAWD-SRC and MAE-SRC methods, the determination of F in all groups of soils was not possible due to the interferences observed using IC. The application of MAWD-SRC method using only H2O2 as decomposition solution allowed Cl, Br and I determination in soils with high content of organic matter However, the determination of Cl was not possible for soils containing low organic content soils extraction by MAE-SRC, it was possible to observe that quantitative results were only obtained for Cl, Br and I in soil used for method optimization (organic matter higher than 95%). When MAE-SRC was applied for the extraction of other soils in the same group (group “C”), lower agreement (in the range of 70 to 80%) were obtained for analytes in comparison to those obtained by the reference method (MIC).Neste trabalho, quatro métodos de preparo de amostra foram avaliados para a posterior determinação de F e Cl por cromatografia de íons (IC) e Br e I por espectrometria de massa com plasma indutivamente acoplado (ICP-MS) em solos contendo teores variados de matéria orgânica (entre 8 a 96%). Os seguintes métodos de preparo de amostra foram avaliados: combustão iniciada por micro-ondas (MIC), combustão em tubo de quartzo seguida por piroidrólise (QTC-P), decomposição por via úmida assistida por radiação micro-ondas em câmara única de reação (MAWD-SRC) e extração assistida por radiação micro-ondas em câmara única de reação (MAE-SRC). Os métodos de preparo foram aplicados para três grupo de solos, separados de acordo com o teor de matéria orgânica presente: i grupo A : baixo teor de matéria orgânica (inferior a 10%); ii grupo B : teor intermediário de matéria orgânica (cerca de 50%) e iii grupo C : elevado teor de matéria orgânica (superior a 95%). Os resultados obtidos após decomposição dos solos por MIC foram usados como valores de referência para a otimização dos outros métodos de preparo de amostra avaliados. De acordo com os resultados obtidos, foi possível observar que, para os métodos de combustão (MIC e QTC-P), o uso de celulose como auxiliar de combustão foi necessário para a volatilização quantitativa de F, Cl, Br e I dos solos dos . Por outro lado, para os solos contendo elevado teor de matéria orgânica ( , o uso da celulose não foi necessário e resultados quantitativos foram obtidos para os halogênios em ambos métodos de combustão. Com relação aos métodos de MAWD-SRC e MAE-SRC, a determinação de F não foi possível nos três grupos de solos devido às interferências observadas por IC. O uso da MAWD-SRC utilizando H2O2 como solução única de decomposição, possibilitou a determinação de Cl, Br e I nos solos com maior teor de matéria orgânica (grupos B e C , porém, a determinação de Cl não foi possível nos solos contendo baixo teor de matéria orgânica (grupo “A”). Após a extração dos solos por MAE-SRC, foi possível observar que resultados quantitativos para Cl, Br e I somente foram obtidos para o solo utilizado na otimização do método (teor de matéria orgânica de 95%). Quando o método de MAE-SRC foi aplicado para os outros solos contendo teor de matéria orgânica semelhante (grupo “C”), concordâncias inferiores foram obtidas (entre 70 e 80%) para os analitos quando comparado aos valores obtidos pelo método de referência (MIC).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/openAccessSolo organicoAmostragemHalogêniosCromatografiaEspectrometriaQuímicaSolosQuímica analíticaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAMétodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômicainfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Müller, Edson Irineuhttp://lattes.cnpq.br/5994311290376153Rodrigues, Luiz Fredericohttp://lattes.cnpq.br/9354290360702855Mesko, Márcia Fosterhttp://lattes.cnpq.br/2461255030745891Mello, Paola de Azevedohttp://lattes.cnpq.br/2189500441942469http://lattes.cnpq.br/0992642014615003Pereira, Letícia Severo Fagundes100600000000600a9c2788c-7913-4d7b-92e1-3429800ac028eb49db49-cf84-4947-bfcb-2f80d5d51ca948134181-e983-450f-9543-d2f1522e87a933b68b9e-17df-4982-9a2b-3ab9ad0a1e02b138c2ba-03fe-46c0-a0a8-40860f82b7142a590691-dda6-4e0c-a095-c5fdeddb22e3reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUIMICA_2016_PEREIRA_LETICIA.pdfTES_PPGQUIMICA_2016_PEREIRA_LETICIA.pdfTese de Doutoradoapplication/pdf7525241http://repositorio.ufsm.br/bitstream/1/17721/1/TES_PPGQUIMICA_2016_PEREIRA_LETICIA.pdf9157ff1a516da3550a017f75995455f2MD51LICENSElicense.txtlicense.txttext/plain; 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dc.title.por.fl_str_mv |
Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica |
title |
Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica |
spellingShingle |
Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica Pereira, Letícia Severo Fagundes Solo organico Amostragem Halogênios Cromatografia Espectrometria Química Solos Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica |
title_full |
Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica |
title_fullStr |
Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica |
title_full_unstemmed |
Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica |
title_sort |
Métodos de preparo de amostras para a posterior determinação de halogênios em solos contendo elevados e baixos teores de matéria orgânica empregando técnicas de cromatografia e de espectrometria atômica |
author |
Pereira, Letícia Severo Fagundes |
author_facet |
Pereira, Letícia Severo Fagundes |
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 |
Müller, Edson Irineu |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/5994311290376153 |
dc.contributor.referee2.fl_str_mv |
Rodrigues, Luiz Frederico |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/9354290360702855 |
dc.contributor.referee3.fl_str_mv |
Mesko, Márcia Foster |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/2461255030745891 |
dc.contributor.referee4.fl_str_mv |
Mello, Paola de Azevedo |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/2189500441942469 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/0992642014615003 |
dc.contributor.author.fl_str_mv |
Pereira, Letícia Severo Fagundes |
contributor_str_mv |
Flores, Érico Marlon de Moraes Müller, Edson Irineu Rodrigues, Luiz Frederico Mesko, Márcia Foster Mello, Paola de Azevedo |
dc.subject.por.fl_str_mv |
Solo organico Amostragem Halogênios Cromatografia Espectrometria Química Solos Química analítica |
topic |
Solo organico Amostragem Halogênios Cromatografia Espectrometria Química Solos 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, four sample preparation methods were evaluated for further determination of F and Cl by ion chromatography (IC) and Br and I by inductively coupled plasma mass spectrometry (ICP-MS) in soils with variable organic matter content (in the range of 8 to 96%). The following sample preparation methods were evaluated: microwave-induced combustion (MIC), quartz combustion tube followed by pyrohydrolysis (QTC-P), microwave-assisted acid wet digestion using a single reaction chamber (MAWD-SRC) and microwave-assisted extraction using a single reaction chamber (MAE-SRC). All the methods were applied for three soil groups based on the organic matter content: i organic matter content lower than 10%; ii) organic matter content about 50% and iii organic matter content higher than 95%. The results obtained after soils digestion by MIC were used as reference values for optimization of other sample preparation methods evaluated. According to the obtained results, it was possible to observe that for combustion methods (MIC and QTC- P), the use of cellulose was necessary for soils containing organic matter lower or about 50% for quantitative recoveries of F, Cl, Br and I. On the other hand, for soils containing higher organic matter content ( , the use of cellulose was not necessary and quantitative results were obtained for all the halogens for both combustion methods. Regarding to the MAWD-SRC and MAE-SRC methods, the determination of F in all groups of soils was not possible due to the interferences observed using IC. The application of MAWD-SRC method using only H2O2 as decomposition solution allowed Cl, Br and I determination in soils with high content of organic matter However, the determination of Cl was not possible for soils containing low organic content soils extraction by MAE-SRC, it was possible to observe that quantitative results were only obtained for Cl, Br and I in soil used for method optimization (organic matter higher than 95%). When MAE-SRC was applied for the extraction of other soils in the same group (group “C”), lower agreement (in the range of 70 to 80%) were obtained for analytes in comparison to those obtained by the reference method (MIC). |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-08-11 |
dc.date.accessioned.fl_str_mv |
2019-08-06T21:33:49Z |
dc.date.available.fl_str_mv |
2019-08-06T21:33:49Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/17721 |
url |
http://repositorio.ufsm.br/handle/1/17721 |
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:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
bitstream.url.fl_str_mv |
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bitstream.checksum.fl_str_mv |
9157ff1a516da3550a017f75995455f2 2f0571ecee68693bd5cd3f17c1e075df 4460e5956bc1d1639be9ae6146a50347 98d366fd3585614b809996699525c4fc 72408d6e3aaf75fd56164db977603d7a |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 MD5 MD5 |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
|
_version_ |
1794524431124529152 |