Determinação de elementos traços em poli-imida de alta pureza por amostragem de sólidos e espectrometria de absorção atômica com forno de grafite

Detalhes bibliográficos
Ano de defesa: 2015
Autor(a) principal: Santos, Rafael Francisco dos lattes
Orientador(a): Flores, Érico Marlon de Moraes lattes
Banca de defesa: Moraes, Diogo Pompéu de lattes, Müller, Edson Irineu lattes
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.
id UFSM_f49020d3507a391252af8407e053fd16
oai_identifier_str oai:repositorio.ufsm.br:1/17498
network_acronym_str UFSM
network_name_str Biblioteca Digital de Teses e Dissertações do UFSM
repository_id_str
spelling 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; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/17498/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD53ORIGINALDIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdfDIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdfDissertação de Mestradoapplication/pdf3271230http://repositorio.ufsm.br/bitstream/1/17498/1/DIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf47fdb6a9459f45b7a4615e87f8f2c4ceMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/17498/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52TEXTDIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf.txtDIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf.txtExtracted texttext/plain231380http://repositorio.ufsm.br/bitstream/1/17498/4/DIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf.txt7f13ca9be97deba206b06a83c388b676MD54THUMBNAILDIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf.jpgDIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf.jpgIM Thumbnailimage/jpeg6035http://repositorio.ufsm.br/bitstream/1/17498/5/DIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf.jpg022f3080315efe92767161f286f3b7f7MD551/174982019-07-19 03:02:03.791oai:repositorio.ufsm.br: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 Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2019-07-19T06:02:03Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false
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 a9c2788c-7913-4d7b-92e1-3429800ac028
095f67f5-092e-4e39-b0d2-facdced6bdab
a24788db-190b-4118-b5c6-084138df6c80
6807df31-e8bb-413e-a246-d79076e2d085
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
instname_str Universidade Federal de Santa Maria (UFSM)
instacron_str UFSM
institution UFSM
reponame_str Biblioteca Digital de Teses e Dissertações do UFSM
collection Biblioteca Digital de Teses e Dissertações do UFSM
bitstream.url.fl_str_mv http://repositorio.ufsm.br/bitstream/1/17498/3/license.txt
http://repositorio.ufsm.br/bitstream/1/17498/1/DIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf
http://repositorio.ufsm.br/bitstream/1/17498/2/license_rdf
http://repositorio.ufsm.br/bitstream/1/17498/4/DIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf.txt
http://repositorio.ufsm.br/bitstream/1/17498/5/DIS_PPGQUIMICA_2015_SANTOS_RAFAEL.pdf.jpg
bitstream.checksum.fl_str_mv 2f0571ecee68693bd5cd3f17c1e075df
47fdb6a9459f45b7a4615e87f8f2c4ce
4460e5956bc1d1639be9ae6146a50347
7f13ca9be97deba206b06a83c388b676
022f3080315efe92767161f286f3b7f7
bitstream.checksumAlgorithm.fl_str_mv MD5
MD5
MD5
MD5
MD5
repository.name.fl_str_mv Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)
repository.mail.fl_str_mv atendimento.sib@ufsm.br||tedebc@gmail.com
_version_ 1793240048436510720