Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares
Ano de defesa: | 2020 |
---|---|
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/1/23096 |
Resumo: | An alternative system for solid sampling and element determination by heated tube coupled to flame atomic absorption spectrometry was developed for the determination of Cd, Co, Mo, Ni and Pb in high purity graphite and carbon nanotubes (CNTs). Three quartz systems were developed and evaluated: without atomizer tube (system A) and with atomizer tube, being one of them of 80 mm of length without slit (system B) and other with the same length and with a 80 mm slit (system C) that allow the flame inlet. Two electrodes were positioned in the system and were connected to an external device, to generate an electric discharge which was responsible to ignite the samples. Samples were introduced in the system, with ethanol as auxiliary reagent to start the combustion before the generation of arch discharge between electrodes, in the presence of a constant O2 flow, that was responsible to react with organic matrix producing CO2 as main product and driving the gaseous products of combustion with the analytes to the atomizer tube. The system B was the most suitable having a quartz atomizer tube connected to a perpendicular tube (“T” shape). This atomizer tube was positioned over the spectrometer flame and acted as an atom trap to increase the atomic density in front of the optical beam, reducing the limits of detections (LODs). The following parameters were investigated to optimize the system: flame stoichiometry of air/acetylene (620/100, 565/100, 430/100 and 400/120 L h-1), distance between atomizer tube and burner (3, 6, 9, 12 e 15 mm), O2 flow-rate (0.3, 0.5, 1.0 and 2.0 L min-1), linear calibration range and the sample mass influence in the determination. The calibration was performed by matrix matching, being added the analyte to a high purity graphite, used as a standard, and the results were statistically compared with reference values obtained by inductively coupled plasma optical emission spectrometry (ICP-OES) and by inductively coupled plasma mass spectrometry (ICP-MS) before decomposition of samples by microwave-induced combustion (MIC). The proposed method allows the introduction of up 50 mg of solid sample, without a sample decomposition for the determination of Cd, Ni and Pb in graphite and CNTs. Low LODs were achieved for the SS-FF AAS system (between 0.107 and 4.20 μg g-1), allowing the determination of analytes at low concentrations. Moreover, the proposed method agreed with several recommendations of green analytical chemistry as reduced sample pre-treatment, low sample consumption, no use of toxic reagents for sample preparation, low residues generation (basically CO2), low electric energy consumption and relatively safety for the analyst. |
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2021-12-01T19:07:11Z2021-12-01T19:07:11Z2020-01-25http://repositorio.ufsm.br/handle/1/23096An alternative system for solid sampling and element determination by heated tube coupled to flame atomic absorption spectrometry was developed for the determination of Cd, Co, Mo, Ni and Pb in high purity graphite and carbon nanotubes (CNTs). Three quartz systems were developed and evaluated: without atomizer tube (system A) and with atomizer tube, being one of them of 80 mm of length without slit (system B) and other with the same length and with a 80 mm slit (system C) that allow the flame inlet. Two electrodes were positioned in the system and were connected to an external device, to generate an electric discharge which was responsible to ignite the samples. Samples were introduced in the system, with ethanol as auxiliary reagent to start the combustion before the generation of arch discharge between electrodes, in the presence of a constant O2 flow, that was responsible to react with organic matrix producing CO2 as main product and driving the gaseous products of combustion with the analytes to the atomizer tube. The system B was the most suitable having a quartz atomizer tube connected to a perpendicular tube (“T” shape). This atomizer tube was positioned over the spectrometer flame and acted as an atom trap to increase the atomic density in front of the optical beam, reducing the limits of detections (LODs). The following parameters were investigated to optimize the system: flame stoichiometry of air/acetylene (620/100, 565/100, 430/100 and 400/120 L h-1), distance between atomizer tube and burner (3, 6, 9, 12 e 15 mm), O2 flow-rate (0.3, 0.5, 1.0 and 2.0 L min-1), linear calibration range and the sample mass influence in the determination. The calibration was performed by matrix matching, being added the analyte to a high purity graphite, used as a standard, and the results were statistically compared with reference values obtained by inductively coupled plasma optical emission spectrometry (ICP-OES) and by inductively coupled plasma mass spectrometry (ICP-MS) before decomposition of samples by microwave-induced combustion (MIC). The proposed method allows the introduction of up 50 mg of solid sample, without a sample decomposition for the determination of Cd, Ni and Pb in graphite and CNTs. Low LODs were achieved for the SS-FF AAS system (between 0.107 and 4.20 μg g-1), allowing the determination of analytes at low concentrations. Moreover, the proposed method agreed with several recommendations of green analytical chemistry as reduced sample pre-treatment, low sample consumption, no use of toxic reagents for sample preparation, low residues generation (basically CO2), low electric energy consumption and relatively safety for the analyst.Um sistema alternativo de introdução direta de amostras sólidas para a posterior determinação elementar por espectrometria de absorção atômica com tubo aquecido na chama (SS-FF AAS) foi desenvolvido, para a determinação de Cd, Co, Mo Ni e Pb em grafite de alta pureza e nanotubos de carbono (CNTs). Foram avaliados três sistemas confeccionados em quartzo: sem tubo atomizador (sistema A) e com tubo atomizador, sendo um deles de 80 mm de comprimento sem fenda (sistema B) e o outro tubo de mesmo comprimento, com uma fenda de 80 mm para entrada da chama (sistema C). Dois eletrodos foram posicionados no sistema avaliado, ligados a um dispositivo externo, para gerar um arco elétrico que daria ignição nas amostras. As amostras foram introduzidas no sistema, contendo etanol como reagente auxiliar para iniciar combustão e a ignição foi feita através de um arco elétrico gerado entre os dois eletrodos, na presença de vazão constante de O2 que, além de reagir com a matéria orgânica gerando majoritariamente CO2, também conduz os vapores da combustão juntamente com os analitos para o tubo atomizador, para a atomização e absorção atômica. O sistema B foi o mais adequado e consistiu em um dispositivo único confeccionado em quartzo, o qual era composto por tubo principal por onde a amostra era conduzida, conectado perpendicularmente a outro tubo formando um “T”. Este tubo perpendicular foi posicionado sobre a chama do espectrômetro de FAAS e atuou como tubo atomizador e aprisionador de átomos (atom trap) para aumentar a densidade atômica em frente ao feixe óptico, melhorando a sensibilidade da técnica e reduzindo os limites de detecção (LDs). Os seguintes parâmetros foram avaliados para otimização do sistema: estequiometria de chama ar/acetileno (620/100, 565/100, 430/100 e 400/120 L h-1), distância entre o queimador e o tubo atomizador (3, 6, 9, 12 e 15 mm), vazão de O2 (0,3, 0,5, 1,0 e 2,0 L min-1), faixa linear de calibração e a influência da massa de amostra. A calibração foi feita empregando a adição de analito sobre a grafite descontaminada, que serviu de carreador dos analitos. Os resultados da SS-FF AAS foram comparados estatisticamente com os valores dos métodos usados como referência, obtidos por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP-OES) e por espectrometria de massa com plasma indutivamente acoplado (ICP-MS) após a decomposição das amostras por combustão iniciada por micro-ondas (MIC). O método proposto permitiu a introdução de até 50 mg de amostra sólida, para a determinação de Cd, Ni e Pb em amostras de grafite e nanotubos de carbono. Foram obtidos baixos valores de LDs para o sistema SS-FF AAS (entre 0,107 e 4,20 μg g-1), viabilizando a determinação dos analitos em baixas concentrações. Além disso, o método proposto está em concordância com diversas recomendações da química analítica verde como a determinação dos analitos em amostra sólida (minimizando a etapa de pré-tratamento), baixo consumo de amostra, sem a necessidade do uso de reagentes tóxicos para o preparo de amostra, pequena geração de resíduos (majoritariamente CO2), baixo consumo de energia, além de ser um método relativamente seguro para o operador.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/openAccessEspectrometria de absorção atômica com chamaAmostragem de sólidosDeterminação elementarGrafiteNanotubos de carbonoSS-FF AASFlame atomic absorption spectrometrySolid sampleElemental determinationGraphiteCarbon nanotubesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementaresDevelopment and aplication of a system based on eletric discharge for SS-FF AAS for further elemental impurities determinationinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Costa, Adilson Ben daBizzi, Cezar AugustoDuarte, Fábio AndreiRodrigues, Luiz Fredericohttp://lattes.cnpq.br/1622139696944992Santos, Rafael Francisco dos100600000000600600600600600a9c2788c-7913-4d7b-92e1-3429800ac028095f67f5-092e-4e39-b0d2-facdced6bdab8fd7d402-38cb-487a-ae04-60b751dc48d6ea5d5aeb-956d-4091-b711-982595b3e995f60c61ec-2b88-485f-8d1e-83d62038970dcfa9ea52-18b4-42b0-8233-4f4ebcf879fareponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUIMICA_2020_SANTOS_RAFAEL.pdfTES_PPGQUIMICA_2020_SANTOS_RAFAEL.pdfTese de Doutoradoapplication/pdf2889315http://repositorio.ufsm.br/bitstream/1/23096/1/TES_PPGQUIMICA_2020_SANTOS_RAFAEL.pdf2731f5b30cad31ef24534f5fd70d773fMD51LICENSElicense.txtlicense.txttext/plain; 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dc.title.por.fl_str_mv |
Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares |
dc.title.alternative.eng.fl_str_mv |
Development and aplication of a system based on eletric discharge for SS-FF AAS for further elemental impurities determination |
title |
Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares |
spellingShingle |
Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares Santos, Rafael Francisco dos Espectrometria de absorção atômica com chama Amostragem de sólidos Determinação elementar Grafite Nanotubos de carbono SS-FF AAS Flame atomic absorption spectrometry Solid sample Elemental determination Graphite Carbon nanotubes CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares |
title_full |
Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares |
title_fullStr |
Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares |
title_full_unstemmed |
Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares |
title_sort |
Desenvolvimento e aplicação de um sistema com arco elétrico para SS-FF AAS para a determinação de impurezas elementares |
author |
Santos, Rafael Francisco dos |
author_facet |
Santos, Rafael Francisco dos |
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 |
Costa, Adilson Ben da |
dc.contributor.referee2.fl_str_mv |
Bizzi, Cezar Augusto |
dc.contributor.referee3.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.referee4.fl_str_mv |
Rodrigues, Luiz Frederico |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/1622139696944992 |
dc.contributor.author.fl_str_mv |
Santos, Rafael Francisco dos |
contributor_str_mv |
Flores, Érico Marlon de Moraes Costa, Adilson Ben da Bizzi, Cezar Augusto Duarte, Fábio Andrei Rodrigues, Luiz Frederico |
dc.subject.por.fl_str_mv |
Espectrometria de absorção atômica com chama Amostragem de sólidos Determinação elementar Grafite Nanotubos de carbono SS-FF AAS |
topic |
Espectrometria de absorção atômica com chama Amostragem de sólidos Determinação elementar Grafite Nanotubos de carbono SS-FF AAS Flame atomic absorption spectrometry Solid sample Elemental determination Graphite Carbon nanotubes CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Flame atomic absorption spectrometry Solid sample Elemental determination Graphite Carbon nanotubes |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
An alternative system for solid sampling and element determination by heated tube coupled to flame atomic absorption spectrometry was developed for the determination of Cd, Co, Mo, Ni and Pb in high purity graphite and carbon nanotubes (CNTs). Three quartz systems were developed and evaluated: without atomizer tube (system A) and with atomizer tube, being one of them of 80 mm of length without slit (system B) and other with the same length and with a 80 mm slit (system C) that allow the flame inlet. Two electrodes were positioned in the system and were connected to an external device, to generate an electric discharge which was responsible to ignite the samples. Samples were introduced in the system, with ethanol as auxiliary reagent to start the combustion before the generation of arch discharge between electrodes, in the presence of a constant O2 flow, that was responsible to react with organic matrix producing CO2 as main product and driving the gaseous products of combustion with the analytes to the atomizer tube. The system B was the most suitable having a quartz atomizer tube connected to a perpendicular tube (“T” shape). This atomizer tube was positioned over the spectrometer flame and acted as an atom trap to increase the atomic density in front of the optical beam, reducing the limits of detections (LODs). The following parameters were investigated to optimize the system: flame stoichiometry of air/acetylene (620/100, 565/100, 430/100 and 400/120 L h-1), distance between atomizer tube and burner (3, 6, 9, 12 e 15 mm), O2 flow-rate (0.3, 0.5, 1.0 and 2.0 L min-1), linear calibration range and the sample mass influence in the determination. The calibration was performed by matrix matching, being added the analyte to a high purity graphite, used as a standard, and the results were statistically compared with reference values obtained by inductively coupled plasma optical emission spectrometry (ICP-OES) and by inductively coupled plasma mass spectrometry (ICP-MS) before decomposition of samples by microwave-induced combustion (MIC). The proposed method allows the introduction of up 50 mg of solid sample, without a sample decomposition for the determination of Cd, Ni and Pb in graphite and CNTs. Low LODs were achieved for the SS-FF AAS system (between 0.107 and 4.20 μg g-1), allowing the determination of analytes at low concentrations. Moreover, the proposed method agreed with several recommendations of green analytical chemistry as reduced sample pre-treatment, low sample consumption, no use of toxic reagents for sample preparation, low residues generation (basically CO2), low electric energy consumption and relatively safety for the analyst. |
publishDate |
2020 |
dc.date.issued.fl_str_mv |
2020-01-25 |
dc.date.accessioned.fl_str_mv |
2021-12-01T19:07:11Z |
dc.date.available.fl_str_mv |
2021-12-01T19:07:11Z |
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/1/23096 |
url |
http://repositorio.ufsm.br/handle/1/23096 |
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 |
dc.relation.authority.fl_str_mv |
a9c2788c-7913-4d7b-92e1-3429800ac028 095f67f5-092e-4e39-b0d2-facdced6bdab 8fd7d402-38cb-487a-ae04-60b751dc48d6 ea5d5aeb-956d-4091-b711-982595b3e995 f60c61ec-2b88-485f-8d1e-83d62038970d cfa9ea52-18b4-42b0-8233-4f4ebcf879fa |
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 |
bitstream.url.fl_str_mv |
http://repositorio.ufsm.br/bitstream/1/23096/1/TES_PPGQUIMICA_2020_SANTOS_RAFAEL.pdf http://repositorio.ufsm.br/bitstream/1/23096/3/license.txt http://repositorio.ufsm.br/bitstream/1/23096/2/license_rdf http://repositorio.ufsm.br/bitstream/1/23096/4/TES_PPGQUIMICA_2020_SANTOS_RAFAEL.pdf.txt http://repositorio.ufsm.br/bitstream/1/23096/5/TES_PPGQUIMICA_2020_SANTOS_RAFAEL.pdf.jpg |
bitstream.checksum.fl_str_mv |
2731f5b30cad31ef24534f5fd70d773f 2f0571ecee68693bd5cd3f17c1e075df 4460e5956bc1d1639be9ae6146a50347 3f20666b4cb0c8bac37c1d67bb0a5632 4628e79a88b60c9d7d5357e140c741dc |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 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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1794524307504758784 |