Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica
Ano de defesa: | 2017 |
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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: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/17920 |
Resumo: | In this work, a method for the determination of rare earth elements (REE) present in low concentrations in crude oil, atmospheric distillation residue (RAT) and vacuum distillation residue (VR) using direct sampling and inductively coupled plasma mass spectrometry (ICP-MS) with electrothermal vaporization (ETV) was developed. Due to the facility of REE in forming refractory compounds inside the graphite furnace during the heating step, the use of a modifier gas (Freon R-12) was necessary to promote the vaporization and transport of these elements to the ICP-MS equipment. The use of 6 mg of citric acid was suitable for external calibration with aqueous reference solution. The heating program was evaluated based on the pyrolysis and vaporization curves for reference solution and samples. Pyrolysis and vaporization temperatures of 700 and 2200 °C were established, respectively. Considering that the transport efficiency of analytes to the plasma is related to the bypass, carrier and modifier (Freon R-12) gases, the flow rates of these gases for the aqueous reference solution and the samples were evaluated. The flow rates of 0.40 L min-1, 0.40 L min-1 e 2.0 mL min-1 were selected for the bypass, carrier and Freon R-12 gases, respectively. Using the operational conditions optimized for the ETV-ICP-MS system, the applicability of the method for the determination of REE in synthetic crude oil emulsions with different water contents and NaCl concentrations was investigated. It was observed that synthetic crude oil emulsions with water content and NaCl concentration up to 10% and 2000 μg g-1, respectively, can be analyzed by ETV-ICP-MS. The influence of sample mass was evaluated and relatively high masses (up to 18 mg of crude oil, 5 mg of RAT and 6 mg of RV) can be employed in the proposed method. The accuracy was evaluated by the comparison of results obtained by ETV-ICP-MS with those obtained by ICP-MS with ultrasonic nebulizer (USN) after microwave assisted wet digestion (MAWD) using a mixture of concentrated HNO3 and H2O2. No statistical difference (t-Student, 95% of confidence level) was observed between the results obtained for REE in crude oil (water content from 0.12 to 2%), RAT and RV by ETV-ICP-MS and USN-ICP-MS after MAWD. The limits of quantification for REE by ETV-ICP-MS were lower (between 0.02 and 2.7 ng g-1) than the values obtained by USN-ICP-MS after MAWD (between 0.6 and 3.7 ng g-1). The ETV-ICP-MS method was proposed for the first time for the determination of REE in low concentrations in crude oil and distillation residues showing to be a promising alternative for routine analysis. |
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2019-08-14T16:14:06Z2019-08-14T16:14:06Z2017-07-29http://repositorio.ufsm.br/handle/1/17920In this work, a method for the determination of rare earth elements (REE) present in low concentrations in crude oil, atmospheric distillation residue (RAT) and vacuum distillation residue (VR) using direct sampling and inductively coupled plasma mass spectrometry (ICP-MS) with electrothermal vaporization (ETV) was developed. Due to the facility of REE in forming refractory compounds inside the graphite furnace during the heating step, the use of a modifier gas (Freon R-12) was necessary to promote the vaporization and transport of these elements to the ICP-MS equipment. The use of 6 mg of citric acid was suitable for external calibration with aqueous reference solution. The heating program was evaluated based on the pyrolysis and vaporization curves for reference solution and samples. Pyrolysis and vaporization temperatures of 700 and 2200 °C were established, respectively. Considering that the transport efficiency of analytes to the plasma is related to the bypass, carrier and modifier (Freon R-12) gases, the flow rates of these gases for the aqueous reference solution and the samples were evaluated. The flow rates of 0.40 L min-1, 0.40 L min-1 e 2.0 mL min-1 were selected for the bypass, carrier and Freon R-12 gases, respectively. Using the operational conditions optimized for the ETV-ICP-MS system, the applicability of the method for the determination of REE in synthetic crude oil emulsions with different water contents and NaCl concentrations was investigated. It was observed that synthetic crude oil emulsions with water content and NaCl concentration up to 10% and 2000 μg g-1, respectively, can be analyzed by ETV-ICP-MS. The influence of sample mass was evaluated and relatively high masses (up to 18 mg of crude oil, 5 mg of RAT and 6 mg of RV) can be employed in the proposed method. The accuracy was evaluated by the comparison of results obtained by ETV-ICP-MS with those obtained by ICP-MS with ultrasonic nebulizer (USN) after microwave assisted wet digestion (MAWD) using a mixture of concentrated HNO3 and H2O2. No statistical difference (t-Student, 95% of confidence level) was observed between the results obtained for REE in crude oil (water content from 0.12 to 2%), RAT and RV by ETV-ICP-MS and USN-ICP-MS after MAWD. The limits of quantification for REE by ETV-ICP-MS were lower (between 0.02 and 2.7 ng g-1) than the values obtained by USN-ICP-MS after MAWD (between 0.6 and 3.7 ng g-1). The ETV-ICP-MS method was proposed for the first time for the determination of REE in low concentrations in crude oil and distillation residues showing to be a promising alternative for routine analysis.Neste trabalho foi desenvolvido um método para a determinação de elementos terras raras (REE) presentes em baixas concentrações em petróleo, resíduo da destilação atmosférica (RAT) e resíduo da destilação a vácuo (RV) utilizando amostragem direta e espectrometria de massa com plasma indutivamente acoplado (ICP-MS) com vaporização eletrotérmica (ETV). Devido à facilidade dos REE em formarem compostos refratários no forno de grafite durante o aquecimento, foi necessário o uso de Freon R-12 para promover a vaporização e transporte desses elementos para o equipamento de ICP-MS. Com o uso de 6 mg de ácido cítrico foi possível efetuar a calibração externa com solução de referência aquosa. A avaliação do programa de aquecimento foi feita com base nas curvas de pirólise e vaporização da solução e amostras. Foram estabelecidas as temperaturas de pirólise e vaporização de 700 e 2200 °C, respectivamente. Tendo em vista que a eficiência de transporte dos analitos para o plasma está relacionada com os gases bypass, carreador e Freon R-12, foram avaliadas as vazões desses gases para a solução de referência aquosa e amostras. Foram estabelecidas as vazões de 0,40 L min-1, 0,40 L min-1 e 2,0 mL min-1 para os gases bypass, carreador e Freon R-12, respectivamente. Após estabelecer as condições operacionais do sistema de ETV-ICP-MS, foi investigada a aplicabilidade do método para a determinação de REE em emulsões sintéticas de petróleo com diferentes teores de água e concentrações de NaCl. Foi verificado que as emulsões sintéticas de petróleo com no máximo 10% de água e até 2000 μg g-1 de NaCl podem ser analisadas por ETV-ICP-MS. A influência da massa de amostra foi avaliada e massas relativamente elevadas (até 18 mg de petróleo, 5 mg de RAT e 6 mg de RV) podem ser empregadas no método proposto. A exatidão foi avaliada pela comparação dos resultados obtidos por ETV-ICP-MS com aqueles obtidos por ICP-MS com nebulizador ultrassônico (USN) após a decomposição por via úmida assistida por radiação micro-ondas (MAWD) utilizando uma mistura de HNO3 concentrado e H2O2. Os resultados obtidos para os REE em petróleo (teor de água de 0,12 a 2%), RAT e RV por ETV-ICP-MS e USN-ICP-MS após MAWD não apresentaram diferença estatística (t-Student, com nível de confiança de 95%). Os limites de quantificação dos REE por ETV-ICP-MS foram menores (entre 0,02 e 2,7 ng g-1) em relação ao método de USN-ICP-MS após MAWD (entre 0,6 e 3,7 ng g-1). O método de ETV-ICP-MS foi proposto pela primeira vez para a determinação de REE em baixas concentrações em petróleo e resíduos de destilação e mostrou ser uma alternativa promissora para a análise de rotina.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/openAccessElementos terras rarasEspectrometria de massa com plasma indutivamente acopladoCurvas de piróliseVaporizaçãoCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmicainfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Bizzi, Cezar Augustohttp://lattes.cnpq.br/2975070149037006Moraes, Diogo Pompéu dehttp://lattes.cnpq.br/3777062632260326Pereira, Juliana Severo Fagundeshttp://lattes.cnpq.br/7210654180380205Bolzan, Rodrigo Cordeirohttp://lattes.cnpq.br/9392316362285896http://lattes.cnpq.br/8753473372692707Silva, Jussiane Souza da100600000000600a9c2788c-7913-4d7b-92e1-3429800ac02858644f32-5c67-4140-b154-33f4a7a579cdbe6876cc-2db6-4d50-8c79-b4b0a2425b0cf14a305a-1edb-4607-8511-83ac442803481455b455-8182-4f00-97d5-0e37ca07b1aa0ef936da-d1b2-40bd-8da8-0ca4bfad89d3reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica |
title |
Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica |
spellingShingle |
Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica Silva, Jussiane Souza da Elementos terras raras Espectrometria de massa com plasma indutivamente acoplado Curvas de pirólise Vaporização CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica |
title_full |
Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica |
title_fullStr |
Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica |
title_full_unstemmed |
Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica |
title_sort |
Determinação de elementos terras raras em petróleo e frações por amostragem direta e ICP-MS com vaporização eletrotérmica |
author |
Silva, Jussiane Souza da |
author_facet |
Silva, Jussiane Souza da |
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 |
Bizzi, Cezar Augusto |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/2975070149037006 |
dc.contributor.referee2.fl_str_mv |
Moraes, Diogo Pompéu de |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/3777062632260326 |
dc.contributor.referee3.fl_str_mv |
Pereira, Juliana Severo Fagundes |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/7210654180380205 |
dc.contributor.referee4.fl_str_mv |
Bolzan, Rodrigo Cordeiro |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/9392316362285896 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/8753473372692707 |
dc.contributor.author.fl_str_mv |
Silva, Jussiane Souza da |
contributor_str_mv |
Flores, Érico Marlon de Moraes Bizzi, Cezar Augusto Moraes, Diogo Pompéu de Pereira, Juliana Severo Fagundes Bolzan, Rodrigo Cordeiro |
dc.subject.por.fl_str_mv |
Elementos terras raras Espectrometria de massa com plasma indutivamente acoplado Curvas de pirólise Vaporização |
topic |
Elementos terras raras Espectrometria de massa com plasma indutivamente acoplado Curvas de pirólise Vaporização CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, a method for the determination of rare earth elements (REE) present in low concentrations in crude oil, atmospheric distillation residue (RAT) and vacuum distillation residue (VR) using direct sampling and inductively coupled plasma mass spectrometry (ICP-MS) with electrothermal vaporization (ETV) was developed. Due to the facility of REE in forming refractory compounds inside the graphite furnace during the heating step, the use of a modifier gas (Freon R-12) was necessary to promote the vaporization and transport of these elements to the ICP-MS equipment. The use of 6 mg of citric acid was suitable for external calibration with aqueous reference solution. The heating program was evaluated based on the pyrolysis and vaporization curves for reference solution and samples. Pyrolysis and vaporization temperatures of 700 and 2200 °C were established, respectively. Considering that the transport efficiency of analytes to the plasma is related to the bypass, carrier and modifier (Freon R-12) gases, the flow rates of these gases for the aqueous reference solution and the samples were evaluated. The flow rates of 0.40 L min-1, 0.40 L min-1 e 2.0 mL min-1 were selected for the bypass, carrier and Freon R-12 gases, respectively. Using the operational conditions optimized for the ETV-ICP-MS system, the applicability of the method for the determination of REE in synthetic crude oil emulsions with different water contents and NaCl concentrations was investigated. It was observed that synthetic crude oil emulsions with water content and NaCl concentration up to 10% and 2000 μg g-1, respectively, can be analyzed by ETV-ICP-MS. The influence of sample mass was evaluated and relatively high masses (up to 18 mg of crude oil, 5 mg of RAT and 6 mg of RV) can be employed in the proposed method. The accuracy was evaluated by the comparison of results obtained by ETV-ICP-MS with those obtained by ICP-MS with ultrasonic nebulizer (USN) after microwave assisted wet digestion (MAWD) using a mixture of concentrated HNO3 and H2O2. No statistical difference (t-Student, 95% of confidence level) was observed between the results obtained for REE in crude oil (water content from 0.12 to 2%), RAT and RV by ETV-ICP-MS and USN-ICP-MS after MAWD. The limits of quantification for REE by ETV-ICP-MS were lower (between 0.02 and 2.7 ng g-1) than the values obtained by USN-ICP-MS after MAWD (between 0.6 and 3.7 ng g-1). The ETV-ICP-MS method was proposed for the first time for the determination of REE in low concentrations in crude oil and distillation residues showing to be a promising alternative for routine analysis. |
publishDate |
2017 |
dc.date.issued.fl_str_mv |
2017-07-29 |
dc.date.accessioned.fl_str_mv |
2019-08-14T16:14:06Z |
dc.date.available.fl_str_mv |
2019-08-14T16:14:06Z |
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/1/17920 |
url |
http://repositorio.ufsm.br/handle/1/17920 |
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 58644f32-5c67-4140-b154-33f4a7a579cd be6876cc-2db6-4d50-8c79-b4b0a2425b0c f14a305a-1edb-4607-8511-83ac44280348 1455b455-8182-4f00-97d5-0e37ca07b1aa 0ef936da-d1b2-40bd-8da8-0ca4bfad89d3 |
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 |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
bitstream.url.fl_str_mv |
http://repositorio.ufsm.br/bitstream/1/17920/2/license_rdf http://repositorio.ufsm.br/bitstream/1/17920/1/TES_PPGQUIMICA_2017_SILVA_JUSSIANE.pdf http://repositorio.ufsm.br/bitstream/1/17920/3/license.txt http://repositorio.ufsm.br/bitstream/1/17920/4/TES_PPGQUIMICA_2017_SILVA_JUSSIANE.pdf.txt http://repositorio.ufsm.br/bitstream/1/17920/5/TES_PPGQUIMICA_2017_SILVA_JUSSIANE.pdf.jpg |
bitstream.checksum.fl_str_mv |
4460e5956bc1d1639be9ae6146a50347 1c415a5c8ae45f006a568b1c246d9728 2f0571ecee68693bd5cd3f17c1e075df 728b6aeb93f84a8b7213a16262aa0059 55a5e86ba93e9dc96f3e1958a7108855 |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 MD5 MD5 |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
|
_version_ |
1794524389987844096 |