Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas
Ano de defesa: | 2017 |
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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/1/17977 |
Resumo: | A new method for analytical applications based on Maxwell-Wagner effect with to use of microwave radiation in closed system is proposed. Considering the interaction of carbonaceous materials with an oscillating electromagnetic field in the microwave frequency range, a very fast heating is observed due to interfacial polarization that results in localized microplasma formation. Such effect was evaluated in a monomode microwave system and temperature was recorded using an infrared camera. For analytical applications, a closed reactor under oxygen pressure was evaluated for carbonaceous materials digestion. The combination of high temperature and oxidant atmosphere resulted in a very effective self-ignition reaction of sample, allowing its use as sample preparation procedure for further elemental analysis. In order to assure the feasibility of the proposed microwave-assisted self-ignition procedure, several parameters were evaluated using graphite sample, including the interaction of microwaves with the sample in pellet form or powder, in both open system at atmospheric pressure and into closed system under oxygen pressure (20 bar), and the maximum sample mass able to be completely digested. The rare earth elements (Ce, Dy, Er, Eu, Gd, Ho, La, Lu, Nd, Pr, Sm, Tb, Tm, Y and Yb) were determined by inductively coupled plasma optical emission spectrometry using ultrasonic nebulizer. After optimization, a sample mass of 400 mg was efficiently digested (residual carbon content lower than 1%) in a closed system using 4 mol L-1 HNO3 as absorbing solution. The accuracy of the proposed procedure was checked by neutron activation analysis and an agREEment better than 95% was achieved in comparison to microwave induced self-ignition results. Additionally, in this study a microwave-assisted extraction and dry ashing methods were performed and an agREEment better than 95 % (p>0.05) was obtained in both methods. The limits of quantification were in the range from 5 up to 70 ng g-1. Finally, the proposed procedure allows to use of high sample mass (400 mg) without to use of auxiliary reagent and also diluted absorbing solution. |
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2019-08-20T20:57:54Z2019-08-20T20:57:54Z2017-06-03http://repositorio.ufsm.br/handle/1/17977A new method for analytical applications based on Maxwell-Wagner effect with to use of microwave radiation in closed system is proposed. Considering the interaction of carbonaceous materials with an oscillating electromagnetic field in the microwave frequency range, a very fast heating is observed due to interfacial polarization that results in localized microplasma formation. Such effect was evaluated in a monomode microwave system and temperature was recorded using an infrared camera. For analytical applications, a closed reactor under oxygen pressure was evaluated for carbonaceous materials digestion. The combination of high temperature and oxidant atmosphere resulted in a very effective self-ignition reaction of sample, allowing its use as sample preparation procedure for further elemental analysis. In order to assure the feasibility of the proposed microwave-assisted self-ignition procedure, several parameters were evaluated using graphite sample, including the interaction of microwaves with the sample in pellet form or powder, in both open system at atmospheric pressure and into closed system under oxygen pressure (20 bar), and the maximum sample mass able to be completely digested. The rare earth elements (Ce, Dy, Er, Eu, Gd, Ho, La, Lu, Nd, Pr, Sm, Tb, Tm, Y and Yb) were determined by inductively coupled plasma optical emission spectrometry using ultrasonic nebulizer. After optimization, a sample mass of 400 mg was efficiently digested (residual carbon content lower than 1%) in a closed system using 4 mol L-1 HNO3 as absorbing solution. The accuracy of the proposed procedure was checked by neutron activation analysis and an agREEment better than 95% was achieved in comparison to microwave induced self-ignition results. Additionally, in this study a microwave-assisted extraction and dry ashing methods were performed and an agREEment better than 95 % (p>0.05) was obtained in both methods. The limits of quantification were in the range from 5 up to 70 ng g-1. Finally, the proposed procedure allows to use of high sample mass (400 mg) without to use of auxiliary reagent and also diluted absorbing solution.Neste trabalho é proposto um novo método de preparo de amostra baseado no efeito Maxwell-Wagner com o uso da radiação micro-ondas em sistema fechado. Esse efeito ocorre devido à interação dos materiais carbonáceos com um campo eletromagnético oscilante, na frequência das micro-ondas. Devido à essa interação um rápido aquecimento do material é observado como resultado da formação de microplasmas em pontos localizados. Inicialmente, este efeito foi avaliado em um sistema de micro-ondas monomodo (sistema aberto) para a autoignição da grafite e o monitoramento da temperatura foi feito utilizando uma câmera de infravermelho. Os seguintes parâmetros foram avaliados: grafite na forma de pó ou comprimido, tamanho de partícula, porosidade e área superficial. Posteriormente, a autoignição da grafite foi avaliada em um sistema fechado sob pressão de oxigênio, visando a aplicação analítica como método de preparo de amostra. Os elementos terras raras, REE (Ce, Dy, Er, Eu, Gd, Ho, La, Lu, Nd, Pr, Sm, Tb, Tm, Y e Yb) foram determinados por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP-OES) utilizando um sistema de nebulização ultrassônica (USN). Para isso, os parâmetros operacionais da técnica de USN-ICP-OES também foram avaliados, como a vazão do gás de nebulização, potência do gerador de radiofrequência do plasma, vazão da bomba peristáltica. Além da temperatura de aquecimento e resfriamento do sistema de nebulização ultrassônico. Após as otimizações, foram digeridos eficientemente 400 mg da grafite, com teor de carbono residual menor que 1%. Outra vantagem refere-se ao uso da solução absorvedora diluída, visto que foi utilizado HNO3 3 mol L-1 para absorção dos REE. A exatidão foi avaliada pela comparação dos resultados obtidos pelo emprego do método proposto com aqueles obtidos por análise por ativação neutrônica, os quais apresentaram concordâncias superiores a 95% para todos os REE. Além disso, quando os resultados foram comparados com os obtidos pelos métodos de extração assistida por micro-ondas e combustão por via seca, não houve diferença significativa (p>0,05) para todos os REE. Os limites de quantificação foram na faixa de 5 a 70 ng g-1. O método proposto permitiu a digestão de elevada massa de amostra (400 mg), sem o uso de reagentes auxiliares, e com o uso de solução absorvedora diluída.porUniversidade 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/openAccessQuímicaAmostragemGrafiteMicroondasQuímica analíticaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricasinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Costa, Adilson Ben dahttp://lattes.cnpq.br/2604778196819181Duarte, Fábio Andreihttp://lattes.cnpq.br/3503633944419329Barin, Juliano Smaniotohttp://lattes.cnpq.br/7545847424095994Rodrigues, Luiz Fredericohttp://lattes.cnpq.br/9354290360702855http://lattes.cnpq.br/7657499830389187Cruz, Sandra Meinen da100600000000600a9c2788c-7913-4d7b-92e1-3429800ac02822d759b6-6653-4428-8db7-a342f8e779e08fd7d402-38cb-487a-ae04-60b751dc48d67b2cc41c-5584-4228-a9bf-b1eb4d91e1e461d23861-d241-4d88-80dc-1de363d97bcfcfa9ea52-18b4-42b0-8233-4f4ebcf879fareponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUIMICA_2017_CRUZ_SANDRA.pdfTES_PPGQUIMICA_2017_CRUZ_SANDRA.pdfTese de Doutoradoapplication/pdf2725189http://repositorio.ufsm.br/bitstream/1/17977/1/TES_PPGQUIMICA_2017_CRUZ_SANDRA.pdf06f6f26b240b3315b5ed0d534e319558MD51LICENSElicense.txtlicense.txttext/plain; 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dc.title.por.fl_str_mv |
Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas |
title |
Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas |
spellingShingle |
Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas Cruz, Sandra Meinen da Química Amostragem Grafite Microondas Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas |
title_full |
Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas |
title_fullStr |
Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas |
title_full_unstemmed |
Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas |
title_sort |
Desenvolvimento de método de preparo de amostras baseado no efeito Maxwell-Wagner e determinação de elementos terras raras por técnicas espectrométricas |
author |
Cruz, Sandra Meinen da |
author_facet |
Cruz, Sandra Meinen da |
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 |
Costa, Adilson Ben da |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/2604778196819181 |
dc.contributor.referee2.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/3503633944419329 |
dc.contributor.referee3.fl_str_mv |
Barin, Juliano Smanioto |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/7545847424095994 |
dc.contributor.referee4.fl_str_mv |
Rodrigues, Luiz Frederico |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/9354290360702855 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/7657499830389187 |
dc.contributor.author.fl_str_mv |
Cruz, Sandra Meinen da |
contributor_str_mv |
Flores, Érico Marlon de Moraes Costa, Adilson Ben da Duarte, Fábio Andrei Barin, Juliano Smanioto Rodrigues, Luiz Frederico |
dc.subject.por.fl_str_mv |
Química Amostragem Grafite Microondas Química analítica |
topic |
Química Amostragem Grafite Microondas Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
A new method for analytical applications based on Maxwell-Wagner effect with to use of microwave radiation in closed system is proposed. Considering the interaction of carbonaceous materials with an oscillating electromagnetic field in the microwave frequency range, a very fast heating is observed due to interfacial polarization that results in localized microplasma formation. Such effect was evaluated in a monomode microwave system and temperature was recorded using an infrared camera. For analytical applications, a closed reactor under oxygen pressure was evaluated for carbonaceous materials digestion. The combination of high temperature and oxidant atmosphere resulted in a very effective self-ignition reaction of sample, allowing its use as sample preparation procedure for further elemental analysis. In order to assure the feasibility of the proposed microwave-assisted self-ignition procedure, several parameters were evaluated using graphite sample, including the interaction of microwaves with the sample in pellet form or powder, in both open system at atmospheric pressure and into closed system under oxygen pressure (20 bar), and the maximum sample mass able to be completely digested. The rare earth elements (Ce, Dy, Er, Eu, Gd, Ho, La, Lu, Nd, Pr, Sm, Tb, Tm, Y and Yb) were determined by inductively coupled plasma optical emission spectrometry using ultrasonic nebulizer. After optimization, a sample mass of 400 mg was efficiently digested (residual carbon content lower than 1%) in a closed system using 4 mol L-1 HNO3 as absorbing solution. The accuracy of the proposed procedure was checked by neutron activation analysis and an agREEment better than 95% was achieved in comparison to microwave induced self-ignition results. Additionally, in this study a microwave-assisted extraction and dry ashing methods were performed and an agREEment better than 95 % (p>0.05) was obtained in both methods. The limits of quantification were in the range from 5 up to 70 ng g-1. Finally, the proposed procedure allows to use of high sample mass (400 mg) without to use of auxiliary reagent and also diluted absorbing solution. |
publishDate |
2017 |
dc.date.issued.fl_str_mv |
2017-06-03 |
dc.date.accessioned.fl_str_mv |
2019-08-20T20:57:54Z |
dc.date.available.fl_str_mv |
2019-08-20T20:57:54Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
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doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/17977 |
url |
http://repositorio.ufsm.br/handle/1/17977 |
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 |
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