Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras
Ano de defesa: | 2018 |
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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: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/14631 |
Resumo: | The involvement of organosulfur species in the aging processes of Brazilian asphalt cements was studied using analytical methodologies such as ultra high performance liquid chromatography with atmospheric pressure photoionization and detection by tandem mass spectrometry (UHPLC-APPI-MS / MS), differential pulse voltammetry (DPV) in non-aqueous medium and immobilized microparticle voltammetry (VIMP). A model group of organosulfur compounds was listed as markers to evaluate the distribution and changes occurring during the forced incidence of UV radiation and high temperatures and pressure by RTFOT / SUNTEST and RTFOT / PAV, respectively on asphalt. The ionization method (APPI) presented several advantages such as the non-use of dopant, which reduce the possibility of interference of matrice compounds like PAHs in the determination of the sulfur compounds. The method still showed an acceptable matrix effect, ranging from 70.58 to 118.18%, regarding the complexity of the asphalt matrix. Good results were obtained in the validation of the method and the lower quantification and detection limits were observed for sulfoxides and sulfones, which was explained by the different ionization mechanisms observed between classes. The electrochemical monitoring of the samples by DPV in non-aqueous medium prior to the chromatographic characterization demonstrated the necessity of cleaning the asphalt matrices for the determination of the markers compounds. The optimization results of the clean-up method demonstrated that a redissolution of the samples in acetone followed by solid phase extraction with stationary phase of aminopropyl gives good recovery results (62.07 to 114.85%). In addition, the electrochemical behavior of the solid-state organosulfur compounds allowed the evaluation of these species in the aging processes of asphaltic matrices by VIMP. The results demonstrated that in addition to oxidation, sulfur compounds, mainly thiophenes and sulfides, are involved in polymerization mechanisms during aging. The determination of organosulfur markers such as thianthrene, 4,6-dimethyl dibenzothiophene, 4-methyl dibenzothiophene, dimethyl sulfoxide and dodecyl sulfoxide by UHPLC-APPI-MS/MS in the different fractions studied corroborated with the results obtained by VIMP. This allowed the establishment of possible reactions routes for these markers during the different aging processes.The Brazilian asphalt samples also demonstrated the presence of dimethyl sulfoxide and dodecyl sulfoxide in significant contents even before submitted to the processes of forced aging. |
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2018-10-22T21:46:07Z2018-10-22T21:46:07Z2018-03-01http://repositorio.ufsm.br/handle/1/14631The involvement of organosulfur species in the aging processes of Brazilian asphalt cements was studied using analytical methodologies such as ultra high performance liquid chromatography with atmospheric pressure photoionization and detection by tandem mass spectrometry (UHPLC-APPI-MS / MS), differential pulse voltammetry (DPV) in non-aqueous medium and immobilized microparticle voltammetry (VIMP). A model group of organosulfur compounds was listed as markers to evaluate the distribution and changes occurring during the forced incidence of UV radiation and high temperatures and pressure by RTFOT / SUNTEST and RTFOT / PAV, respectively on asphalt. The ionization method (APPI) presented several advantages such as the non-use of dopant, which reduce the possibility of interference of matrice compounds like PAHs in the determination of the sulfur compounds. The method still showed an acceptable matrix effect, ranging from 70.58 to 118.18%, regarding the complexity of the asphalt matrix. Good results were obtained in the validation of the method and the lower quantification and detection limits were observed for sulfoxides and sulfones, which was explained by the different ionization mechanisms observed between classes. The electrochemical monitoring of the samples by DPV in non-aqueous medium prior to the chromatographic characterization demonstrated the necessity of cleaning the asphalt matrices for the determination of the markers compounds. The optimization results of the clean-up method demonstrated that a redissolution of the samples in acetone followed by solid phase extraction with stationary phase of aminopropyl gives good recovery results (62.07 to 114.85%). In addition, the electrochemical behavior of the solid-state organosulfur compounds allowed the evaluation of these species in the aging processes of asphaltic matrices by VIMP. The results demonstrated that in addition to oxidation, sulfur compounds, mainly thiophenes and sulfides, are involved in polymerization mechanisms during aging. The determination of organosulfur markers such as thianthrene, 4,6-dimethyl dibenzothiophene, 4-methyl dibenzothiophene, dimethyl sulfoxide and dodecyl sulfoxide by UHPLC-APPI-MS/MS in the different fractions studied corroborated with the results obtained by VIMP. This allowed the establishment of possible reactions routes for these markers during the different aging processes.The Brazilian asphalt samples also demonstrated the presence of dimethyl sulfoxide and dodecyl sulfoxide in significant contents even before submitted to the processes of forced aging.O envolvimento de espécies organosulfuradas nos processos de envelhecimento de matrizes asfálticas brasileiras foi estudado utilizando metodologias analíticas como, a cromatografia de ultra alta eficiência com fotoionização atmosférica e detecção por espectrometria de massas (UHPLC-APPI-MS/MS), voltametria de pulso diferencial (DPV) em meio não aquoso e voltametria de micropartículas imobilizadas (VIMP). Um grupo modelo de compostos organosulfurados foi elencado como marcadores para avaliar a distribuição e as mudanças ocorridas durante a incidência forçada de radiação UV e elevadas temperaturas e pressão pelos métodos RTFOT/SUNTEST e RTFOT/PAV, respectivamente no asfalto. O método de ionização (APPI) apresentou diversas vantagens como a não utilização de dopante, diminuindo a possibilidade de interferência de compostos como os HPAs na determinação dos compostos orgnaosulfurados. O método ainda demonstrou um efeito de matriz aceitável, variando de 70.58 a 118.18 %, dada a complexidade da matriz de asfalto. Foram alcançados bons resultados na validação do método e os limites de quantificação e detecção mais baixos foram observados para sulfóxidos e sulfonas, o que foi explicado pelos diferentes mecanismos de ionização observados entre as classes. O monitoramento eletroquímico das amostras por DPV em meio não aquoso previamente a caracterização cromatográfica, demonstrou a necessidade de limpeza das matrizes de asfalto para a determinação dos compostos sulfurados. Os resultados de otimização do método de clean up demonstraram que uma redissolução das amostras em acetona seguida de extração em fase sólida com fase estacionária de aminopropil proporciona bons resultados de recuperação (62.07 a 114.85 %). Ademais, o comportamento eletroquímico dos compostos organosulfurados em estado sólido permitiu a avaliação dessas espécies nos processos de envelhecimento de matrizes asfálticas por VIMP. Os resultados demonstraram que além da oxidação, os compostos sulfurados, principalmente tiofenos e sulfetos, estão envolvidos em mecanismos de polimerização durante o envelhecimento. A determinação de compostos marcadores como tiantreno, 4,6-dimetil dibenzotiofeno, 4-metil dibenzotiofeno, dimetil sulfóxido e dodecil sulfóxido por UHPLC-MS/MS nas diferentes frações estudadas corroboraram com os resultados obtidos por VIMP, o que permitiu o estabelecimento de possíveis rotas reacionais para esses marcadores durante os diferentes processos de envelhecimento. As amostras de CAP brasileiro ainda demonstraram a presença de dimetil sulfóxido e dodecil sulfóxido em teores significativos mesmo antes de submetidas aos processos de envelhecimento forçado.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade 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/openAccessAsfaltoEnvelhecimentoExtração em fase sólidaFotoionizaçãoOrganosulfuradosPolimerizaçãoPolitiofenosMicropartículas imobilizadasAsphaltAgingSolid phase extractionPhotoionizationOrganosulfur compoundsPolimarizationPolythiophenesImmobilized microparticlesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileirasDetermination of organosulfur compounds as chemical markers of aging processes in brazilian asphalt cementsinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisCarvalho, Leandro Machado dehttp://lattes.cnpq.br/6652387343920028Nascimento, Paulo Cícero dohttp://lattes.cnpq.br/7151513617218161Stülp, Simonehttp://lattes.cnpq.br/1793007242678493Coutinho, Margareth Carvalhohttp://lattes.cnpq.br/4864820308964549Pilau, Eduardo Jorgehttp://lattes.cnpq.br/0859421816184957http://lattes.cnpq.br/8988345841275985Silveira, Géssica Domingos da1006000000006009da44f2c-6556-4846-9d66-386f290b802f7a101498-3229-44b5-9a7f-b2e0bf45bc8585427cca-012d-472d-8ef0-778272202571bd0b9ea7-a89e-4396-a9d9-8040c33be38bcb360ff3-7f9f-45d6-b0d3-362654052fbfb11b45df-a35d-496c-95ab-533f642fb333reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUIMICA_2018_SILVEIRA_GESSICA.pdfTES_PPGQUIMICA_2018_SILVEIRA_GESSICA.pdfTese de Doutoradoapplication/pdf11051148http://repositorio.ufsm.br/bitstream/1/14631/1/TES_PPGQUIMICA_2018_SILVEIRA_GESSICA.pdfe2609ab92effff09119cb72a02044f49MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras |
dc.title.alternative.eng.fl_str_mv |
Determination of organosulfur compounds as chemical markers of aging processes in brazilian asphalt cements |
title |
Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras |
spellingShingle |
Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras Silveira, Géssica Domingos da Asfalto Envelhecimento Extração em fase sólida Fotoionização Organosulfurados Polimerização Politiofenos Micropartículas imobilizadas Asphalt Aging Solid phase extraction Photoionization Organosulfur compounds Polimarization Polythiophenes Immobilized microparticles CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras |
title_full |
Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras |
title_fullStr |
Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras |
title_full_unstemmed |
Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras |
title_sort |
Determinação de compostos organosulfurados como marcadores dos processos de envelhecimento em matrizes asfálticas brasileiras |
author |
Silveira, Géssica Domingos da |
author_facet |
Silveira, Géssica Domingos da |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Carvalho, Leandro Machado de |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/6652387343920028 |
dc.contributor.referee1.fl_str_mv |
Nascimento, Paulo Cícero do |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/7151513617218161 |
dc.contributor.referee2.fl_str_mv |
Stülp, Simone |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/1793007242678493 |
dc.contributor.referee3.fl_str_mv |
Coutinho, Margareth Carvalho |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/4864820308964549 |
dc.contributor.referee4.fl_str_mv |
Pilau, Eduardo Jorge |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/0859421816184957 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/8988345841275985 |
dc.contributor.author.fl_str_mv |
Silveira, Géssica Domingos da |
contributor_str_mv |
Carvalho, Leandro Machado de Nascimento, Paulo Cícero do Stülp, Simone Coutinho, Margareth Carvalho Pilau, Eduardo Jorge |
dc.subject.por.fl_str_mv |
Asfalto Envelhecimento Extração em fase sólida Fotoionização Organosulfurados Polimerização Politiofenos Micropartículas imobilizadas |
topic |
Asfalto Envelhecimento Extração em fase sólida Fotoionização Organosulfurados Polimerização Politiofenos Micropartículas imobilizadas Asphalt Aging Solid phase extraction Photoionization Organosulfur compounds Polimarization Polythiophenes Immobilized microparticles CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Asphalt Aging Solid phase extraction Photoionization Organosulfur compounds Polimarization Polythiophenes Immobilized microparticles |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The involvement of organosulfur species in the aging processes of Brazilian asphalt cements was studied using analytical methodologies such as ultra high performance liquid chromatography with atmospheric pressure photoionization and detection by tandem mass spectrometry (UHPLC-APPI-MS / MS), differential pulse voltammetry (DPV) in non-aqueous medium and immobilized microparticle voltammetry (VIMP). A model group of organosulfur compounds was listed as markers to evaluate the distribution and changes occurring during the forced incidence of UV radiation and high temperatures and pressure by RTFOT / SUNTEST and RTFOT / PAV, respectively on asphalt. The ionization method (APPI) presented several advantages such as the non-use of dopant, which reduce the possibility of interference of matrice compounds like PAHs in the determination of the sulfur compounds. The method still showed an acceptable matrix effect, ranging from 70.58 to 118.18%, regarding the complexity of the asphalt matrix. Good results were obtained in the validation of the method and the lower quantification and detection limits were observed for sulfoxides and sulfones, which was explained by the different ionization mechanisms observed between classes. The electrochemical monitoring of the samples by DPV in non-aqueous medium prior to the chromatographic characterization demonstrated the necessity of cleaning the asphalt matrices for the determination of the markers compounds. The optimization results of the clean-up method demonstrated that a redissolution of the samples in acetone followed by solid phase extraction with stationary phase of aminopropyl gives good recovery results (62.07 to 114.85%). In addition, the electrochemical behavior of the solid-state organosulfur compounds allowed the evaluation of these species in the aging processes of asphaltic matrices by VIMP. The results demonstrated that in addition to oxidation, sulfur compounds, mainly thiophenes and sulfides, are involved in polymerization mechanisms during aging. The determination of organosulfur markers such as thianthrene, 4,6-dimethyl dibenzothiophene, 4-methyl dibenzothiophene, dimethyl sulfoxide and dodecyl sulfoxide by UHPLC-APPI-MS/MS in the different fractions studied corroborated with the results obtained by VIMP. This allowed the establishment of possible reactions routes for these markers during the different aging processes.The Brazilian asphalt samples also demonstrated the presence of dimethyl sulfoxide and dodecyl sulfoxide in significant contents even before submitted to the processes of forced aging. |
publishDate |
2018 |
dc.date.accessioned.fl_str_mv |
2018-10-22T21:46:07Z |
dc.date.available.fl_str_mv |
2018-10-22T21:46:07Z |
dc.date.issued.fl_str_mv |
2018-03-01 |
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/1/14631 |
url |
http://repositorio.ufsm.br/handle/1/14631 |
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 |
9da44f2c-6556-4846-9d66-386f290b802f 7a101498-3229-44b5-9a7f-b2e0bf45bc85 85427cca-012d-472d-8ef0-778272202571 bd0b9ea7-a89e-4396-a9d9-8040c33be38b cb360ff3-7f9f-45d6-b0d3-362654052fbf b11b45df-a35d-496c-95ab-533f642fb333 |
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 |
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Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM) |
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atendimento.sib@ufsm.br||tedebc@gmail.com |
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