Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica
Ano de defesa: | 2018 |
---|---|
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: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/15930 |
Resumo: | Among the heteroatoms present in petroleum, sulfur stands out as being the most abundant. Henceforth it can be found on many quantities in oil derivate, such as Petroleum Asphalt Cement (CAP). The presence of organosulfur compounds on asphalt matrix is related to the matrix aging processes, making it brittle and reducing the useful life of the pavement. Even more some of these compounds can be used as pollution markers in environmental analysis, and geological markers. We can also tie the presence of such elements as an occupational health hazard, seeing as some of them have a known carcinogenic and mutagenic potential. In face of that, this research had the objective of developing and validate a high performance liquid chromatography method with pulsed amperometric detection (HPLC-PAD), which allow the determination of sulfur compounds in asphalt matrices. Using a gold electrode as a working electrode, a method with isocratic elution was developed that allows the determination of 11 organosulfur compounds. Two methodologies of sample preparation were studied in order to verify the presence of the organosulphur compounds in the crude sample, through a procedure of solid phase extraction (SPE) utilizing aminopropyl cartdriges, and in form of volatiles, through extraction using an extraction and collector device (DEC). In addition, a study of the amperometric detection of 22 compounds containing sulfur, including some in its oxidized form, was carried out in order to compare the reaction efficiency in a gold and carbon electrodes. The developed and validated chromatographic method present low detection limits, between 0,05 mg L-1 for dibutyldisulphite and 0,95 mg L-1 for 4-metyldibenzothiophene. The method was applied in the characterization of a crude sample of asphalt cement, allowing to determine the 3-phenylthiophene compound in form of volatiles, in the concentration of 0,160 mg kg-1. |
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2019-03-19T14:19:46Z2019-03-19T14:19:46Z2018-08-01http://repositorio.ufsm.br/handle/1/15930Among the heteroatoms present in petroleum, sulfur stands out as being the most abundant. Henceforth it can be found on many quantities in oil derivate, such as Petroleum Asphalt Cement (CAP). The presence of organosulfur compounds on asphalt matrix is related to the matrix aging processes, making it brittle and reducing the useful life of the pavement. Even more some of these compounds can be used as pollution markers in environmental analysis, and geological markers. We can also tie the presence of such elements as an occupational health hazard, seeing as some of them have a known carcinogenic and mutagenic potential. In face of that, this research had the objective of developing and validate a high performance liquid chromatography method with pulsed amperometric detection (HPLC-PAD), which allow the determination of sulfur compounds in asphalt matrices. Using a gold electrode as a working electrode, a method with isocratic elution was developed that allows the determination of 11 organosulfur compounds. Two methodologies of sample preparation were studied in order to verify the presence of the organosulphur compounds in the crude sample, through a procedure of solid phase extraction (SPE) utilizing aminopropyl cartdriges, and in form of volatiles, through extraction using an extraction and collector device (DEC). In addition, a study of the amperometric detection of 22 compounds containing sulfur, including some in its oxidized form, was carried out in order to compare the reaction efficiency in a gold and carbon electrodes. The developed and validated chromatographic method present low detection limits, between 0,05 mg L-1 for dibutyldisulphite and 0,95 mg L-1 for 4-metyldibenzothiophene. The method was applied in the characterization of a crude sample of asphalt cement, allowing to determine the 3-phenylthiophene compound in form of volatiles, in the concentration of 0,160 mg kg-1.Dentre os heteroátomos presentes no petróleo, o enxofre se destaca por ser o mais abundante. Sendo assim, este pode ser encontrado em grandes quantidades em derivados do petróleo, como o Cimento Asfáltico de Petróleo (CAP). A presença de compostos organossulfurados nas matrizes asfálticas é relacionada com processos de envelhecimento da matriz, tornando-a quebradiça e diminuindo o tempo de vida útil do pavimento. Além disto, alguns destes compostos podem ser utilizados como marcadores de poluição em análises ambientais e marcadores geológicos. Também podemos relacionar a presença destes compostos com problemas de saúde ocupacional, visto que alguns possuem conhecido potencial carcinogênico e mutagênico. Assim sendo, este trabalho teve o objetivo de desenvolver e validar um método de cromatografia líquida de alta eficiência com detecção pulso amperométrica (HPLC-PAD), que permitisse a determinação de compostos de enxofre nas matrizes asfálticas. Utilizando um eletrodo de ouro como eletrodo de trabalho, foi desenvolvido um método com eluição isocrática que permite a determinação de 11 compostos organossulfurados. Foram abordadas duas metodologias de preparo de amostras, a fim de verificar a presença dos compostos organossulfurados na amostra bruta, através de um procedimento de extração em fase sólida (SPE) utilizando cartuchos de aminopropil, e na forma de voláteis, através de uma extração utilizando um dispositivo de extração e coleta (DEC). Além disto, foi realizado um estudo da detecção amperométrica de 22 compostos contendo enxofre, incluindo alguns em sua forma oxidada a fim de comparar a eficiência da reação em eletrodo de ouro e de carbono. O método cromatográfico desenvolvido e validado, apresentou limites de detecção baixos, variando de 0,05 mg L-1 para o dibutil dissulfeto e 0,95 mg L-1 para o 4-metildibenzotiofeno. Este foi aplicado na caracterização de uma amostra bruta de cimento asfáltico, permitindo a determinação e quantificação do composto 3- feniltiofeno na forma de voláteis, na concentração de 0,160 mg kg-1.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/openAccessAsfalto de petróleoCompostos de enxofreDetecção pulsoamperométricaEletrodo de ouroPetroleum asphaltSulphur compoundsPulsed amperometric detectionGold electrodeCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométricaDetermination of sulfur compounds in petroleun asphalt sample using liquid chromatography with pulsed-amperometric detectioninfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisCarvalho, Leandro Machado dehttp://lattes.cnpq.br/6652387343920028Stülp, Simonehttp://lattes.cnpq.br/1793007242678493Boldrin, Maria Valnicehttp://lattes.cnpq.br/1183672452248157http://lattes.cnpq.br/4892773806882378Schmidt, Patricia1006000000006009da44f2c-6556-4846-9d66-386f290b802f38464520-5c0c-4f00-8deb-42e085cfa00fda9a49d4-c69e-4e99-8367-7938fe72b4268748d9df-0fe1-4677-8bd1-6e05b3788861reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2018_SCHMIDT_PATRICIA.pdfDIS_PPGQUIMICA_2018_SCHMIDT_PATRICIA.pdfDissertação de Mestradoapplication/pdf5113324http://repositorio.ufsm.br/bitstream/1/15930/1/DIS_PPGQUIMICA_2018_SCHMIDT_PATRICIA.pdf3c5576cbe3f9bd335db85362f70d7cfcMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica |
dc.title.alternative.eng.fl_str_mv |
Determination of sulfur compounds in petroleun asphalt sample using liquid chromatography with pulsed-amperometric detection |
title |
Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica |
spellingShingle |
Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica Schmidt, Patricia Asfalto de petróleo Compostos de enxofre Detecção pulsoamperométrica Eletrodo de ouro Petroleum asphalt Sulphur compounds Pulsed amperometric detection Gold electrode CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica |
title_full |
Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica |
title_fullStr |
Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica |
title_full_unstemmed |
Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica |
title_sort |
Determinação de compostos sulfurados em amostras de asfalto de petróleo empregando cromatografia líquida com detecção pulso-amperométrica |
author |
Schmidt, Patricia |
author_facet |
Schmidt, Patricia |
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 |
Stülp, Simone |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/1793007242678493 |
dc.contributor.referee2.fl_str_mv |
Boldrin, Maria Valnice |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/1183672452248157 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/4892773806882378 |
dc.contributor.author.fl_str_mv |
Schmidt, Patricia |
contributor_str_mv |
Carvalho, Leandro Machado de Stülp, Simone Boldrin, Maria Valnice |
dc.subject.por.fl_str_mv |
Asfalto de petróleo Compostos de enxofre Detecção pulsoamperométrica Eletrodo de ouro |
topic |
Asfalto de petróleo Compostos de enxofre Detecção pulsoamperométrica Eletrodo de ouro Petroleum asphalt Sulphur compounds Pulsed amperometric detection Gold electrode CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Petroleum asphalt Sulphur compounds Pulsed amperometric detection Gold electrode |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Among the heteroatoms present in petroleum, sulfur stands out as being the most abundant. Henceforth it can be found on many quantities in oil derivate, such as Petroleum Asphalt Cement (CAP). The presence of organosulfur compounds on asphalt matrix is related to the matrix aging processes, making it brittle and reducing the useful life of the pavement. Even more some of these compounds can be used as pollution markers in environmental analysis, and geological markers. We can also tie the presence of such elements as an occupational health hazard, seeing as some of them have a known carcinogenic and mutagenic potential. In face of that, this research had the objective of developing and validate a high performance liquid chromatography method with pulsed amperometric detection (HPLC-PAD), which allow the determination of sulfur compounds in asphalt matrices. Using a gold electrode as a working electrode, a method with isocratic elution was developed that allows the determination of 11 organosulfur compounds. Two methodologies of sample preparation were studied in order to verify the presence of the organosulphur compounds in the crude sample, through a procedure of solid phase extraction (SPE) utilizing aminopropyl cartdriges, and in form of volatiles, through extraction using an extraction and collector device (DEC). In addition, a study of the amperometric detection of 22 compounds containing sulfur, including some in its oxidized form, was carried out in order to compare the reaction efficiency in a gold and carbon electrodes. The developed and validated chromatographic method present low detection limits, between 0,05 mg L-1 for dibutyldisulphite and 0,95 mg L-1 for 4-metyldibenzothiophene. The method was applied in the characterization of a crude sample of asphalt cement, allowing to determine the 3-phenylthiophene compound in form of volatiles, in the concentration of 0,160 mg kg-1. |
publishDate |
2018 |
dc.date.issued.fl_str_mv |
2018-08-01 |
dc.date.accessioned.fl_str_mv |
2019-03-19T14:19:46Z |
dc.date.available.fl_str_mv |
2019-03-19T14:19:46Z |
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/1/15930 |
url |
http://repositorio.ufsm.br/handle/1/15930 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
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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:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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UFSM |
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UFSM |
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