Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada
Ano de defesa: | 2017 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
Tipo de documento: | Dissertação |
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/1/18143 |
Resumo: | A method was developed to determine low molecular weight polycyclic aromatic hydrocarbons (naphthalene, anthracene, fluorantene, phenanthrene and acenaphthene) in aqueous leachates from soils and sediments using a salting-out assisted liquid-liquid extraction, synchronous fluorescence spectrometry and a multivariate calibration technique. Several experimental parameters were controlled and the optimum conditions were: sodium carbonate as the salting-out agent at concentration of 2 mol L-1, 3 mL of acetonitrile as extraction solvent, 6 mL of aqueous leachate, vortexing for 5 min and centrifuging at 4000 rpm for 5 min. The partial least squares calibration was optimized to the lowest values of root mean squared error and five latent variables were chosen for each of the targeted compounds. The regression coefficients for the true versus predicted concentrations were higher than 0.99. Figures of merit for the multivariate method were calculated, namely sensitivity, multivariate detection limit and multivariate quantification limit. The selectivity was also evaluated and other polycyclic aromatic hydrocarbons did not interfere in the analysis. Likewise, high performance liquid chromatography was used as a comparative methodology, and the regression analysis between the methods showed no statistical difference (t-test). The proposed methodology was applied to soils and sediments of a Brazilian river and the recoveries ranged from 74.3% to 105.8%. Overall, the proposed methodology was suitable for the targeted compounds, showing that the extraction method can be applied to spectrofluorometric analysis and that the multivariate calibration is also suitable for these compounds in leachates from real samples. Moreover, a proof of concept multivariate method to determine seven other polycyclic aromatic hydrocarbons (2-naphthol, hydroxypyrene, hydroxyfluorene, crysene, benzo(a)anthracene, benzo(b)fluoranthene and benzo(b)pyrene) was developed and its figure of merits were calculated. The built method had its prediction ability evaluated and it showed to be promising for application in real samples. |
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2019-09-04T21:50:00Z2019-09-04T21:50:00Z2017-01-31http://repositorio.ufsm.br/handle/1/18143A method was developed to determine low molecular weight polycyclic aromatic hydrocarbons (naphthalene, anthracene, fluorantene, phenanthrene and acenaphthene) in aqueous leachates from soils and sediments using a salting-out assisted liquid-liquid extraction, synchronous fluorescence spectrometry and a multivariate calibration technique. Several experimental parameters were controlled and the optimum conditions were: sodium carbonate as the salting-out agent at concentration of 2 mol L-1, 3 mL of acetonitrile as extraction solvent, 6 mL of aqueous leachate, vortexing for 5 min and centrifuging at 4000 rpm for 5 min. The partial least squares calibration was optimized to the lowest values of root mean squared error and five latent variables were chosen for each of the targeted compounds. The regression coefficients for the true versus predicted concentrations were higher than 0.99. Figures of merit for the multivariate method were calculated, namely sensitivity, multivariate detection limit and multivariate quantification limit. The selectivity was also evaluated and other polycyclic aromatic hydrocarbons did not interfere in the analysis. Likewise, high performance liquid chromatography was used as a comparative methodology, and the regression analysis between the methods showed no statistical difference (t-test). The proposed methodology was applied to soils and sediments of a Brazilian river and the recoveries ranged from 74.3% to 105.8%. Overall, the proposed methodology was suitable for the targeted compounds, showing that the extraction method can be applied to spectrofluorometric analysis and that the multivariate calibration is also suitable for these compounds in leachates from real samples. Moreover, a proof of concept multivariate method to determine seven other polycyclic aromatic hydrocarbons (2-naphthol, hydroxypyrene, hydroxyfluorene, crysene, benzo(a)anthracene, benzo(b)fluoranthene and benzo(b)pyrene) was developed and its figure of merits were calculated. The built method had its prediction ability evaluated and it showed to be promising for application in real samples.Um método foi desenvolvido para a determinação de hidrocarbonetos policíclicos aromáticos de baixo peso molecular (naftaleno, antraceno, fluoreno, acenafteno e fenantreno) em lixiviados aquosos de solos e sedimentos utilizando uma extração líquido-líquido assistida por salting-out, espectrometria de fluorescência síncrona e calibração multivariada. Diversos parâmetros experimentais foram controlados e as condições otimizadas foram: carbonato de sódio como agente de salting-out em concentração de 2 mol L-1, 3 mL de acetonitrila como solvente de extração, 6 mL de lixiviado aquoso, agitação com vórtex por 5 minutos e centrifugação a 4000 rotações por minutos por 5 minutos. A calibração por mínimos quadrados parciais foi otimizada para os menores valores da raiz do erro médio quadrático e cinco variáveis latentes foram escolhidas para cada um dos compostos de interesse. Os coeficientes de correlação para as concentrações preditas versus medida foram maiores que 0,99. Figuras de mérito para o método multivariado foram calculadas (sensibilidade, limite de detecção multivariado e limite de quantificação multivariado). A seletividade também foi avaliada e outros hidrocarbonetos policíclicos aromáticos não interferiram na análise. Além disto, cromatografia líquida de alta performance foi utilizada como um método de comparação e as análises de regressão entre os métodos não mostraram diferença estatística (teste t). O método proposto foi aplicado a solos e sedimentos do rio Xingú e as recuperações dos ensaios de fortificação foram de 74,3% a 105,8%. De maneira geral, o método proposto teve êxito na análise dos compostos de interesse, mostrando que o método de extração pode ser aplicado a análises espectrofluorimétricas e que a calibração multivariada também é aplicável a estes compostos em lixiviados de amostras reais. Ainda, um método de calibração multivariada como proof of concept foi desenvolvido para a determinação de outros sete hidrocarbonetos policíclicos aromáticos (2-naftol, hidroxipireno, hidroxifluoreno, criseno, benzo(a)antraceno, benzo(b)fluoranteno e benzo(b)pireno) e seus valores da raiz do erro médio quadrático foram utilizados para a escolha de sete variáveis latentes para a calibração. Os coeficientes de correlação entre as concentrações preditas versus medidas ficaram acima de 0,99. De maneira geral, este método se mostrou promissor a aplicações em amostras reais.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/openAccessHidrocarbonetos policíclicos aromáticosMetodologia de extraçãoMétodo multivariadoQuantificaçãoAmostras reaisPolycyclic aromatic hydrocarbonsExtraction methodologyMultivariate methodsQuantificationReal samplesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariadaPolycyclic aromatic hidrocarbons determination using multivariate calibrationinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisNascimento, Paulo Cícero dohttp://lattes.cnpq.br/7151513617218161Nascimento, Denise Bohrer dohttp://lattes.cnpq.br/9817093263802769Dias, Daianehttp://lattes.cnpq.br/1610292752294501http://lattes.cnpq.br/9179740187493517Bressan, Lucas Paines100600000000600578b51ed-b12f-4664-9b87-387ad073b32cbcaa42e0-d78d-4958-9160-1c98fad00a106b8b95ca-db02-4fbf-80ea-848fdb5e586e278565d5-d7b0-49cd-94d1-7224a97540c8reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2017_BRESSAN_LUCAS.pdfDIS_PPGQUIMICA_2017_BRESSAN_LUCAS.pdfDissertação de Mestradoapplication/pdf5789298http://repositorio.ufsm.br/bitstream/1/18143/1/DIS_PPGQUIMICA_2017_BRESSAN_LUCAS.pdf562d12f680e3db1c23bc83d8d806a529MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada |
dc.title.alternative.eng.fl_str_mv |
Polycyclic aromatic hidrocarbons determination using multivariate calibration |
title |
Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada |
spellingShingle |
Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada Bressan, Lucas Paines Hidrocarbonetos policíclicos aromáticos Metodologia de extração Método multivariado Quantificação Amostras reais Polycyclic aromatic hydrocarbons Extraction methodology Multivariate methods Quantification Real samples CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada |
title_full |
Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada |
title_fullStr |
Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada |
title_full_unstemmed |
Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada |
title_sort |
Determinação de hidrocarbonetos policíclicos aromáticos utilizando calibração multivariada |
author |
Bressan, Lucas Paines |
author_facet |
Bressan, Lucas Paines |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Nascimento, Paulo Cícero do |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/7151513617218161 |
dc.contributor.referee1.fl_str_mv |
Nascimento, Denise Bohrer do |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/9817093263802769 |
dc.contributor.referee2.fl_str_mv |
Dias, Daiane |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/1610292752294501 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/9179740187493517 |
dc.contributor.author.fl_str_mv |
Bressan, Lucas Paines |
contributor_str_mv |
Nascimento, Paulo Cícero do Nascimento, Denise Bohrer do Dias, Daiane |
dc.subject.por.fl_str_mv |
Hidrocarbonetos policíclicos aromáticos Metodologia de extração Método multivariado Quantificação Amostras reais |
topic |
Hidrocarbonetos policíclicos aromáticos Metodologia de extração Método multivariado Quantificação Amostras reais Polycyclic aromatic hydrocarbons Extraction methodology Multivariate methods Quantification Real samples CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Polycyclic aromatic hydrocarbons Extraction methodology Multivariate methods Quantification Real samples |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
A method was developed to determine low molecular weight polycyclic aromatic hydrocarbons (naphthalene, anthracene, fluorantene, phenanthrene and acenaphthene) in aqueous leachates from soils and sediments using a salting-out assisted liquid-liquid extraction, synchronous fluorescence spectrometry and a multivariate calibration technique. Several experimental parameters were controlled and the optimum conditions were: sodium carbonate as the salting-out agent at concentration of 2 mol L-1, 3 mL of acetonitrile as extraction solvent, 6 mL of aqueous leachate, vortexing for 5 min and centrifuging at 4000 rpm for 5 min. The partial least squares calibration was optimized to the lowest values of root mean squared error and five latent variables were chosen for each of the targeted compounds. The regression coefficients for the true versus predicted concentrations were higher than 0.99. Figures of merit for the multivariate method were calculated, namely sensitivity, multivariate detection limit and multivariate quantification limit. The selectivity was also evaluated and other polycyclic aromatic hydrocarbons did not interfere in the analysis. Likewise, high performance liquid chromatography was used as a comparative methodology, and the regression analysis between the methods showed no statistical difference (t-test). The proposed methodology was applied to soils and sediments of a Brazilian river and the recoveries ranged from 74.3% to 105.8%. Overall, the proposed methodology was suitable for the targeted compounds, showing that the extraction method can be applied to spectrofluorometric analysis and that the multivariate calibration is also suitable for these compounds in leachates from real samples. Moreover, a proof of concept multivariate method to determine seven other polycyclic aromatic hydrocarbons (2-naphthol, hydroxypyrene, hydroxyfluorene, crysene, benzo(a)anthracene, benzo(b)fluoranthene and benzo(b)pyrene) was developed and its figure of merits were calculated. The built method had its prediction ability evaluated and it showed to be promising for application in real samples. |
publishDate |
2017 |
dc.date.issued.fl_str_mv |
2017-01-31 |
dc.date.accessioned.fl_str_mv |
2019-09-04T21:50:00Z |
dc.date.available.fl_str_mv |
2019-09-04T21:50:00Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
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masterThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/18143 |
url |
http://repositorio.ufsm.br/handle/1/18143 |
dc.language.iso.fl_str_mv |
por |
language |
por |
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100600000000 |
dc.relation.confidence.fl_str_mv |
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 |
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