Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo
Ano de defesa: | 2020 |
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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/1/29998 |
Resumo: | In this work, four sample preparation methods were investigated for further alkaline, alkaline earth metals and halogens determination in crude oil: i ) microwave assisted wet digestion using a pressurized digestion cavity (MAWD PDC), ii ), ultrasound assisted extraction (USAE), iii ) microwave assisted extraction (MAE) and iv ) reversed phase dispersive liquid liquid microextraction (RP DLLME). The results obtained after microwave assisted wet digestion (MAWD) and micr owave induced combustion (MIC) were used as reference values for developed methods (for metals and halogen determination, respectively). Additionally, two standard methods proposed by the American Society for Testing and Materials (ASTM D 5863 and D 6470, for metals and Cl, respectively) were applied. M etals determination was performed by using inductively coupled plasma optical emission spectrometry (ICP OES), the F was determined by ion chromatography (IC) and potentiometry using ion selective electrode ISE), the Cl was determined by inductively coupled plasma mass spectrometry (ICP MS), IC and by potentiometric titration, Br and I were determined by ICP MS. The methods were applied to five crude oil samples, which contained different physical and chemica l properties: API gravity (9.5 a 28.8), water content (0.2 a 79.9%) and sediment content (< 0.1 a 2.8%). Concerning USAE, independent of the experimental conditions used, it was observed that this method was not suitable for the separation of water emulsif ied in crude oil making unfeasible the determination of the elements. The MAWD PDC method showed a good performance for the decomposition of 1.2 g of heavy and medium crude oils using 8 mL of concentrated HNO 3 and 20 min of heating at 270 ºC. However, as e xpected, this method was only suitable for the subsequent determination of metals. In addition, a study related to the effect of carbon concentration (for ICP OES) on the determination of alkaline and alkaline earth metals was performed with digests contai ning 4 g L 1 of carbon from a digest obtained after the MAWD PDC. After the investigation, no interference was observed for any of the investigated elements. The MAE method was applied for the determination of alkaline and alkaline earth metals, as well as for Cl, Br and I in medium and heavy crude oil using 10 g of sample, 15 mL of water as extraction medium and 20 min of heating at 240 ºC. Using MAE, concordances greater than 90% were obtained compared to the reference values. The use of RP DLLME allowed the extraction of alkaline, alkaline earth metals (except Ba), Cl and Br in medium crude oil using only 0.5 mol L 1 HNO 3 . The MAE and RP DLLME methods allowed the use of a high sample mass (10 g), providing LOQs very low, in comparison with the MAWD PDC me thod, for example. In view of the applicability of the developed sample preparation methods, it is important to emphasize that the choice for each of them was dependent directly on intrinsic factors to each crude oil (API gravity sediment content and water content, for example), the elements to be determined, the analytical frequency and the instrumentation available in each laboratory. |
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2023-08-21T17:33:39Z2023-08-21T17:33:39Z2020-03-27http://repositorio.ufsm.br/handle/1/29998In this work, four sample preparation methods were investigated for further alkaline, alkaline earth metals and halogens determination in crude oil: i ) microwave assisted wet digestion using a pressurized digestion cavity (MAWD PDC), ii ), ultrasound assisted extraction (USAE), iii ) microwave assisted extraction (MAE) and iv ) reversed phase dispersive liquid liquid microextraction (RP DLLME). The results obtained after microwave assisted wet digestion (MAWD) and micr owave induced combustion (MIC) were used as reference values for developed methods (for metals and halogen determination, respectively). Additionally, two standard methods proposed by the American Society for Testing and Materials (ASTM D 5863 and D 6470, for metals and Cl, respectively) were applied. M etals determination was performed by using inductively coupled plasma optical emission spectrometry (ICP OES), the F was determined by ion chromatography (IC) and potentiometry using ion selective electrode ISE), the Cl was determined by inductively coupled plasma mass spectrometry (ICP MS), IC and by potentiometric titration, Br and I were determined by ICP MS. The methods were applied to five crude oil samples, which contained different physical and chemica l properties: API gravity (9.5 a 28.8), water content (0.2 a 79.9%) and sediment content (< 0.1 a 2.8%). Concerning USAE, independent of the experimental conditions used, it was observed that this method was not suitable for the separation of water emulsif ied in crude oil making unfeasible the determination of the elements. The MAWD PDC method showed a good performance for the decomposition of 1.2 g of heavy and medium crude oils using 8 mL of concentrated HNO 3 and 20 min of heating at 270 ºC. However, as e xpected, this method was only suitable for the subsequent determination of metals. In addition, a study related to the effect of carbon concentration (for ICP OES) on the determination of alkaline and alkaline earth metals was performed with digests contai ning 4 g L 1 of carbon from a digest obtained after the MAWD PDC. After the investigation, no interference was observed for any of the investigated elements. The MAE method was applied for the determination of alkaline and alkaline earth metals, as well as for Cl, Br and I in medium and heavy crude oil using 10 g of sample, 15 mL of water as extraction medium and 20 min of heating at 240 ºC. Using MAE, concordances greater than 90% were obtained compared to the reference values. The use of RP DLLME allowed the extraction of alkaline, alkaline earth metals (except Ba), Cl and Br in medium crude oil using only 0.5 mol L 1 HNO 3 . The MAE and RP DLLME methods allowed the use of a high sample mass (10 g), providing LOQs very low, in comparison with the MAWD PDC me thod, for example. In view of the applicability of the developed sample preparation methods, it is important to emphasize that the choice for each of them was dependent directly on intrinsic factors to each crude oil (API gravity sediment content and water content, for example), the elements to be determined, the analytical frequency and the instrumentation available in each laboratory.Neste trabalho foram investigados quatro métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino terrosos e halogênios em petróleo: i ) digestão por via úmida assistida por radiação micro ondas usando uma cavidade de digestão pressurizada (MAWD PDC), ii ) extração assistida por ultrassom (USAE), iii ) extração assistida por micro ondas (MAE) e iv ) microextração líquido líquido dispersiva em fase reversa (RP DLLME). Os resultados obtidos por digestão por via ú mida assistida por radi ação micro ondas (MAWD) e combustão iniciada por micro ondas (MIC) foram utilizados como valores de referência para os métodos de preparo de amostras desenvolvidos (para a determinação dos metais e halogênios, respectivamente). Adici onalmente, duas normas oficiais propostas pela American Society for Testing and Materials (ASTM D 5863 e D 6470, para metais e Cl, respectivamente) foram aplicadas. A determinação de metais foi feita por espectrometria de emissão óptica com plasma indutiva mente acoplado (ICP OES), F foi determinado por cromatografia de íons (IC) e eletrodo íon seletivo (ISE), Cl foi determinado por espectrometria de massa com plasma indutivamente acoplado (ICP MS), IC e titulação potenciométrica, Br e I foram determinados p or ICP MS. Os métodos foram aplicados para cinco amostras de petróleo, as quais continham diferentes propriedades físico químicas: ºAPI (9,5 a 28,8), teor de água (0,2 a 79,9%) e teor de sedimentos (< 0,1 a 2,8%). Com relação à USAE, independente das condi ções experimentais utilizadas, foi observado que este método não foi adequado para a separação da água emulsionada no petróleo inviabilizando a determinação dos elementos. O método MAWD-PDC apresentou bom desempenho para a decomposição de 1,2 g de petróleo pesado e médio usando 8 mL de HNO3 concentrado e 20 min de aquecimento, a 270 ºC. No entanto, como esperado, este método foi adequado apenas para a posterior determinação de metais. Adicionalmente, estudos relacionados ao efeito da concentração de carbon o na determinação de metais alcalinos e alcalino terrosos por ICP OES foram feitos a partir de digeridos contendo 4 g L 1 de carbono oriundo de um digerido obtido após a MAWD PDC. Após a investigação, não foram observadas interferências para nenhum dos ele mentos investigados. O método da MAE foi aplicado para a determinação de metais alcalinos e alcalino terrosos, bem como para Cl, Br e I em petróleo médio e pesado utilizando 10 g de amostra , 15 mL de água como meio extrator e 20 min de aquecimento a 240 ºC . Usando a MAE, concordâncias superiores à 90% foram obtidas em comparação com os valores de referência. O uso da RP DLLME permitiu a extração de metais alcalinos, alcalino terrosos (exceto o Ba), Cl e Br em petróleo médio utilizando apenas HNO 3 0,5 mol L 1 . Os métodos da MAE e RP DLLME permitiram o uso de elevada massa de amostra (10 g), fornecendo LOQs muito baixos, quando relacionados à MAWD PDC, por exemplo. Em vista da aplicabilidade dos métodos de preparo de amostras, é importante enfatizar que a escolha por cada um deles dependeu diretamente de fatores intrínsecos a cada petróleo (°API, teor de sedimentos, teor de água, por exemplo), os elementos a serem determinadas, a frequência analítica e a instrumentação disponível em cada laboratório.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade 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/openAccessPetróleoMetaisHalogêniosMAWD PDCMAERP DLLMECrude oilMetalsHalogensCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleoDevelopment of sample preparation methods for further determination of alkaline,alkaline-earth metalsand halogensin crude oilinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Picoloto, Rochele SogariRodrigues, Luiz FredericoMello, Paola de AzevedoBolzan, Rodrigo CardeiroDuarte, Fábio Andreihttp://lattes.cnpq.br/1963905835261695Nascimento, Mariele Samuel do100600000000600600600600600600600600a9c2788c-7913-4d7b-92e1-3429800ac0288c7eed4a-3935-4001-8d57-472fe198b9233cf6ce3f-79bb-41fc-a26d-232a194d51933989f67e-ae54-4740-88e3-bd1e6a4b2d88a33c2787-11dc-4032-8dda-91a38ea80867716ddc16-abf6-42d3-a1c9-a91c37ae7ac1474f025e-1dbf-4bf8-8613-ca00f4a20db4reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2020_NASCIMENTO_MARIELE.pdfTES_PPGQUÍMICA_2020_NASCIMENTO_MARIELE.pdfTese de doutoradoapplication/pdf2322072http://repositorio.ufsm.br/bitstream/1/29998/1/TES_PPGQU%c3%8dMICA_2020_NASCIMENTO_MARIELE.pdff25b4681ce845814961db354a1c874c2MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo |
dc.title.alternative.eng.fl_str_mv |
Development of sample preparation methods for further determination of alkaline,alkaline-earth metalsand halogensin crude oil |
title |
Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo |
spellingShingle |
Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo Nascimento, Mariele Samuel do Petróleo Metais Halogênios MAWD PDC MAE RP DLLME Crude oil Metals Halogens CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo |
title_full |
Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo |
title_fullStr |
Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo |
title_full_unstemmed |
Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo |
title_sort |
Desenvolvimento de métodos de preparo de amostras para a posterior determinação de metais alcalinos, alcalino-terrosos e halogênios em petróleo |
author |
Nascimento, Mariele Samuel do |
author_facet |
Nascimento, Mariele Samuel do |
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.advisor-co1.fl_str_mv |
Picoloto, Rochele Sogari |
dc.contributor.referee1.fl_str_mv |
Rodrigues, Luiz Frederico |
dc.contributor.referee2.fl_str_mv |
Mello, Paola de Azevedo |
dc.contributor.referee3.fl_str_mv |
Bolzan, Rodrigo Cardeiro |
dc.contributor.referee4.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/1963905835261695 |
dc.contributor.author.fl_str_mv |
Nascimento, Mariele Samuel do |
contributor_str_mv |
Flores, Érico Marlon de Moraes Picoloto, Rochele Sogari Rodrigues, Luiz Frederico Mello, Paola de Azevedo Bolzan, Rodrigo Cardeiro Duarte, Fábio Andrei |
dc.subject.por.fl_str_mv |
Petróleo Metais Halogênios MAWD PDC MAE RP DLLME |
topic |
Petróleo Metais Halogênios MAWD PDC MAE RP DLLME Crude oil Metals Halogens CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Crude oil Metals Halogens |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, four sample preparation methods were investigated for further alkaline, alkaline earth metals and halogens determination in crude oil: i ) microwave assisted wet digestion using a pressurized digestion cavity (MAWD PDC), ii ), ultrasound assisted extraction (USAE), iii ) microwave assisted extraction (MAE) and iv ) reversed phase dispersive liquid liquid microextraction (RP DLLME). The results obtained after microwave assisted wet digestion (MAWD) and micr owave induced combustion (MIC) were used as reference values for developed methods (for metals and halogen determination, respectively). Additionally, two standard methods proposed by the American Society for Testing and Materials (ASTM D 5863 and D 6470, for metals and Cl, respectively) were applied. M etals determination was performed by using inductively coupled plasma optical emission spectrometry (ICP OES), the F was determined by ion chromatography (IC) and potentiometry using ion selective electrode ISE), the Cl was determined by inductively coupled plasma mass spectrometry (ICP MS), IC and by potentiometric titration, Br and I were determined by ICP MS. The methods were applied to five crude oil samples, which contained different physical and chemica l properties: API gravity (9.5 a 28.8), water content (0.2 a 79.9%) and sediment content (< 0.1 a 2.8%). Concerning USAE, independent of the experimental conditions used, it was observed that this method was not suitable for the separation of water emulsif ied in crude oil making unfeasible the determination of the elements. The MAWD PDC method showed a good performance for the decomposition of 1.2 g of heavy and medium crude oils using 8 mL of concentrated HNO 3 and 20 min of heating at 270 ºC. However, as e xpected, this method was only suitable for the subsequent determination of metals. In addition, a study related to the effect of carbon concentration (for ICP OES) on the determination of alkaline and alkaline earth metals was performed with digests contai ning 4 g L 1 of carbon from a digest obtained after the MAWD PDC. After the investigation, no interference was observed for any of the investigated elements. The MAE method was applied for the determination of alkaline and alkaline earth metals, as well as for Cl, Br and I in medium and heavy crude oil using 10 g of sample, 15 mL of water as extraction medium and 20 min of heating at 240 ºC. Using MAE, concordances greater than 90% were obtained compared to the reference values. The use of RP DLLME allowed the extraction of alkaline, alkaline earth metals (except Ba), Cl and Br in medium crude oil using only 0.5 mol L 1 HNO 3 . The MAE and RP DLLME methods allowed the use of a high sample mass (10 g), providing LOQs very low, in comparison with the MAWD PDC me thod, for example. In view of the applicability of the developed sample preparation methods, it is important to emphasize that the choice for each of them was dependent directly on intrinsic factors to each crude oil (API gravity sediment content and water content, for example), the elements to be determined, the analytical frequency and the instrumentation available in each laboratory. |
publishDate |
2020 |
dc.date.issued.fl_str_mv |
2020-03-27 |
dc.date.accessioned.fl_str_mv |
2023-08-21T17:33:39Z |
dc.date.available.fl_str_mv |
2023-08-21T17:33:39Z |
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/1/29998 |
url |
http://repositorio.ufsm.br/handle/1/29998 |
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 |
a9c2788c-7913-4d7b-92e1-3429800ac028 8c7eed4a-3935-4001-8d57-472fe198b923 3cf6ce3f-79bb-41fc-a26d-232a194d5193 3989f67e-ae54-4740-88e3-bd1e6a4b2d88 a33c2787-11dc-4032-8dda-91a38ea80867 716ddc16-abf6-42d3-a1c9-a91c37ae7ac1 474f025e-1dbf-4bf8-8613-ca00f4a20db4 |
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 |
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http://repositorio.ufsm.br/bitstream/1/29998/1/TES_PPGQU%c3%8dMICA_2020_NASCIMENTO_MARIELE.pdf http://repositorio.ufsm.br/bitstream/1/29998/2/license_rdf http://repositorio.ufsm.br/bitstream/1/29998/3/license.txt |
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bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
|
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1794524309213937664 |