Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado
Ano de defesa: | 2006 |
---|---|
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
|
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
BR
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/10376 |
Resumo: | A rapid digestion procedure for further determination of inorganic elements in carbon black-containing elastomers has been developed using sample combustion in closed quartz vessels with oxygen pressure. Microwave radiation was used for the ignition step. Samples containing high levels of carbon black (up to 30%) were digested using the proposed procedure: nitrile-butadiene rubber (NBR) and ethylenepropylene-diene monomer (EPDM). A quartz device was used simultaneously as a sample holder and for the protection of vessel cap. Sample was pressed as pellet and placed together a small piece of low-ash content paper in the holder. Ammonium nitrate solution (50 ml of 50% m/v) was added to the paper as aid for ignition. The influence of the absorption solution (nitric acid or water) and the necessity of an additional reflux step were evaluated. Determination of Al, Fe, Mn, Sr and Zn was performed by inductively coupled plasma optical emission spectrometry. A reference method (ASTM D 4004-064) based on conventional dry ashing followed by flame atomic absorption spectrometry determination was used for results comparison (Mn and Zn). Results were also compared to those obtained by using wet acid digestion in closed systems. As no certified reference elastomers were available analyte spikes were made for NBR and EPDM digests. Concentrated and diluted (4 mol l-1) nitric acid, with 5 min for reflux step after the combustion process, gave better recoveries for all analytes (from 97 to 101%). For Al and Mn recoveries were bellow 90% for both open and closed vessels using HNO3 and H2SO4 mixture. For dry ashing quantitative recoveries were found only for Zn (for Al recovery was 14%). Residual carbon content was bellow 0.5% for the proposed procedure. With the proposed procedure further determination of Al, Mn, Sr and Zn is feasible with only the combustion step but for Fe a reflux with diluted HNO3 was necessary. Then, using the proposed procedure complete sample digestion is obtained is less time than other procedures and no need of concentrated acids was considered necessary. |
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2017-05-152017-05-152006-07-28MORAES, Diogo Pompéu de. Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado. 2006. 85 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006.http://repositorio.ufsm.br/handle/1/10376A rapid digestion procedure for further determination of inorganic elements in carbon black-containing elastomers has been developed using sample combustion in closed quartz vessels with oxygen pressure. Microwave radiation was used for the ignition step. Samples containing high levels of carbon black (up to 30%) were digested using the proposed procedure: nitrile-butadiene rubber (NBR) and ethylenepropylene-diene monomer (EPDM). A quartz device was used simultaneously as a sample holder and for the protection of vessel cap. Sample was pressed as pellet and placed together a small piece of low-ash content paper in the holder. Ammonium nitrate solution (50 ml of 50% m/v) was added to the paper as aid for ignition. The influence of the absorption solution (nitric acid or water) and the necessity of an additional reflux step were evaluated. Determination of Al, Fe, Mn, Sr and Zn was performed by inductively coupled plasma optical emission spectrometry. A reference method (ASTM D 4004-064) based on conventional dry ashing followed by flame atomic absorption spectrometry determination was used for results comparison (Mn and Zn). Results were also compared to those obtained by using wet acid digestion in closed systems. As no certified reference elastomers were available analyte spikes were made for NBR and EPDM digests. Concentrated and diluted (4 mol l-1) nitric acid, with 5 min for reflux step after the combustion process, gave better recoveries for all analytes (from 97 to 101%). For Al and Mn recoveries were bellow 90% for both open and closed vessels using HNO3 and H2SO4 mixture. For dry ashing quantitative recoveries were found only for Zn (for Al recovery was 14%). Residual carbon content was bellow 0.5% for the proposed procedure. With the proposed procedure further determination of Al, Mn, Sr and Zn is feasible with only the combustion step but for Fe a reflux with diluted HNO3 was necessary. Then, using the proposed procedure complete sample digestion is obtained is less time than other procedures and no need of concentrated acids was considered necessary.Neste trabalho foi proposto um procedimento para a decomposição de elastômeros (Etileno-propileno-dieno monômero e borracha do tipo nitrílica) em sistema fechado por combustão iniciada por microondas. Após a decomposição das amostras foram determinados Al, Fe, Mn, Sr e Zn por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). Para Mn e Zn, a metodologia proposta foi comparada com a metodologia oficial ASTM D 4004-064 para a decomposição de elastômeros e posterior determinação por espectrometria de absorção atômica com chama (F AAS). Os resultados obtidos foram concordantes com a metodologia oficial para a determinação de Mn e Zn. Adicionalmente, ensaios de recuperação foram empregados para Al, Fe, Mn, Sr e Zn para avaliação do método proposto. Além disso, foram estudados dois tipos de solução absorvedora (H2O e HNO3 diluído e concentrado), além da variação do emprego do tempo de aquecimento com microondas (1 min ou 5 min). Entretanto, para se obter recuperações quantitativas para todos os elementos, em ambas as amostras, é necessário que se utilize HNO3 4 molar ou concentrado como solução absorvedora e uma etapa adicional de refluxo ao procedimento de combustão. Cabe destacar que outras condições podem ser utilizadas, como por exemplo, HNO3 concentrado sem a etapa adicional de refluxo, entretanto nestas condições as recuperações podem ser quantitativas para todos os elementos com exceção de ferro. Cabe salientar que, o procedimento proposto foi comparado com o procedimento da norma ASTM, onde os valores encontrados para Zn e Mn nas amostras foram concordantes pelas duas técnicas. O teor de carbono residual é baixo e comparável aos do sistema de decomposição por via seca em mufla. Desta forma é possível propor este procedimento para a decomposição de elastômeros do tipo EPDM e NBR, sendo adequado para a posterior determinação de Al, Fe, Mn, Sr e Zn.application/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaQuímicaQuímica analíticaElastômeroCombustãoDecomposiçãoMicrowave-induced combustionCarbon black-containing elastomersSample digestionTrace metals determinationICP OESCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADecomposição de elastômeros por combustão iniciada por microondas em sistema fechadoinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Dressler, Valderi Luizhttp://lattes.cnpq.br/4054740296547580Santelli, Ricardo Erthalhttp://lattes.cnpq.br/1694260923221276http://lattes.cnpq.br/3777062632260326Moraes, Diogo Pompéu de100600000000400500500500300a9c2788c-7913-4d7b-92e1-3429800ac028c1926813-0a39-4f8a-98dd-808e204f642f4b5cf48d-ff12-42fa-8bc5-88bffc1df54269b4f28e-e1ce-4dae-8e13-6acc8303c603info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIOGODEMORAES.pdfapplication/pdf1303310http://repositorio.ufsm.br/bitstream/1/10376/1/DIOGODEMORAES.pdfb7033f9313d9290138f213dd53db0943MD51TEXTDIOGODEMORAES.pdf.txtDIOGODEMORAES.pdf.txtExtracted texttext/plain168991http://repositorio.ufsm.br/bitstream/1/10376/2/DIOGODEMORAES.pdf.txtd7bd5772ea5f2b59e6d87e7abe37f5b2MD52THUMBNAILDIOGODEMORAES.pdf.jpgDIOGODEMORAES.pdf.jpgIM Thumbnailimage/jpeg5802http://repositorio.ufsm.br/bitstream/1/10376/3/DIOGODEMORAES.pdf.jpg0498f24bcfe31a5a3bda1dae66967302MD531/103762023-01-23 14:10:09.025oai:repositorio.ufsm.br:1/10376Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132023-01-23T17:10:09Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado |
title |
Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado |
spellingShingle |
Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado Moraes, Diogo Pompéu de Química Química analítica Elastômero Combustão Decomposição Microwave-induced combustion Carbon black-containing elastomers Sample digestion Trace metals determination ICP OES CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado |
title_full |
Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado |
title_fullStr |
Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado |
title_full_unstemmed |
Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado |
title_sort |
Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado |
author |
Moraes, Diogo Pompéu de |
author_facet |
Moraes, Diogo Pompéu de |
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 |
Dressler, Valderi Luiz |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/4054740296547580 |
dc.contributor.referee2.fl_str_mv |
Santelli, Ricardo Erthal |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/1694260923221276 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3777062632260326 |
dc.contributor.author.fl_str_mv |
Moraes, Diogo Pompéu de |
contributor_str_mv |
Flores, Érico Marlon de Moraes Dressler, Valderi Luiz Santelli, Ricardo Erthal |
dc.subject.por.fl_str_mv |
Química Química analítica Elastômero Combustão Decomposição |
topic |
Química Química analítica Elastômero Combustão Decomposição Microwave-induced combustion Carbon black-containing elastomers Sample digestion Trace metals determination ICP OES CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Microwave-induced combustion Carbon black-containing elastomers Sample digestion Trace metals determination ICP OES |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
A rapid digestion procedure for further determination of inorganic elements in carbon black-containing elastomers has been developed using sample combustion in closed quartz vessels with oxygen pressure. Microwave radiation was used for the ignition step. Samples containing high levels of carbon black (up to 30%) were digested using the proposed procedure: nitrile-butadiene rubber (NBR) and ethylenepropylene-diene monomer (EPDM). A quartz device was used simultaneously as a sample holder and for the protection of vessel cap. Sample was pressed as pellet and placed together a small piece of low-ash content paper in the holder. Ammonium nitrate solution (50 ml of 50% m/v) was added to the paper as aid for ignition. The influence of the absorption solution (nitric acid or water) and the necessity of an additional reflux step were evaluated. Determination of Al, Fe, Mn, Sr and Zn was performed by inductively coupled plasma optical emission spectrometry. A reference method (ASTM D 4004-064) based on conventional dry ashing followed by flame atomic absorption spectrometry determination was used for results comparison (Mn and Zn). Results were also compared to those obtained by using wet acid digestion in closed systems. As no certified reference elastomers were available analyte spikes were made for NBR and EPDM digests. Concentrated and diluted (4 mol l-1) nitric acid, with 5 min for reflux step after the combustion process, gave better recoveries for all analytes (from 97 to 101%). For Al and Mn recoveries were bellow 90% for both open and closed vessels using HNO3 and H2SO4 mixture. For dry ashing quantitative recoveries were found only for Zn (for Al recovery was 14%). Residual carbon content was bellow 0.5% for the proposed procedure. With the proposed procedure further determination of Al, Mn, Sr and Zn is feasible with only the combustion step but for Fe a reflux with diluted HNO3 was necessary. Then, using the proposed procedure complete sample digestion is obtained is less time than other procedures and no need of concentrated acids was considered necessary. |
publishDate |
2006 |
dc.date.issued.fl_str_mv |
2006-07-28 |
dc.date.accessioned.fl_str_mv |
2017-05-15 |
dc.date.available.fl_str_mv |
2017-05-15 |
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.citation.fl_str_mv |
MORAES, Diogo Pompéu de. Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado. 2006. 85 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10376 |
identifier_str_mv |
MORAES, Diogo Pompéu de. Decomposição de elastômeros por combustão iniciada por microondas em sistema fechado. 2006. 85 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006. |
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http://repositorio.ufsm.br/handle/1/10376 |
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Universidade Federal de Santa Maria |
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