Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite
Ano de defesa: | 2015 |
---|---|
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/1/17498 |
Resumo: | Polyimides are widely used in the industry for manufacture of crystal liquid displays, dielectric materials, and also for, aerospace applications, among others. Due to the several possibilities of application of polyimide, the quality control of this material is extremely important, making necessary the development of new methods for impurities determination. As well as for other polymers, the presence of trace amounts of metals may catalyze auto-oxidation reactions, affecting the characteristics of polymeric material. In this work it was proposed the use of solid sampling graphite furnace atomic absorption spectrometry for the determination of Cr, Cu, Mn, Na and Ni in polyimide. Pyrolysis and atomization curves were optimized using polyimide sample (BTDA-TDI/MDI) as well as reference solution. After this evaluation, the heating program for each analyte was stablished. Aqueous reference solutions were used for instrument calibration. A background correction system based on Zeeman effect was used.The linearity of calibration curves was higher than 0.99 and limits of detection were about ng g-1. For results comparison, polyimide (BTDA-TDI/MDI) was digested by dry ashing in a muffle furnace, microwave induced combustion (MIC) and by wet digestion using a single reaction chamber (SRC). Analytes determination in digests was performed by inductively coupled plasma optical emission spectrometry (ICP-OES). Results obtained for SS-GF AAS were compared with those obtained by ICP-OES after digestion by muffle furnace, MIC and SRC. No significant difference was found for Cr, Mn and Ni when compared to SRC, MIC and SS-GF AAS, while using muffle furnace the results were lower than limit of quantification. For SRC and MIC methods, the concentration of Cu and Na was lower than limit of detection impairing the comparison with SS-GF AAS. |
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2019-07-18T21:13:47Z2019-07-18T21:13:47Z2015-07-20http://repositorio.ufsm.br/handle/1/17498Polyimides are widely used in the industry for manufacture of crystal liquid displays, dielectric materials, and also for, aerospace applications, among others. Due to the several possibilities of application of polyimide, the quality control of this material is extremely important, making necessary the development of new methods for impurities determination. As well as for other polymers, the presence of trace amounts of metals may catalyze auto-oxidation reactions, affecting the characteristics of polymeric material. In this work it was proposed the use of solid sampling graphite furnace atomic absorption spectrometry for the determination of Cr, Cu, Mn, Na and Ni in polyimide. Pyrolysis and atomization curves were optimized using polyimide sample (BTDA-TDI/MDI) as well as reference solution. After this evaluation, the heating program for each analyte was stablished. Aqueous reference solutions were used for instrument calibration. A background correction system based on Zeeman effect was used.The linearity of calibration curves was higher than 0.99 and limits of detection were about ng g-1. For results comparison, polyimide (BTDA-TDI/MDI) was digested by dry ashing in a muffle furnace, microwave induced combustion (MIC) and by wet digestion using a single reaction chamber (SRC). Analytes determination in digests was performed by inductively coupled plasma optical emission spectrometry (ICP-OES). Results obtained for SS-GF AAS were compared with those obtained by ICP-OES after digestion by muffle furnace, MIC and SRC. No significant difference was found for Cr, Mn and Ni when compared to SRC, MIC and SS-GF AAS, while using muffle furnace the results were lower than limit of quantification. For SRC and MIC methods, the concentration of Cu and Na was lower than limit of detection impairing the comparison with SS-GF AAS.As poli-imidas são amplamente empregadas na indústria para a fabricação de telas de cristal líquido, materiais dielétricos e, também, para aplicações aeroespaciais, dentre outros usos. Devido às diversas possibilidades de aplicação e à necessidade de um rígido controle de qualidade, o desenvolvimento de métodos analíticos adequados para tal controle tornam-se importantes. Assim como para outros polímeros, a presença de impurezas elementares em níveis traço pode catalisar reações de auto-oxidação, levando à degradação e afetando diretamente as características do material polimérico. Neste sentido, este trabalho propõe um procedimento para análise direta por espectrometria de absorção atômica com forno de grafite (SS-GF AAS) para a determinação de Cr, Cu, Mn, Na e Ni em poli-imida. Foram avaliadas as curvas de pirólise e atomização empregando o sistema SS-GF AAS para as amostras de poli-imida (BTDA-TDI/MDI) e para as soluções de referência. A partir destas curvas, foram estabelecidas as temperaturas adequadas para o programa de aquecimento. A calibração foi feita empregando soluções de referência aquosas e, como corretor de fundo, foi utilizado o sistema baseado no efeito Zeeman. Para as curvas de calibração, foram obtidos coeficientes de correlação linear maiores que 0,99 e limites de quantificação da ordem de ng g-1. Para comparação dos resultados, a amostra de poli-imida (BTDA-TDI/MDI) foi decomposta por via seca em forno tipo mufla, combustão iniciada por micro-ondas (MIC) e por digestão ácida em sistema com câmara única de reação (SRC). A determinação dos analitos foi feita por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP-OES). Os resultados obtidos por SS-GF AAS foram comparados com aqueles obtidos por ICP-OES após a decomposição por mufla, SRC e MIC. Não houve diferença significativa para Cr, Mn e Ni entre os métodos de SRC, MIC e SS-GF AAS, enquanto que os resultados obtidos para os digeridos por mufla foram inferiores ao limite de quantificação (LQ). Para SRC e MIC, os resultados para Cu e Na foram inferiores ao LQ, impossibilitando a comparação com o procedimento proposto por SS-GF AAS.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/openAccessQuímicaQuímica analíticaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafiteinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Moraes, Diogo Pompéu dehttp://lattes.cnpq.br/3777062632260326Müller, Edson Irineuhttp://lattes.cnpq.br/5994311290376153http://lattes.cnpq.br/1622139696944992Santos, Rafael Francisco dos100600000000600a9c2788c-7913-4d7b-92e1-3429800ac028095f67f5-092e-4e39-b0d2-facdced6bdaba24788db-190b-4118-b5c6-084138df6c806807df31-e8bb-413e-a246-d79076e2d085reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMLICENSElicense.txtlicense.txttext/plain; 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dc.title.por.fl_str_mv |
Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite |
title |
Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite |
spellingShingle |
Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite Santos, Rafael Francisco dos Química Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite |
title_full |
Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite |
title_fullStr |
Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite |
title_full_unstemmed |
Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite |
title_sort |
Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite |
author |
Santos, Rafael Francisco dos |
author_facet |
Santos, Rafael Francisco dos |
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 |
Müller, Edson Irineu |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/5994311290376153 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/1622139696944992 |
dc.contributor.author.fl_str_mv |
Santos, Rafael Francisco dos |
contributor_str_mv |
Flores, Érico Marlon de Moraes Moraes, Diogo Pompéu de Müller, Edson Irineu |
dc.subject.por.fl_str_mv |
Química Química analítica |
topic |
Química Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Polyimides are widely used in the industry for manufacture of crystal liquid displays, dielectric materials, and also for, aerospace applications, among others. Due to the several possibilities of application of polyimide, the quality control of this material is extremely important, making necessary the development of new methods for impurities determination. As well as for other polymers, the presence of trace amounts of metals may catalyze auto-oxidation reactions, affecting the characteristics of polymeric material. In this work it was proposed the use of solid sampling graphite furnace atomic absorption spectrometry for the determination of Cr, Cu, Mn, Na and Ni in polyimide. Pyrolysis and atomization curves were optimized using polyimide sample (BTDA-TDI/MDI) as well as reference solution. After this evaluation, the heating program for each analyte was stablished. Aqueous reference solutions were used for instrument calibration. A background correction system based on Zeeman effect was used.The linearity of calibration curves was higher than 0.99 and limits of detection were about ng g-1. For results comparison, polyimide (BTDA-TDI/MDI) was digested by dry ashing in a muffle furnace, microwave induced combustion (MIC) and by wet digestion using a single reaction chamber (SRC). Analytes determination in digests was performed by inductively coupled plasma optical emission spectrometry (ICP-OES). Results obtained for SS-GF AAS were compared with those obtained by ICP-OES after digestion by muffle furnace, MIC and SRC. No significant difference was found for Cr, Mn and Ni when compared to SRC, MIC and SS-GF AAS, while using muffle furnace the results were lower than limit of quantification. For SRC and MIC methods, the concentration of Cu and Na was lower than limit of detection impairing the comparison with SS-GF AAS. |
publishDate |
2015 |
dc.date.issued.fl_str_mv |
2015-07-20 |
dc.date.accessioned.fl_str_mv |
2019-07-18T21:13:47Z |
dc.date.available.fl_str_mv |
2019-07-18T21:13:47Z |
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/1/17498 |
url |
http://repositorio.ufsm.br/handle/1/17498 |
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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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
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Biblioteca Digital de Teses e Dissertações do UFSM |
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