Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS)
Autor(a) principal: | |
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Data de Publicação: | 2019 |
Tipo de documento: | Tese |
Idioma: | eng |
Título da fonte: | Repositório Institucional da UFSCAR |
Texto Completo: | https://repositorio.ufscar.br/handle/ufscar/11842 |
Resumo: | This doctoral thesis proposes sample preparation combined with the use of laser-induced breakdown spectroscopy (LIBS) for analysis of difficult-to-mineralize samples focusing on the analytical development of LIBS as well as for the development of sample preparation for the technique. The LIBS technique consists of focusing a laser pulse with high fluence (> GW s-1) under the surface of a sample. Following the incidence of this laser pulse, atoms are vaporized, atomized, ionized and brought into an excited energy state. When atoms and ions return to their lowest energy levels, they release photons of specific wavelengths that are translated into the electromagnetic spectrum. The technique has inherent challenges in the analysis of solid samples, which are mostly its applications, such as microheterogeneity and high limits of detection (LOD). Although the technique has great ability in solid sample analysis, it can also be used for liquid sample analysis, however, some specific problems arise, such as sample splashing with laser pulse impact and low reproducibility, and sample preparation can help minimize them. As goal, the present thesis focuses on the development of sample preparation of nickel ores, solder masks and sunscreens for analysis of elements of interest in each of the presented samples. The strategy for the analysis of nickel ore and sunscreen samples consisted of converting the matrix of liquid to solid in order to minimize the problems inherent to liquid analysis by LIBS. For this, polyvinyl alcohol (PVA), a water-soluble polymer, was used. For solder masks, the samples were completely dried on glass support for further analysis. Chemometric tools were used during the work to aid in data processing (normalization), exploratory analysis (PCA (principal component analysis)) and univariate and multivariate calibration (PCR (principal component regression), PLS (partial least squares), MLR (multiple linear regression)). |
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Sperança, Marco AurelioPereira Filho, Edenir Rodrigueshttp://lattes.cnpq.br/3394181280355442http://lattes.cnpq.br/5905694821382851d138e1fb-bcd7-4edf-ac6d-f1795a2b2d2f2019-09-17T13:05:03Z2019-09-17T13:05:03Z2019-08-27SPERANÇA, Marco Aurelio. Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS). 2019. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2019. Disponível em: https://repositorio.ufscar.br/handle/ufscar/11842.https://repositorio.ufscar.br/handle/ufscar/11842This doctoral thesis proposes sample preparation combined with the use of laser-induced breakdown spectroscopy (LIBS) for analysis of difficult-to-mineralize samples focusing on the analytical development of LIBS as well as for the development of sample preparation for the technique. The LIBS technique consists of focusing a laser pulse with high fluence (> GW s-1) under the surface of a sample. Following the incidence of this laser pulse, atoms are vaporized, atomized, ionized and brought into an excited energy state. When atoms and ions return to their lowest energy levels, they release photons of specific wavelengths that are translated into the electromagnetic spectrum. The technique has inherent challenges in the analysis of solid samples, which are mostly its applications, such as microheterogeneity and high limits of detection (LOD). Although the technique has great ability in solid sample analysis, it can also be used for liquid sample analysis, however, some specific problems arise, such as sample splashing with laser pulse impact and low reproducibility, and sample preparation can help minimize them. As goal, the present thesis focuses on the development of sample preparation of nickel ores, solder masks and sunscreens for analysis of elements of interest in each of the presented samples. The strategy for the analysis of nickel ore and sunscreen samples consisted of converting the matrix of liquid to solid in order to minimize the problems inherent to liquid analysis by LIBS. For this, polyvinyl alcohol (PVA), a water-soluble polymer, was used. For solder masks, the samples were completely dried on glass support for further analysis. Chemometric tools were used during the work to aid in data processing (normalization), exploratory analysis (PCA (principal component analysis)) and univariate and multivariate calibration (PCR (principal component regression), PLS (partial least squares), MLR (multiple linear regression)).Esta tese de doutorado propõe preparos de amostra aliados a utilização da técnica espectroanalítica de emissão atômica induzida por laser (laser-induced breakdown spectroscopy, LIBS) para análise de amostras de difícil mineralização com foco no desenvolvimento analítico da LIBS bem como para o desenvolvimento de preparo de amostras para a técnica. A técnica LIBS consiste na focalização de um pulso de laser com alta fluência (> GW s-1) sob a superfície de uma amostra. Após a incidência desse laser, os átomos são vaporizados, atomizados, ionizados e levados a um estado de energia excitado. Quando átomos e íons retornam aos seus níveis energéticos mais baixos liberam fótons com comprimentos de onda específicos que são traduzidos em espectro eletromagnético. A técnica possui desafios inerentes à análise de amostras sólidas, que são majoritariamente suas aplicações, como microheterogeneidade e altos limites de detecção (LOD). Apesar da técnica possuir grande habilidade na análise de amostras sólidas, pode também ser usada para análise de amostras líquidas, no entanto, alguns problemas específicos surgem, como espalhamento da amostra com o impacto do pulso de laser e baixa reprodutibilidade, e o preparo das amostras pode ajudar a minimizá-los. Como objetivo, a presente tese se concentra no desenvolvimento de preparo de amostras de minério de níquel, máscara de solda e protetores solares para análise de elementos de interesse em cada uma das amostras apresentadas. A estratégia para análise de amostras de minério de níquel e protetor solar consistiu na conversão da matriz de líquido para sólido no intuito de minimizar os problemas inerentes à análise de líquidos por LIBS, para isso, álcool poli vinílico (PVA), polímero hidrossolúvel, foi utilizado. Para máscaras de solda, as amostras foram totalmente secas em suporte de vidro para posterior análise. Ferramentas quimiométricas foram utilizadas durante o trabalho para auxílio do tratamento de dados (normalizações), análise exploratória (PCA (principal component analysis)) e calibração uni e multivariada (PCR (principal component regression), PLS (partial least squares), MLR (multiple linear regression)).Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)CNPq: 160152/2015-1CAPES: Código de Financiamento 001engUniversidade Federal de São CarlosCâmpus São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarCC0 1.0 Universalhttp://creativecommons.org/publicdomain/zero/1.0/info:eu-repo/semantics/openAccessLIBSQuiomiometriaAmostras líquidasPreparo de amostrasProtetor solarMáscara de soldaMinério de níquelChemometricsLiquid samplesSample preparationSunscreenSolder maskNickel oreCIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS)Development of sample preparation procedures for difficult-to-mineralize samples for direct analysis by laser-induced breakdown spectroscopy (LIBS)info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesis600600cc86aeec-dd0e-4a5e-9ae0-d3a038091433reponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINALtese_MAS_vfinal.pdftese_MAS_vfinal.pdfTexto integral da teseapplication/pdf4431477https://repositorio.ufscar.br/bitstream/ufscar/11842/1/tese_MAS_vfinal.pdf71a496f81316bb5d07b80ca59c2d82f9MD51cartahomologacao_pos2.pdfcartahomologacao_pos2.pdfCarta comprovante assinada pelo orientadorapplication/pdf333237https://repositorio.ufscar.br/bitstream/ufscar/11842/3/cartahomologacao_pos2.pdf6d1e50603a5b4e4fbcd6b6af29b37313MD53CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8701https://repositorio.ufscar.br/bitstream/ufscar/11842/4/license_rdf42fd4ad1e89814f5e4a476b409eb708cMD54TEXTtese_MAS_vfinal.pdf.txttese_MAS_vfinal.pdf.txtExtracted texttext/plain156093https://repositorio.ufscar.br/bitstream/ufscar/11842/5/tese_MAS_vfinal.pdf.txt07bc845e6820d919de14aa75d9a5410bMD55cartahomologacao_pos2.pdf.txtcartahomologacao_pos2.pdf.txtExtracted texttext/plain1477https://repositorio.ufscar.br/bitstream/ufscar/11842/7/cartahomologacao_pos2.pdf.txt1a5728f7fb3fb0e108577fde42e09471MD57THUMBNAILtese_MAS_vfinal.pdf.jpgtese_MAS_vfinal.pdf.jpgIM Thumbnailimage/jpeg15762https://repositorio.ufscar.br/bitstream/ufscar/11842/6/tese_MAS_vfinal.pdf.jpgf0d76460ee04e44f867bb61a0371e0f5MD56cartahomologacao_pos2.pdf.jpgcartahomologacao_pos2.pdf.jpgIM Thumbnailimage/jpeg11888https://repositorio.ufscar.br/bitstream/ufscar/11842/8/cartahomologacao_pos2.pdf.jpgabb48b5607d552c0e19c6f5b1c570bbbMD58ufscar/118422023-09-18 18:31:44.602oai:repositorio.ufscar.br:ufscar/11842Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-09-18T18:31:44Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false |
dc.title.por.fl_str_mv |
Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS) |
dc.title.alternative.eng.fl_str_mv |
Development of sample preparation procedures for difficult-to-mineralize samples for direct analysis by laser-induced breakdown spectroscopy (LIBS) |
title |
Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS) |
spellingShingle |
Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS) Sperança, Marco Aurelio LIBS Quiomiometria Amostras líquidas Preparo de amostras Protetor solar Máscara de solda Minério de níquel Chemometrics Liquid samples Sample preparation Sunscreen Solder mask Nickel ore CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS) |
title_full |
Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS) |
title_fullStr |
Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS) |
title_full_unstemmed |
Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS) |
title_sort |
Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS) |
author |
Sperança, Marco Aurelio |
author_facet |
Sperança, Marco Aurelio |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/5905694821382851 |
dc.contributor.author.fl_str_mv |
Sperança, Marco Aurelio |
dc.contributor.advisor1.fl_str_mv |
Pereira Filho, Edenir Rodrigues |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/3394181280355442 |
dc.contributor.authorID.fl_str_mv |
d138e1fb-bcd7-4edf-ac6d-f1795a2b2d2f |
contributor_str_mv |
Pereira Filho, Edenir Rodrigues |
dc.subject.por.fl_str_mv |
LIBS Quiomiometria Amostras líquidas Preparo de amostras Protetor solar Máscara de solda Minério de níquel |
topic |
LIBS Quiomiometria Amostras líquidas Preparo de amostras Protetor solar Máscara de solda Minério de níquel Chemometrics Liquid samples Sample preparation Sunscreen Solder mask Nickel ore CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Chemometrics Liquid samples Sample preparation Sunscreen Solder mask Nickel ore |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
This doctoral thesis proposes sample preparation combined with the use of laser-induced breakdown spectroscopy (LIBS) for analysis of difficult-to-mineralize samples focusing on the analytical development of LIBS as well as for the development of sample preparation for the technique. The LIBS technique consists of focusing a laser pulse with high fluence (> GW s-1) under the surface of a sample. Following the incidence of this laser pulse, atoms are vaporized, atomized, ionized and brought into an excited energy state. When atoms and ions return to their lowest energy levels, they release photons of specific wavelengths that are translated into the electromagnetic spectrum. The technique has inherent challenges in the analysis of solid samples, which are mostly its applications, such as microheterogeneity and high limits of detection (LOD). Although the technique has great ability in solid sample analysis, it can also be used for liquid sample analysis, however, some specific problems arise, such as sample splashing with laser pulse impact and low reproducibility, and sample preparation can help minimize them. As goal, the present thesis focuses on the development of sample preparation of nickel ores, solder masks and sunscreens for analysis of elements of interest in each of the presented samples. The strategy for the analysis of nickel ore and sunscreen samples consisted of converting the matrix of liquid to solid in order to minimize the problems inherent to liquid analysis by LIBS. For this, polyvinyl alcohol (PVA), a water-soluble polymer, was used. For solder masks, the samples were completely dried on glass support for further analysis. Chemometric tools were used during the work to aid in data processing (normalization), exploratory analysis (PCA (principal component analysis)) and univariate and multivariate calibration (PCR (principal component regression), PLS (partial least squares), MLR (multiple linear regression)). |
publishDate |
2019 |
dc.date.accessioned.fl_str_mv |
2019-09-17T13:05:03Z |
dc.date.available.fl_str_mv |
2019-09-17T13:05:03Z |
dc.date.issued.fl_str_mv |
2019-08-27 |
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.citation.fl_str_mv |
SPERANÇA, Marco Aurelio. Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS). 2019. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2019. Disponível em: https://repositorio.ufscar.br/handle/ufscar/11842. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/11842 |
identifier_str_mv |
SPERANÇA, Marco Aurelio. Desenvolvimento de procedimentos de preparo de amostras de difícil mineralização para análise direta por laser-induced breakdown spectroscopy (LIBS). 2019. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2019. Disponível em: https://repositorio.ufscar.br/handle/ufscar/11842. |
url |
https://repositorio.ufscar.br/handle/ufscar/11842 |
dc.language.iso.fl_str_mv |
eng |
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eng |
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Universidade Federal de São Carlos Câmpus São Carlos |
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Programa de Pós-Graduação em Química - PPGQ |
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UFSCar |
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Universidade Federal de São Carlos Câmpus São Carlos |
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