Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel
Ano de defesa: | 2022 |
---|---|
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/1/27860 |
Resumo: | This work aimed to developed methods to contribute to the understanding of the structure of sulfur and nitrogen compounds, as well as the fraction of basic nitrogen present in diesel oil. Sample preparation methods were evaluated for the extraction of sulfur and nitrogen compounds from diesel oil, as well as for the selective extraction of basic nitrogen compounds. For this purpose, liquid-liquid extraction, solid phase extraction (SPE) and reversed-phase liquid-liquid dispersive microextraction (RPDLLME, with and without the use of ultrasound) were evaluated, and the parameters influencing each procedure, such as sample mass, amount of solid phase, type of extract and dispersant solvent, proportion between solvents, among others, were optimized. The determination of total sulfur and nitrogen in the diesel oil before and after extraction, using an elemental analyzer was carried out to evaluate the extraction efficiency. The extraction efficiency for basic nitrogen was evaluated using the UOP 269 standard method, using potentiometric titration and with HClO4 as the titrant. About sulfur extraction, none of those methods provided extraction efficiency greater than 55%, which demonstrates the difficulty in extracting such compounds from diesel oil. Regarding nitrogen, it was possible to obtain an extraction efficiency of 91% when using the SPE method with 1 g of silica gel as a solid phase, 0.5 mL of diesel oil and acetic acid as the extract solvent. With the RP-DLLME method, 69% extraction efficiency was obtained when using 60 µL of formic acid as extract solvent, 200 µL of isopropanol as dispersant solvent and 0.5 g of diesel oil. Under specific conditions, it was possible to carry out the extraction of basic nitrogen fraction for RP-DLLME using 5 g of diesel oil, 400 µL of formic acid and 600 µL of isopropanol (extract and dispersant solvents, respectively), resulting in a concentration factor of 10.2. Extracts were analyzed by time-of-flight mass spectrometry with electrospray ionization (ESIToFMS). With emphasis on the basic nitrogen content, a miniaturized method was developed using a portable device with digital image acquisition and PhotoMetrix PRO, based on the colorimetric titration described in the UOP 269 standard method and making a multivariate calibration model with the partial least squares (PLS) method. Some conditions were optimized, such as the volume of indicator, volume and concentration of HClO4, as well as the accuracy with the variation of the volume of diesel oil. With the use of 60 µL of indicator, 20 µL of 20 mmol L-1 HClO4 and using from 50 to 100 µL of sample the best conditions for calibration were obtained (RMSEP of 0.38 mg kg-1 , RMSECV of 0.31 mg kg-1 with the use of 4 factors). |
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2023-02-23T12:53:24Z2023-02-23T12:53:24Z2022-08-26http://repositorio.ufsm.br/handle/1/27860This work aimed to developed methods to contribute to the understanding of the structure of sulfur and nitrogen compounds, as well as the fraction of basic nitrogen present in diesel oil. Sample preparation methods were evaluated for the extraction of sulfur and nitrogen compounds from diesel oil, as well as for the selective extraction of basic nitrogen compounds. For this purpose, liquid-liquid extraction, solid phase extraction (SPE) and reversed-phase liquid-liquid dispersive microextraction (RPDLLME, with and without the use of ultrasound) were evaluated, and the parameters influencing each procedure, such as sample mass, amount of solid phase, type of extract and dispersant solvent, proportion between solvents, among others, were optimized. The determination of total sulfur and nitrogen in the diesel oil before and after extraction, using an elemental analyzer was carried out to evaluate the extraction efficiency. The extraction efficiency for basic nitrogen was evaluated using the UOP 269 standard method, using potentiometric titration and with HClO4 as the titrant. About sulfur extraction, none of those methods provided extraction efficiency greater than 55%, which demonstrates the difficulty in extracting such compounds from diesel oil. Regarding nitrogen, it was possible to obtain an extraction efficiency of 91% when using the SPE method with 1 g of silica gel as a solid phase, 0.5 mL of diesel oil and acetic acid as the extract solvent. With the RP-DLLME method, 69% extraction efficiency was obtained when using 60 µL of formic acid as extract solvent, 200 µL of isopropanol as dispersant solvent and 0.5 g of diesel oil. Under specific conditions, it was possible to carry out the extraction of basic nitrogen fraction for RP-DLLME using 5 g of diesel oil, 400 µL of formic acid and 600 µL of isopropanol (extract and dispersant solvents, respectively), resulting in a concentration factor of 10.2. Extracts were analyzed by time-of-flight mass spectrometry with electrospray ionization (ESIToFMS). With emphasis on the basic nitrogen content, a miniaturized method was developed using a portable device with digital image acquisition and PhotoMetrix PRO, based on the colorimetric titration described in the UOP 269 standard method and making a multivariate calibration model with the partial least squares (PLS) method. Some conditions were optimized, such as the volume of indicator, volume and concentration of HClO4, as well as the accuracy with the variation of the volume of diesel oil. With the use of 60 µL of indicator, 20 µL of 20 mmol L-1 HClO4 and using from 50 to 100 µL of sample the best conditions for calibration were obtained (RMSEP of 0.38 mg kg-1 , RMSECV of 0.31 mg kg-1 with the use of 4 factors).Esse trabalho teve como objetivo desenvolver métodos para contribuir com o entendimento sobre a estrutura dos compostos sulfurados e nitrogenados, bem como da fração de nitrogênio básico, presente em óleo diesel. Foram avaliados métodos de preparo de amostra para a extração de compostos de enxofre e de nitrogênio do óleo diesel, bem como para a extração seletiva de compostos de nitrogênio básico. Para isso, os métodos de extração líquido-líquido, extração em fase sólida (SPE) e microextração dispersiva líquido-líquido em fase reversa (RP-DLLME, com e sem uso de ultrassom) foram avaliados, sendo otimizados os parâmetros que mais influenciariam em cada procedimento, como massa de óleo diesel, quantidade de fase sólida, tipo de solvente extrator e dispersor, proporção entre solventes, dentre outros. A determinação de enxofre e nitrogênio total no óleo diesel antes e após extração foi feita utilizando um analisador elementar, viabilizando a avaliação da eficiência de extração. A eficiência de extração para nitrogênio básico foi avaliada utilizando a norma UOP 269, com o uso de titulação potenciométrica e com HClO4 como titulante. No que diz respeito à extração de enxofre, nenhum dos métodos avaliados proporcionou eficiência de extração superior a 55%, o que demonstra a dificuldade em se extrair tais compostos de óleo diesel. Em relação à extração de nitrogênio, foi possível obter eficiência de extração de 91% quando utilizado o método de SPE com 1 g de sílica gel como fase sólida, 0,5 mL de óleo diesel e ácido acético como solvente extrator. Com o método de RP-DLLME, foi obtida uma extração de 69% quando utilizado 60 µL de ácido fórmico como solvente extrator, 200 µL de isopropanol como solvente dispersor e 0,5 g de óleo diesel. Sob condições específicas, foi possível realizar a extração seletiva de nitrogênio básico usando a RP-DLLME, com 5 g de óleo diesel, 400 µL de ácido fórmico e 600 µL de isopropanol (solventes extrator e dispersor, respectivamente), resultando em um fator de concentração de 10,2. Os extratos foram avaliados por espectrometria de massas por tempo de vôo com ionização por electrospray (ESI-ToFMS). Com ênfase no teor de nitrogênio básico, foi desenvolvido um método com uso de sistema miniaturizado utilizando dispositivo portátil e obtenção de imagem digital e PhotoMetrix PRO, tomando como base a titulação colorimétrica descrita na norma UOP 269 e fazendo uma calibração multivariada com o método dos mínimos quadrados parciais (PLS). Algumas condições foram otimizadas, como o volume de indicador, volume e concentração de HClO4, bem como a verificação da exatidão com a variação do volume de óleo diesel. Com o uso de 60 µL de indicador, 20 µL de HClO4 20 mmol L-1 e 50 a 100 µL de amostra, foram obtidas as melhores condições para calibração (RMSEP de 0,38 mg kg-1 , RMSECV de 0,31 mg kg-1 com uso de 4 fatores) e quantificação de nitrogênio básico.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/openAccessÓleo dieselExtração seletivaEnxofre e nitrogênioNitrogênio básicoPhotoMetrix PRODiesel oilSelective extractionSulfur and nitrogenBasic nitrogenCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo dieselAlternative methods development for extraction and determination of sulfur and nitrogen compounds in diesel oilinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisMello, Paola de Azevedohttp://lattes.cnpq.br/2189500441942469Duarte, Fábio AndreiCruz, Sandra Meinen daFlores, Éder Lisandro de MoraesMüller, Edson IrineuBarin, Juliano Smaniotohttp://lattes.cnpq.br/6803677326638722Iop, Gabrielle Dineck1006000000006006006006006006006006000128b934-4b3f-43d6-8526-fb278da0f67341b81590-6308-4707-9f14-a70a1cb13cb98c8f72b3-143f-45af-ad25-36f309ba9a0cd207d062-dacc-4b87-a08b-f3af79cb2b533e5cf21b-1b38-4d13-9721-12aea4448f365340e61b-ef9c-45e3-9754-7c9649711f61a67ec841-c91a-41e1-a3fb-56107c9ca986reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2022_IOP_GABRIELLE.pdfTES_PPGQUÍMICA_2022_IOP_GABRIELLE.pdfTese de doutoradoapplication/pdf2012049http://repositorio.ufsm.br/bitstream/1/27860/1/TES_PPGQU%c3%8dMICA_2022_IOP_GABRIELLE.pdf6e95d435a2e9b33f6cce479dde9a4f71MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel |
dc.title.alternative.eng.fl_str_mv |
Alternative methods development for extraction and determination of sulfur and nitrogen compounds in diesel oil |
title |
Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel |
spellingShingle |
Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel Iop, Gabrielle Dineck Óleo diesel Extração seletiva Enxofre e nitrogênio Nitrogênio básico PhotoMetrix PRO Diesel oil Selective extraction Sulfur and nitrogen Basic nitrogen CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel |
title_full |
Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel |
title_fullStr |
Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel |
title_full_unstemmed |
Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel |
title_sort |
Desenvolvimento de métodos alternativos para a extração e determinação de compostos sulfurados e nitrogenados em óleo diesel |
author |
Iop, Gabrielle Dineck |
author_facet |
Iop, Gabrielle Dineck |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Mello, Paola de Azevedo |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2189500441942469 |
dc.contributor.advisor-co1.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.referee1.fl_str_mv |
Cruz, Sandra Meinen da |
dc.contributor.referee2.fl_str_mv |
Flores, Éder Lisandro de Moraes |
dc.contributor.referee3.fl_str_mv |
Müller, Edson Irineu |
dc.contributor.referee4.fl_str_mv |
Barin, Juliano Smanioto |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/6803677326638722 |
dc.contributor.author.fl_str_mv |
Iop, Gabrielle Dineck |
contributor_str_mv |
Mello, Paola de Azevedo Duarte, Fábio Andrei Cruz, Sandra Meinen da Flores, Éder Lisandro de Moraes Müller, Edson Irineu Barin, Juliano Smanioto |
dc.subject.por.fl_str_mv |
Óleo diesel Extração seletiva Enxofre e nitrogênio Nitrogênio básico PhotoMetrix PRO |
topic |
Óleo diesel Extração seletiva Enxofre e nitrogênio Nitrogênio básico PhotoMetrix PRO Diesel oil Selective extraction Sulfur and nitrogen Basic nitrogen CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Diesel oil Selective extraction Sulfur and nitrogen Basic nitrogen |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
This work aimed to developed methods to contribute to the understanding of the structure of sulfur and nitrogen compounds, as well as the fraction of basic nitrogen present in diesel oil. Sample preparation methods were evaluated for the extraction of sulfur and nitrogen compounds from diesel oil, as well as for the selective extraction of basic nitrogen compounds. For this purpose, liquid-liquid extraction, solid phase extraction (SPE) and reversed-phase liquid-liquid dispersive microextraction (RPDLLME, with and without the use of ultrasound) were evaluated, and the parameters influencing each procedure, such as sample mass, amount of solid phase, type of extract and dispersant solvent, proportion between solvents, among others, were optimized. The determination of total sulfur and nitrogen in the diesel oil before and after extraction, using an elemental analyzer was carried out to evaluate the extraction efficiency. The extraction efficiency for basic nitrogen was evaluated using the UOP 269 standard method, using potentiometric titration and with HClO4 as the titrant. About sulfur extraction, none of those methods provided extraction efficiency greater than 55%, which demonstrates the difficulty in extracting such compounds from diesel oil. Regarding nitrogen, it was possible to obtain an extraction efficiency of 91% when using the SPE method with 1 g of silica gel as a solid phase, 0.5 mL of diesel oil and acetic acid as the extract solvent. With the RP-DLLME method, 69% extraction efficiency was obtained when using 60 µL of formic acid as extract solvent, 200 µL of isopropanol as dispersant solvent and 0.5 g of diesel oil. Under specific conditions, it was possible to carry out the extraction of basic nitrogen fraction for RP-DLLME using 5 g of diesel oil, 400 µL of formic acid and 600 µL of isopropanol (extract and dispersant solvents, respectively), resulting in a concentration factor of 10.2. Extracts were analyzed by time-of-flight mass spectrometry with electrospray ionization (ESIToFMS). With emphasis on the basic nitrogen content, a miniaturized method was developed using a portable device with digital image acquisition and PhotoMetrix PRO, based on the colorimetric titration described in the UOP 269 standard method and making a multivariate calibration model with the partial least squares (PLS) method. Some conditions were optimized, such as the volume of indicator, volume and concentration of HClO4, as well as the accuracy with the variation of the volume of diesel oil. With the use of 60 µL of indicator, 20 µL of 20 mmol L-1 HClO4 and using from 50 to 100 µL of sample the best conditions for calibration were obtained (RMSEP of 0.38 mg kg-1 , RMSECV of 0.31 mg kg-1 with the use of 4 factors). |
publishDate |
2022 |
dc.date.issued.fl_str_mv |
2022-08-26 |
dc.date.accessioned.fl_str_mv |
2023-02-23T12:53:24Z |
dc.date.available.fl_str_mv |
2023-02-23T12:53:24Z |
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/1/27860 |
url |
http://repositorio.ufsm.br/handle/1/27860 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 600 600 |
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 |
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Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
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