Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS
Autor(a) principal: | |
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Data de Publicação: | 2023 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Biblioteca Digital de Teses e Dissertações do UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/30519 |
Resumo: | In this work, three sample preparation methods were evaluated for the subsequent determination of rare earth elements (REE) in insects using inductively coupled plasma mass spectrometry (ICP-MS). To avoid possible interferences in the REE determination step, an ultrasonic nebulizer (USN) was coupled to the ICP-MS equipment. The methods evaluated were: i) microwave-assisted wet digestion (MAWD) with diluted acids, ii) microwave-assisted ultraviolet digestion (MAWD-UV) and iii) microwave-induced combustion (MIC). In MAWD, up to 500 mg of sample were decomposed with a heating time of 60 min and using 5 mol L-1 of HNO3 + 1 mL of 12 mol L-1 of HCl. For MAWD-UV, up to 500 mg of sample mass were decomposed with a heating time of 60 min using a solution of 3 mol L-1 of HNO3 + 1 mL of 12 mol L-1 of HCl. For MIC method, up to 500 mg of sample were digested with a heating program of 35 min and using aqua regia as absorbing solution. Three samples of edible crickets from China, Brazil and Thailand were used. To obtain reference values, the cricket samples were digested using the following methods: i) MAWD with 14.4 mol L-1 HNO3 and ii) conventional wet digestion in open system (CWD-OS). However, due to the relatively high limits of quantification (LOQs) obtained for CWD-OS, MAWD with 14.4 mol L-1 HNO3 was chosen as the reference method, allowing the comparison of a higher number of analytes for all samples. To evaluate the accuracy of the proposed methods, a certified reference material of mussel tissue (CRM BCR-668) was used. The results obtained for CRM, using the three proposed methods, showed no significant difference with the certified value (p > 0.05). The results obtained after the determination of the REE did not show significant difference (p > 0.05) between the three proposed methods and the reference method. During the evaluation of the methods, it was observed that only using HCl in the decomposition/absorbing solution it was possible to quantitatively retain the REE in solution, possibly due to the presence of insoluble species of these elements, which makes complete solubilization difficult when diluted HNO3 is used. MAWD and MAWD-UV allowed the use of diluted solutions and lower LOQs, while with MIC it was possible to decompose with shorter preparation time and lower carbon contents in solution (< 18.3 mg L-1 ). The limits of quantification (LOQs) obtained for the evaluated methods were relatively low: between 0.12 ng g-1 (Eu) and 21.8 ng g-1 (La) for MAWD, between 0.15 ng g-1 (Eu) and 37.3 ng g-1 (Ce) for MAWD-UV and between 1.58 ng g-1 (Eu) and 69.4 ng g -1 (Ce) for MIC. Finally, all three methods were suitable for the decomposition of up to 500 mg of cricket samples, enabling the determination of REE by USN-ICP-MS. |
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2023-11-16T19:22:12Z2023-11-16T19:22:12Z2023-08-11http://repositorio.ufsm.br/handle/1/30519In this work, three sample preparation methods were evaluated for the subsequent determination of rare earth elements (REE) in insects using inductively coupled plasma mass spectrometry (ICP-MS). To avoid possible interferences in the REE determination step, an ultrasonic nebulizer (USN) was coupled to the ICP-MS equipment. The methods evaluated were: i) microwave-assisted wet digestion (MAWD) with diluted acids, ii) microwave-assisted ultraviolet digestion (MAWD-UV) and iii) microwave-induced combustion (MIC). In MAWD, up to 500 mg of sample were decomposed with a heating time of 60 min and using 5 mol L-1 of HNO3 + 1 mL of 12 mol L-1 of HCl. For MAWD-UV, up to 500 mg of sample mass were decomposed with a heating time of 60 min using a solution of 3 mol L-1 of HNO3 + 1 mL of 12 mol L-1 of HCl. For MIC method, up to 500 mg of sample were digested with a heating program of 35 min and using aqua regia as absorbing solution. Three samples of edible crickets from China, Brazil and Thailand were used. To obtain reference values, the cricket samples were digested using the following methods: i) MAWD with 14.4 mol L-1 HNO3 and ii) conventional wet digestion in open system (CWD-OS). However, due to the relatively high limits of quantification (LOQs) obtained for CWD-OS, MAWD with 14.4 mol L-1 HNO3 was chosen as the reference method, allowing the comparison of a higher number of analytes for all samples. To evaluate the accuracy of the proposed methods, a certified reference material of mussel tissue (CRM BCR-668) was used. The results obtained for CRM, using the three proposed methods, showed no significant difference with the certified value (p > 0.05). The results obtained after the determination of the REE did not show significant difference (p > 0.05) between the three proposed methods and the reference method. During the evaluation of the methods, it was observed that only using HCl in the decomposition/absorbing solution it was possible to quantitatively retain the REE in solution, possibly due to the presence of insoluble species of these elements, which makes complete solubilization difficult when diluted HNO3 is used. MAWD and MAWD-UV allowed the use of diluted solutions and lower LOQs, while with MIC it was possible to decompose with shorter preparation time and lower carbon contents in solution (< 18.3 mg L-1 ). The limits of quantification (LOQs) obtained for the evaluated methods were relatively low: between 0.12 ng g-1 (Eu) and 21.8 ng g-1 (La) for MAWD, between 0.15 ng g-1 (Eu) and 37.3 ng g-1 (Ce) for MAWD-UV and between 1.58 ng g-1 (Eu) and 69.4 ng g -1 (Ce) for MIC. Finally, all three methods were suitable for the decomposition of up to 500 mg of cricket samples, enabling the determination of REE by USN-ICP-MS.Neste trabalho foram avaliados três métodos de preparo de amostras para a posterior determinação de elementos terras-raras (REE) em insetos comestíveis empregando a técnica de espectrometria de massa com plasma indutivamente acoplado (ICP-MS). Para contornar possíveis interferências na etapa de determinação dos REE, um nebulizador ultrassônico foi acoplado ao equipamento de ICP-MS. Os métodos avaliados, todos empregando soluções de ácidos diluídos com exceção da combustão iniciada por micro-ondas (MIC), foram: i) decomposição por via úmida assistida por radiação micro-ondas (MAWD), ii) decomposição por via úmida assistida por radiação micro-ondas e ultravioleta (MAWDUV) e iii) MIC. Na MAWD, 500 mg de amostra foram decompostos com um tempo de aquecimento de 60 min e solução de decomposição com HNO3 5 mol L-1 + 1 mL de HCl 12 mol L-1 . Na MAWD-UV, 500 mg de amostras foram decompostos com um tempo de aquecimento de 60 min empregando uma solução de decomposição com HNO3 3 mol L-1 + 1 mL de HCl 12 mol L-1 . Na MIC, até 500 mg de amostra foram decompostos em 35 min, usando água régia como solução absorvedora. Foram utilizadas três amostras de insetos comestíveis, provenientes da China, Brasil e Tailândia. Para a obtenção de valores de referência, as amostras de grilos foram decompostas empregando os seguintes métodos: i) MAWD com HNO3 14,4 mol L-1 e ii) decomposição por via úmida com aquecimento convencional em sistema aberto (CWD-OS). Porém, devido aos altos limites de quantificação (LOQs) obtidos para a CWD-OS, a MAWD com HNO3 14,4 mol L-1 foi escolhida como método de referência, possibilitando a comparação de um maior número de analitos para todas as amostras. Foi utilizado um material de referência certificado de tecido de mexilhão (CRM BCR-668) para avaliação da exatidão dos métodos propostos. Os resultados obtidos para o CRM, utilizando os três métodos propostos, não apresentaram diferença significativa com o valor certificado (p > 0,05). Os resultados obtidos após a determinação dos REE não apresentaram diferença significativa (p > 0,05) entre os três métodos propostos e o método de referência. Durante a avaliação dos métodos foi observado que somente com a presença de HCl na solução de decomposição/absorvedora foi possível a retenção quantitativa dos REE nos digeridos, possivelmente pela presença de espécies pouco solúveis destes elementos, o que dificulta a solubilização completa quando somente HNO3 diluído é utilizado. A MAWD e a MAWD-UV permitiram o uso de soluções diluídas e menores LOQs, enquanto com MIC foi possível a decomposição com menor tempo de preparo e menores teores de carbono em solução (< 18 mg L-1 ). Os limites de quantificação (LOQs) obtidos para os métodos avaliados foram relativamente baixos: entre 0,12 ng g-1 (Eu) e 22 ng g-1 (La) para a MAWD, entre 0,15 ng g-1 (Eu) e 37 ng g-1 (Ce) para MAWD-UV e entre 1,6 ng g-1 (Eu) e 69 ng g -1 (Ce) para a MIC. Por fim, os três métodos mostraram-se adequados para a decomposição de até 500 mg de amostras de grilos, possibilitando a determinação de REE por espectrometria de massa com plasma indutivamente acoplado com nebulizador ultrassônico (USN-ICP-MS).porUniversidade 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/openAccessDeterminação de elementos terras-rarasPreparo de amostrasAnálise de insetos comestíveisUSN-ICP-MSRare earth elements determinationSample preparationAnalysis of edible insectsCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAvaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MSEvaluation of sample preparation methods for the determination of rare earth elements in edible insects by USN-ICP-MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Silva, Jussiane Souza daDuarte, Fábio Andreihttp://lattes.cnpq.br/4433875881053191Rocha, João Lucas Kipper100600000000600600600600600a9c2788c-7913-4d7b-92e1-3429800ac028643b80c8-ae95-46ba-8d54-6d0d8d12d2733af0f519-51ea-4ebd-a63d-a1560feb47f97b2cc41c-5584-4228-a9bf-b1eb4d91e1e4reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2023_ROCHA_JOAO.pdfDIS_PPGQUIMICA_2023_ROCHA_JOAO.pdfDissertação de mestradoapplication/pdf1548904http://repositorio.ufsm.br/bitstream/1/30519/1/DIS_PPGQUIMICA_2023_ROCHA_JOAO.pdf5466df6a11e5cb0f34154c7b6f0a7343MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS |
dc.title.alternative.eng.fl_str_mv |
Evaluation of sample preparation methods for the determination of rare earth elements in edible insects by USN-ICP-MS |
title |
Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS |
spellingShingle |
Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS Rocha, João Lucas Kipper Determinação de elementos terras-raras Preparo de amostras Análise de insetos comestíveis USN-ICP-MS Rare earth elements determination Sample preparation Analysis of edible insects CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS |
title_full |
Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS |
title_fullStr |
Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS |
title_full_unstemmed |
Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS |
title_sort |
Avaliação de métodos de preparo de amostras para a determinação de elementos terras-raras em insetos comestíveis por USN-ICP-MS |
author |
Rocha, João Lucas Kipper |
author_facet |
Rocha, João Lucas Kipper |
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 |
Silva, Jussiane Souza da |
dc.contributor.referee2.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/4433875881053191 |
dc.contributor.author.fl_str_mv |
Rocha, João Lucas Kipper |
contributor_str_mv |
Flores, Érico Marlon de Moraes Silva, Jussiane Souza da Duarte, Fábio Andrei |
dc.subject.por.fl_str_mv |
Determinação de elementos terras-raras Preparo de amostras Análise de insetos comestíveis USN-ICP-MS |
topic |
Determinação de elementos terras-raras Preparo de amostras Análise de insetos comestíveis USN-ICP-MS Rare earth elements determination Sample preparation Analysis of edible insects CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Rare earth elements determination Sample preparation Analysis of edible insects |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, three sample preparation methods were evaluated for the subsequent determination of rare earth elements (REE) in insects using inductively coupled plasma mass spectrometry (ICP-MS). To avoid possible interferences in the REE determination step, an ultrasonic nebulizer (USN) was coupled to the ICP-MS equipment. The methods evaluated were: i) microwave-assisted wet digestion (MAWD) with diluted acids, ii) microwave-assisted ultraviolet digestion (MAWD-UV) and iii) microwave-induced combustion (MIC). In MAWD, up to 500 mg of sample were decomposed with a heating time of 60 min and using 5 mol L-1 of HNO3 + 1 mL of 12 mol L-1 of HCl. For MAWD-UV, up to 500 mg of sample mass were decomposed with a heating time of 60 min using a solution of 3 mol L-1 of HNO3 + 1 mL of 12 mol L-1 of HCl. For MIC method, up to 500 mg of sample were digested with a heating program of 35 min and using aqua regia as absorbing solution. Three samples of edible crickets from China, Brazil and Thailand were used. To obtain reference values, the cricket samples were digested using the following methods: i) MAWD with 14.4 mol L-1 HNO3 and ii) conventional wet digestion in open system (CWD-OS). However, due to the relatively high limits of quantification (LOQs) obtained for CWD-OS, MAWD with 14.4 mol L-1 HNO3 was chosen as the reference method, allowing the comparison of a higher number of analytes for all samples. To evaluate the accuracy of the proposed methods, a certified reference material of mussel tissue (CRM BCR-668) was used. The results obtained for CRM, using the three proposed methods, showed no significant difference with the certified value (p > 0.05). The results obtained after the determination of the REE did not show significant difference (p > 0.05) between the three proposed methods and the reference method. During the evaluation of the methods, it was observed that only using HCl in the decomposition/absorbing solution it was possible to quantitatively retain the REE in solution, possibly due to the presence of insoluble species of these elements, which makes complete solubilization difficult when diluted HNO3 is used. MAWD and MAWD-UV allowed the use of diluted solutions and lower LOQs, while with MIC it was possible to decompose with shorter preparation time and lower carbon contents in solution (< 18.3 mg L-1 ). The limits of quantification (LOQs) obtained for the evaluated methods were relatively low: between 0.12 ng g-1 (Eu) and 21.8 ng g-1 (La) for MAWD, between 0.15 ng g-1 (Eu) and 37.3 ng g-1 (Ce) for MAWD-UV and between 1.58 ng g-1 (Eu) and 69.4 ng g -1 (Ce) for MIC. Finally, all three methods were suitable for the decomposition of up to 500 mg of cricket samples, enabling the determination of REE by USN-ICP-MS. |
publishDate |
2023 |
dc.date.accessioned.fl_str_mv |
2023-11-16T19:22:12Z |
dc.date.available.fl_str_mv |
2023-11-16T19:22:12Z |
dc.date.issued.fl_str_mv |
2023-08-11 |
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/1/30519 |
url |
http://repositorio.ufsm.br/handle/1/30519 |
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 |
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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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MD5 MD5 MD5 |
repository.name.fl_str_mv |
Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
_version_ |
1801485251179970560 |