Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo
Ano de defesa: | 2019 |
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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/1/21399 |
Resumo: | In this work, the ASTM D 4807 standard method combined with scanning electron microscopy (SEM) was used and evaluated for the identification of the morphology and composition of saline species present in sediments isolated from emulsions of Brazilian pre-salt crude oils. Modifications to ASTM D 4807 were evaluated in order to assess the amount of isolated sediments and the solubility of the saline species present on the membrane surface. The evaluated modifications were: (I) mixture composed of 50% toluene + 50% isopropanol (v / v) as solvent; (II) mixture of 50% toluene + 49.5% isopropanol + 0.5% water as solvent and (III) additional membrane washing step with hot water after filtration following ASTM D 4807. For the sediment content determination, membranes with porosity of 0.10 and 0.22 μm were used. Additionally, the saline species retained on the membranes with porosity 0.45, 0.22 and 0.10 μm after filtration according to ASTM D 4807 were solubilized in water for further Ca, Cl, Mg and Na determination by ICP OES. Using SEM, different structures of inorganic solids were identified on the membrane surface post filtration according to ASTM D 4807, among which cubic, spherical, star, rod and finely divided solids can be highlighted. Regarding sediment composition, the elements Na, Cl, Ca, Ba Fe, K, Mg, S, Si and Sr were identified in the sediments retained on the nylon membranes. ASTM D 4807 with modification I produced a reduction (greater than 50%) of sediment content when compared to the method without modification. The toluene + isopropanol mixture possibly minimized the crystallization of some inorganic solids, as there is an increase in the solubility of chloride containing salts in isopropanol when compared to toluene. Modification I allowed the isolation of a larger amount of crystalline structures in the form of “salt spheres”. Apparently, the presence of these structures appears to be related to the presence of isopropanol in the solvent mixture used in the filtration. Regarding modification II, a reduction in sediment content was also observed. The use of water in the solvent mixture allowed the partial solubilization of part of inorganic solids otherwise insoluble (using the unmodified method or modification I). When modification III was used, a reduction of more than 82% in the amount of inorganic solids retained on the membrane surface was observed. This indicates that the additional washing step using hot water allows the solubilization of nearly all soluble inorganic species present in the sediment retained on nylon membranes. After washing with water, the presence of water-insoluble salts, probably composed of alkaline earth elements of sulfates and carbonates, iron and silicates was detected on the membrane surface. When membranes with smaller porosity (0.10 and 0.22 μm) were used, no significant difference in sediment content was observed for most samples when compared to the 0.45 μm membrane. Thus, some experimental conditions proposed by ASTM D 4807, especially the type of solvent used, induce crystallization of saline species present in petroleum emulsions. These species are probably soluble in the aqueous phase of the emulsions and the use of ASTM D 4807 with toluene originates these solid species, which are retained on the membrane surface. This conclusion is corroborated by the fact that modifications I, II and III allowed a reduction in sediment content. |
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2021-07-12T13:28:54Z2021-07-12T13:28:54Z2019-07-18http://repositorio.ufsm.br/handle/1/21399In this work, the ASTM D 4807 standard method combined with scanning electron microscopy (SEM) was used and evaluated for the identification of the morphology and composition of saline species present in sediments isolated from emulsions of Brazilian pre-salt crude oils. Modifications to ASTM D 4807 were evaluated in order to assess the amount of isolated sediments and the solubility of the saline species present on the membrane surface. The evaluated modifications were: (I) mixture composed of 50% toluene + 50% isopropanol (v / v) as solvent; (II) mixture of 50% toluene + 49.5% isopropanol + 0.5% water as solvent and (III) additional membrane washing step with hot water after filtration following ASTM D 4807. For the sediment content determination, membranes with porosity of 0.10 and 0.22 μm were used. Additionally, the saline species retained on the membranes with porosity 0.45, 0.22 and 0.10 μm after filtration according to ASTM D 4807 were solubilized in water for further Ca, Cl, Mg and Na determination by ICP OES. Using SEM, different structures of inorganic solids were identified on the membrane surface post filtration according to ASTM D 4807, among which cubic, spherical, star, rod and finely divided solids can be highlighted. Regarding sediment composition, the elements Na, Cl, Ca, Ba Fe, K, Mg, S, Si and Sr were identified in the sediments retained on the nylon membranes. ASTM D 4807 with modification I produced a reduction (greater than 50%) of sediment content when compared to the method without modification. The toluene + isopropanol mixture possibly minimized the crystallization of some inorganic solids, as there is an increase in the solubility of chloride containing salts in isopropanol when compared to toluene. Modification I allowed the isolation of a larger amount of crystalline structures in the form of “salt spheres”. Apparently, the presence of these structures appears to be related to the presence of isopropanol in the solvent mixture used in the filtration. Regarding modification II, a reduction in sediment content was also observed. The use of water in the solvent mixture allowed the partial solubilization of part of inorganic solids otherwise insoluble (using the unmodified method or modification I). When modification III was used, a reduction of more than 82% in the amount of inorganic solids retained on the membrane surface was observed. This indicates that the additional washing step using hot water allows the solubilization of nearly all soluble inorganic species present in the sediment retained on nylon membranes. After washing with water, the presence of water-insoluble salts, probably composed of alkaline earth elements of sulfates and carbonates, iron and silicates was detected on the membrane surface. When membranes with smaller porosity (0.10 and 0.22 μm) were used, no significant difference in sediment content was observed for most samples when compared to the 0.45 μm membrane. Thus, some experimental conditions proposed by ASTM D 4807, especially the type of solvent used, induce crystallization of saline species present in petroleum emulsions. These species are probably soluble in the aqueous phase of the emulsions and the use of ASTM D 4807 with toluene originates these solid species, which are retained on the membrane surface. This conclusion is corroborated by the fact that modifications I, II and III allowed a reduction in sediment content.Neste trabalho foi utilizada e avaliada a norma ASTM D 4807 combinada a microscopia eletrônica de varredura (MEV), para a identificação da morfologia e composição das espécies salinas presentes nos sedimentos isolados de emulsões de petróleos brasileiros da camada pré-sal. Foram avaliadas modificações na norma ASTM D 4807 a fim de avaliar a quantidade de sedimentos isolados e a solubilidade das espécies salinas presentes na superfície das membranas. As modificações avaliadas foram: (I) utilização da mistura de solventes composta por 50% isopropanol + 50% tolueno (v/v); (II) mistura de solventes com 49,5% isopropanol + 50% tolueno + 0,5% água e, também, (III) etapa adicional de lavagem das membranas com água quente após a filtração seguindo a norma ASTM D 4807. Também foram utilizadas, para a determinação do teor de sedimentos, membranas de porosidades de 0,10 e 0,22 μm. Adicionalmente, foi feita a solubilização em água das espécies salinas retidas nas membranas de 0,45, 0,22 e 0,10 μm após a filtração segundo a norma ASTM D 4807, e posterior quantificação de Ca, Cl, Mg e Na por ICP OES. Diferentes estruturas de sólidos inorgânicos foram identificadas na superfície das membranas obtidas utilizando a norma ASTM D4807, dentre as quais se destacam sólidos cúbicos, esféricos, na forma de “estrela”, na forma de “bastões” e sólidos finamente divididos. Com relação a composição dos sedimentos, foram identificados os elementos Na, Cl, Ca, Ba Fe, K, Mg, S, Si e Sr nos sedimentos retidos na membrana de nylon. A ASTM D 4807 com a modificação I produziu uma redução (superior a 50%) do teor de sedimentos quando comparado com a norma sem modificação. Provavelmente, a utilização da mistura tolueno+isopropanol minimizou a cristalização de alguns sólidos inorgânicos, já que há um aumento da solubilidade dos sais contendo cloreto em isopropanol em comparação a utilização somente do tolueno. A utilização da modificação I permitiu o isolamento de uma maior quantidade de estruturas cristalinas na forma de “esfera salina”. Aparentemente, a presença destas estruturas parece estar relacionada com a presença de isopropanol na mistura de solventes usada na filtração. Com relação a modificação II, também foi observada uma redução no teor de sedimentos. A utilização de água na mistura de solventes permitiu a solubilização de parte dos sólidos inorgânicos que não são solúveis utilizando a norma não modificada e na modificação I. Quando utilizada a modificação III, observa-se uma redução superior a 82% na quantidade de sólidos inorgânicos retidos na superfície da membrana. Isto indica que a utilização da lavagem adicional com água quente permite a solubilização de praticamente todas as espécies inorgânicas solúveis presentes nos sedimentos retidos nas membranas de nylon. Após a lavagem com água foi detectada na superfície das membranas a presença de sais insolúveis em água, constituídos provavelmente por sulfatos e carbonatos insolúveis de elementos alcalino-terrosos, ferro e silicatos insolúveis. Quando foram utilizadas membranas de menor porosidade (0,10 e 0,22 μm) não foi observada diferença significativa no teor de sedimentos, para a maioria das amostras, quando comparada com a membrana de 0,45 μm. Assim, constata-se que algumas condições experimentais propostas pela norma ASTM D 4807, principalmente o tipo de solvente utilizado, induz a cristalização de espécies salinas presentes nas emulsões de petróleo. Provavelmente, estas espécies estejam solúveis na fase aquosa das emulsões e a utilização da norma ASTM D 4807 com tolueno produza estas espécies sólidas que são retidas na superfície das membranas. Esta conclusão é corroborada pelo fato de que as modificações I, II e III permitiram a redução no teor de sedimentos.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/openAccessPetróleoMicroscopia eletrônica de varreduraTeor de sedimentosCrude oilScanning electron microscopySediment contentCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAMétodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleoMethods for identification and quantification of salin species and sediments in crude oilinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisMüller, Edson Irineuhttp://lattes.cnpq.br/5994311290376153Flores, Érico Marlon de MoraesCosta, Adilson Ben daMortari, Sergio RobertoDuarte, Fábio AndreiDressler, Valderi Luizhttp://lattes.cnpq.br/4654501431167414Enders, Michele Stéfani Peters1006000000006006006006006006006006004e7df89a-0ba0-4c75-958f-19ced0bb95c33d8918a4-ca98-478f-aed2-1dc867f02c2b554c6802-fa60-428b-831e-5bd7861206148fd7d402-38cb-487a-ae04-60b751dc48d63c621a6d-38be-4e61-b644-40b0cc92afcbf60c61ec-2b88-485f-8d1e-83d62038970d041d14df-2bfb-4de7-ba28-c81b80787eaereponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUIMICA_2019_ENDERS_MICHELE.pdfTES_PPGQUIMICA_2019_ENDERS_MICHELE.pdfTeseapplication/pdf4121524http://repositorio.ufsm.br/bitstream/1/21399/1/TES_PPGQUIMICA_2019_ENDERS_MICHELE.pdf03fac7ada3fbd97551c879ad0fa09ccfMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo |
dc.title.alternative.eng.fl_str_mv |
Methods for identification and quantification of salin species and sediments in crude oil |
title |
Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo |
spellingShingle |
Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo Enders, Michele Stéfani Peters Petróleo Microscopia eletrônica de varredura Teor de sedimentos Crude oil Scanning electron microscopy Sediment content CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo |
title_full |
Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo |
title_fullStr |
Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo |
title_full_unstemmed |
Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo |
title_sort |
Métodos analíticos para identificação e quantificação de espécies salinas e sedimentos em petróleo |
author |
Enders, Michele Stéfani Peters |
author_facet |
Enders, Michele Stéfani Peters |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Müller, Edson Irineu |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/5994311290376153 |
dc.contributor.advisor-co1.fl_str_mv |
Flores, Érico Marlon de Moraes |
dc.contributor.referee1.fl_str_mv |
Costa, Adilson Ben da |
dc.contributor.referee2.fl_str_mv |
Mortari, Sergio Roberto |
dc.contributor.referee3.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.referee4.fl_str_mv |
Dressler, Valderi Luiz |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/4654501431167414 |
dc.contributor.author.fl_str_mv |
Enders, Michele Stéfani Peters |
contributor_str_mv |
Müller, Edson Irineu Flores, Érico Marlon de Moraes Costa, Adilson Ben da Mortari, Sergio Roberto Duarte, Fábio Andrei Dressler, Valderi Luiz |
dc.subject.por.fl_str_mv |
Petróleo Microscopia eletrônica de varredura Teor de sedimentos |
topic |
Petróleo Microscopia eletrônica de varredura Teor de sedimentos Crude oil Scanning electron microscopy Sediment content CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Crude oil Scanning electron microscopy Sediment content |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, the ASTM D 4807 standard method combined with scanning electron microscopy (SEM) was used and evaluated for the identification of the morphology and composition of saline species present in sediments isolated from emulsions of Brazilian pre-salt crude oils. Modifications to ASTM D 4807 were evaluated in order to assess the amount of isolated sediments and the solubility of the saline species present on the membrane surface. The evaluated modifications were: (I) mixture composed of 50% toluene + 50% isopropanol (v / v) as solvent; (II) mixture of 50% toluene + 49.5% isopropanol + 0.5% water as solvent and (III) additional membrane washing step with hot water after filtration following ASTM D 4807. For the sediment content determination, membranes with porosity of 0.10 and 0.22 μm were used. Additionally, the saline species retained on the membranes with porosity 0.45, 0.22 and 0.10 μm after filtration according to ASTM D 4807 were solubilized in water for further Ca, Cl, Mg and Na determination by ICP OES. Using SEM, different structures of inorganic solids were identified on the membrane surface post filtration according to ASTM D 4807, among which cubic, spherical, star, rod and finely divided solids can be highlighted. Regarding sediment composition, the elements Na, Cl, Ca, Ba Fe, K, Mg, S, Si and Sr were identified in the sediments retained on the nylon membranes. ASTM D 4807 with modification I produced a reduction (greater than 50%) of sediment content when compared to the method without modification. The toluene + isopropanol mixture possibly minimized the crystallization of some inorganic solids, as there is an increase in the solubility of chloride containing salts in isopropanol when compared to toluene. Modification I allowed the isolation of a larger amount of crystalline structures in the form of “salt spheres”. Apparently, the presence of these structures appears to be related to the presence of isopropanol in the solvent mixture used in the filtration. Regarding modification II, a reduction in sediment content was also observed. The use of water in the solvent mixture allowed the partial solubilization of part of inorganic solids otherwise insoluble (using the unmodified method or modification I). When modification III was used, a reduction of more than 82% in the amount of inorganic solids retained on the membrane surface was observed. This indicates that the additional washing step using hot water allows the solubilization of nearly all soluble inorganic species present in the sediment retained on nylon membranes. After washing with water, the presence of water-insoluble salts, probably composed of alkaline earth elements of sulfates and carbonates, iron and silicates was detected on the membrane surface. When membranes with smaller porosity (0.10 and 0.22 μm) were used, no significant difference in sediment content was observed for most samples when compared to the 0.45 μm membrane. Thus, some experimental conditions proposed by ASTM D 4807, especially the type of solvent used, induce crystallization of saline species present in petroleum emulsions. These species are probably soluble in the aqueous phase of the emulsions and the use of ASTM D 4807 with toluene originates these solid species, which are retained on the membrane surface. This conclusion is corroborated by the fact that modifications I, II and III allowed a reduction in sediment content. |
publishDate |
2019 |
dc.date.issued.fl_str_mv |
2019-07-18 |
dc.date.accessioned.fl_str_mv |
2021-07-12T13:28:54Z |
dc.date.available.fl_str_mv |
2021-07-12T13:28:54Z |
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/1/21399 |
url |
http://repositorio.ufsm.br/handle/1/21399 |
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 |
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openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
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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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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
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UFSM |
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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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