Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos
Ano de defesa: | 2010 |
---|---|
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
|
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
BR
|
Palavras-chave em Português: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/4201 |
Resumo: | Methods for fluorine (F) and chlorine (Cl) determination by molecular absorption spectrometry with graphite furnace vaporization and solid sampling (DSS-GF MAS) were developed. The developed methods were applied for F determination in coal and alumina and Cl determination in petroleum coke. As a preliminary treatment, the samples were grounded (<100 m, except to the alumina samples) and dried at temperatures ranging from 80 to 105 ºC. The determinations of F and Cl by DSS-GF MAS technique is based on the molecular absorption measures from the diatomic molecules AlF and AlCl, wich are generated in the vaporization step in the presence of an excess of Al in relation to F and Cl present in the sample. The furnace heating programs were optimized which consists of the following steps: drying (600 ºC for F and Cl), pyrolysis (F: 800 ºC, Cl: 700 ºC) and vaporization (F: 2300 ºC, Cl: 2100 ºC). The measurements of integrated absorbance were made at 227,5 nm for AlF and 261,4 nm for AlCl using hallow cathode lamps of Pt and Pb as radiation source, respectively. In order to prevent losses of F and Cl during the pyrolysis step, it is necessary the addition of chemical modifiers (10 Direct determination of halogen in alumina, coal and petroleum coke by gf mas with solid sampling Ba2+ for F and 20 g Sr2+ for Cl). The pyrolysis and vaporization temperatures for F and Cl were established with use of aqueous reference solutions and solid samples. By using the optimized conditions it was possible the determination of F and Cl based on the calibration with aqueous reference solutions. The accuracy of the methods was evaluated by analyzing certified reference materials and by comparison with results obtained by independent methods. No statistical significant difference at a confidence level of 95% was observed between results obtained and certified values or the results obtained by independent methods. The detection limits for F and Cl were 100 pg and 200 pg, respectively. Calibration curves were linear from 1 to 20 ng and from 20 to 80 ng (using mini-flow in the vaporization step) for F and from 1 to 25 ng for Cl. This is the first time that DSS-GF MAS was applied for F and Cl determination. Besides, the developed methods are simple to be applied to complex matrix for F and Cl determination due to the direct introduction of samples and by not requiring no prior stage of sample decomposition. |
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2017-05-152017-05-152010-01-27FLORES, éder Lisandro de Moraes. Direct determination of halogen in alumina, coal and petroleum coke by gf mas with solid sampling. 2010. 138 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010.http://repositorio.ufsm.br/handle/1/4201Methods for fluorine (F) and chlorine (Cl) determination by molecular absorption spectrometry with graphite furnace vaporization and solid sampling (DSS-GF MAS) were developed. The developed methods were applied for F determination in coal and alumina and Cl determination in petroleum coke. As a preliminary treatment, the samples were grounded (<100 m, except to the alumina samples) and dried at temperatures ranging from 80 to 105 ºC. The determinations of F and Cl by DSS-GF MAS technique is based on the molecular absorption measures from the diatomic molecules AlF and AlCl, wich are generated in the vaporization step in the presence of an excess of Al in relation to F and Cl present in the sample. The furnace heating programs were optimized which consists of the following steps: drying (600 ºC for F and Cl), pyrolysis (F: 800 ºC, Cl: 700 ºC) and vaporization (F: 2300 ºC, Cl: 2100 ºC). The measurements of integrated absorbance were made at 227,5 nm for AlF and 261,4 nm for AlCl using hallow cathode lamps of Pt and Pb as radiation source, respectively. In order to prevent losses of F and Cl during the pyrolysis step, it is necessary the addition of chemical modifiers (10 Direct determination of halogen in alumina, coal and petroleum coke by gf mas with solid sampling Ba2+ for F and 20 g Sr2+ for Cl). The pyrolysis and vaporization temperatures for F and Cl were established with use of aqueous reference solutions and solid samples. By using the optimized conditions it was possible the determination of F and Cl based on the calibration with aqueous reference solutions. The accuracy of the methods was evaluated by analyzing certified reference materials and by comparison with results obtained by independent methods. No statistical significant difference at a confidence level of 95% was observed between results obtained and certified values or the results obtained by independent methods. The detection limits for F and Cl were 100 pg and 200 pg, respectively. Calibration curves were linear from 1 to 20 ng and from 20 to 80 ng (using mini-flow in the vaporization step) for F and from 1 to 25 ng for Cl. This is the first time that DSS-GF MAS was applied for F and Cl determination. Besides, the developed methods are simple to be applied to complex matrix for F and Cl determination due to the direct introduction of samples and by not requiring no prior stage of sample decomposition.Neste trabalho foram desenvolvidos métodos para a determinação de flúor (F) e cloro (Cl) por espectrometria de absorção molecular com vaporização em forno de grafite com amostragem direta de sólidas (DSS-GF MAS). O método foi aplicado para a determinação de F em carvão mineral e alumina e Cl em coque de petróleo. Como tratamento prévio, as amostras foram cominuídas (<100 m exceto para alumina) e secadas a 80 e 105 ºC. A determinação de F e Cl pela técnica DSS-GF MAS é baseada na medição da absorção molecular das moléculas diatômicas AlF e AlCl formadas na etapa de vaporização pela adição prévia de excesso de Al em relação ao F e Cl contidos na amostra. Os programas de aquecimento ajustados do forno de grafite consistem nas etapas de secagem (600 ºC para F e Cl), pirólise (F: 800 ºC, Cl: 700 ºC) e vaporização (F: 2300 ºC, Cl: 2100 ºC). As medições da absorvância integrada são feitas a 227,5 nm para AlF e 261,4 nm para AlCl e como fonte de radiação foram usadas lâmpadas catodo oco de Pt e Pb, respectivamente. Para evitar perdas de F e Cl durante a etapa de pirólise, foi feita a adição de modificadores químicos (10 g Ba2+ para F e 20 g Sr2+ para Cl). As temperaturas de pirólise e vaporização para F e Cl foram estabelecidas com o emprego de soluções de referência aquosas e amostras sólidas. Foi possível a determinação de F e Cl nas amostras sólidas com calibração com soluções de referência aquosas. A exatidão foi avaliada pela comparação com valores de materiais de referência certificados e determinação por métodos independentes. Para as amostras sólidas analisadas não houve diferença significativa com um nível de confiança a 95%. Os limites de detecção foram de 100 pg para F e 200 pg para Cl. As intensidades de absorvância integrada foram lineares de 1 a 20 ng e 20 a 80 ng (com uso de mini-flow na vaporização) para F e de 1 a 25 ng para Cl. Os métodos desenvolvidos para F e Cl são caracterizados por serem inéditos quanto ao uso de DSS na de terminação por GF MAS e pela simplicidade, devido a possibilidade da introdução direta de amostras, não requerendo etapa de decomposição prévia.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaHalogêniosEspectrometria de absorção molecularAmostragem de sólidosCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidosDirect determination of halogen in alumina, coal and petroleum coke by gf mas with solid samplinginfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisDressler, Valderi Luizhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4723641Z7Barin, Juliano Smaniotohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4760000H0Bolzan, Rodrigo Cordeirohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4769083A1Mortari, Sergio Robertohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4721640J6Duarte, Fábio Andreihttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4777620A9http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4701043P4Flores, Éder Lisandro de Moraes10060000000040030030030030030030029c59cfe-a489-425c-88a5-18fdf7cbf258c0a4a6fd-50da-4b61-9a28-dafb44b9074ad879840d-dd75-40ca-b31c-925512af4b420b6036d2-a4c4-4565-bfc3-5fef0aae60609f6ffcda-3f02-4b6c-9f1f-03883c27e383474f025e-1dbf-4bf8-8613-ca00f4a20db4info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALFLORES, EDER LISANDRO DE MORAES.pdfapplication/pdf1574738http://repositorio.ufsm.br/bitstream/1/4201/1/FLORES%2c%20EDER%20LISANDRO%20DE%20MORAES.pdf139e4385d75b49ae1f1058d5f2396397MD51TEXTFLORES, EDER LISANDRO DE MORAES.pdf.txtFLORES, EDER LISANDRO DE MORAES.pdf.txtExtracted texttext/plain230303http://repositorio.ufsm.br/bitstream/1/4201/2/FLORES%2c%20EDER%20LISANDRO%20DE%20MORAES.pdf.txt6ed9f4464a5622ffe747eb790e8deb0dMD52THUMBNAILFLORES, EDER LISANDRO DE MORAES.pdf.jpgFLORES, EDER LISANDRO DE MORAES.pdf.jpgIM Thumbnailimage/jpeg5285http://repositorio.ufsm.br/bitstream/1/4201/3/FLORES%2c%20EDER%20LISANDRO%20DE%20MORAES.pdf.jpg4e4316ba8fb92169f5eb2bd2f2180126MD531/42012021-05-18 09:08:10.575oai:repositorio.ufsm.br:1/4201Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2021-05-18T12:08:10Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos |
dc.title.alternative.eng.fl_str_mv |
Direct determination of halogen in alumina, coal and petroleum coke by gf mas with solid sampling |
title |
Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos |
spellingShingle |
Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos Flores, Éder Lisandro de Moraes Halogênios Espectrometria de absorção molecular Amostragem de sólidos CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos |
title_full |
Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos |
title_fullStr |
Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos |
title_full_unstemmed |
Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos |
title_sort |
Determinação direta de halogênios em alumina, carvão e coque de petróleo por GF mas com amostragem de sólidos |
author |
Flores, Éder Lisandro de Moraes |
author_facet |
Flores, Éder Lisandro de Moraes |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Dressler, Valderi Luiz |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4723641Z7 |
dc.contributor.referee1.fl_str_mv |
Barin, Juliano Smanioto |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4760000H0 |
dc.contributor.referee2.fl_str_mv |
Bolzan, Rodrigo Cordeiro |
dc.contributor.referee2Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4769083A1 |
dc.contributor.referee3.fl_str_mv |
Mortari, Sergio Roberto |
dc.contributor.referee3Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4721640J6 |
dc.contributor.referee4.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.referee4Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4777620A9 |
dc.contributor.authorLattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4701043P4 |
dc.contributor.author.fl_str_mv |
Flores, Éder Lisandro de Moraes |
contributor_str_mv |
Dressler, Valderi Luiz Barin, Juliano Smanioto Bolzan, Rodrigo Cordeiro Mortari, Sergio Roberto Duarte, Fábio Andrei |
dc.subject.por.fl_str_mv |
Halogênios Espectrometria de absorção molecular Amostragem de sólidos |
topic |
Halogênios Espectrometria de absorção molecular Amostragem de sólidos CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Methods for fluorine (F) and chlorine (Cl) determination by molecular absorption spectrometry with graphite furnace vaporization and solid sampling (DSS-GF MAS) were developed. The developed methods were applied for F determination in coal and alumina and Cl determination in petroleum coke. As a preliminary treatment, the samples were grounded (<100 m, except to the alumina samples) and dried at temperatures ranging from 80 to 105 ºC. The determinations of F and Cl by DSS-GF MAS technique is based on the molecular absorption measures from the diatomic molecules AlF and AlCl, wich are generated in the vaporization step in the presence of an excess of Al in relation to F and Cl present in the sample. The furnace heating programs were optimized which consists of the following steps: drying (600 ºC for F and Cl), pyrolysis (F: 800 ºC, Cl: 700 ºC) and vaporization (F: 2300 ºC, Cl: 2100 ºC). The measurements of integrated absorbance were made at 227,5 nm for AlF and 261,4 nm for AlCl using hallow cathode lamps of Pt and Pb as radiation source, respectively. In order to prevent losses of F and Cl during the pyrolysis step, it is necessary the addition of chemical modifiers (10 Direct determination of halogen in alumina, coal and petroleum coke by gf mas with solid sampling Ba2+ for F and 20 g Sr2+ for Cl). The pyrolysis and vaporization temperatures for F and Cl were established with use of aqueous reference solutions and solid samples. By using the optimized conditions it was possible the determination of F and Cl based on the calibration with aqueous reference solutions. The accuracy of the methods was evaluated by analyzing certified reference materials and by comparison with results obtained by independent methods. No statistical significant difference at a confidence level of 95% was observed between results obtained and certified values or the results obtained by independent methods. The detection limits for F and Cl were 100 pg and 200 pg, respectively. Calibration curves were linear from 1 to 20 ng and from 20 to 80 ng (using mini-flow in the vaporization step) for F and from 1 to 25 ng for Cl. This is the first time that DSS-GF MAS was applied for F and Cl determination. Besides, the developed methods are simple to be applied to complex matrix for F and Cl determination due to the direct introduction of samples and by not requiring no prior stage of sample decomposition. |
publishDate |
2010 |
dc.date.issued.fl_str_mv |
2010-01-27 |
dc.date.accessioned.fl_str_mv |
2017-05-15 |
dc.date.available.fl_str_mv |
2017-05-15 |
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 |
FLORES, éder Lisandro de Moraes. Direct determination of halogen in alumina, coal and petroleum coke by gf mas with solid sampling. 2010. 138 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/4201 |
identifier_str_mv |
FLORES, éder Lisandro de Moraes. Direct determination of halogen in alumina, coal and petroleum coke by gf mas with solid sampling. 2010. 138 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010. |
url |
http://repositorio.ufsm.br/handle/1/4201 |
dc.language.iso.fl_str_mv |
por |
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por |
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100600000000 |
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400 300 300 300 300 300 300 |
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Universidade Federal de Santa Maria |
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UFSM |
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Universidade Federal de Santa Maria |
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