Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas
Autor(a) principal: | |
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Data de Publicação: | 2008 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
dARK ID: | ark:/26339/001300000p618 |
Texto Completo: | http://repositorio.ufsm.br/handle/1/4162 |
Resumo: | The microwave-induced combustion (MIC) method was applied for coal and petroleum coke digestion for further determination of bromine, chlorine, fluorine and iodine by ion chromatography (IC). Samples (up to 500 mg) were combusted at 20 bar of oxygen and analytes were absorbed either in water or (NH4)2CO3 (10 to 50 mmol l-1) solutions. A reflux step was applied to improve analyte absorption. Accuracy was evaluated for Br, Cl, F and I using coal and coke certified reference materials as well as using spike recoveries. For Br, Cl and F the agreement was from 96 to 103% using 50 mmol l-1 (NH4)2CO3 as absorbing solution and reflux step. For I, recoveries were higher than 97%. Bromine, Cl and I were also determined in MIC digests by inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma optical emission spectrometry (ICP OES), and F by ion selective electrode (ISE) with agreement higher than 95% to the values obtained using IC. The procedure was also compared with wet digestion procedure for coal and petroleum coke, as well as with procedures of extraction using different solutions. Neverthless, the results were always lower than those obtained using MIC. Temperature during combustion was higher than 1350 and 1500 ºC for coal and petroleum coke, respectively, and the residual carbon content was lower than 1%. Using MIC technique up to eight samples may be simultaneously processed and a single absorbing solution may be suitable for all analytes and determination techniques. The limits of detection (LODs, 3s) using the proposed MIC-IC method were 2.5, 0.8, 0.25 e 3.0 mg g-1, respectively. Additionally, the same MIC procedure was applied for food sample digestion for further iodine determination by ICP-MS. Using MIC technique the LOD for iodine by ICP-MS was 0.001 mg g-1 and the agreement with certified values for iodine in food were higher than 96% for all analyzed samples. |
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Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondasDetermination of halogens in coal, petroleum coke and food after microwave induced combustionQuímicaQuímica analíticaHalogêniosCombustãoCarvãoCoque petroquímicoMicroondasCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAThe microwave-induced combustion (MIC) method was applied for coal and petroleum coke digestion for further determination of bromine, chlorine, fluorine and iodine by ion chromatography (IC). Samples (up to 500 mg) were combusted at 20 bar of oxygen and analytes were absorbed either in water or (NH4)2CO3 (10 to 50 mmol l-1) solutions. A reflux step was applied to improve analyte absorption. Accuracy was evaluated for Br, Cl, F and I using coal and coke certified reference materials as well as using spike recoveries. For Br, Cl and F the agreement was from 96 to 103% using 50 mmol l-1 (NH4)2CO3 as absorbing solution and reflux step. For I, recoveries were higher than 97%. Bromine, Cl and I were also determined in MIC digests by inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma optical emission spectrometry (ICP OES), and F by ion selective electrode (ISE) with agreement higher than 95% to the values obtained using IC. The procedure was also compared with wet digestion procedure for coal and petroleum coke, as well as with procedures of extraction using different solutions. Neverthless, the results were always lower than those obtained using MIC. Temperature during combustion was higher than 1350 and 1500 ºC for coal and petroleum coke, respectively, and the residual carbon content was lower than 1%. Using MIC technique up to eight samples may be simultaneously processed and a single absorbing solution may be suitable for all analytes and determination techniques. The limits of detection (LODs, 3s) using the proposed MIC-IC method were 2.5, 0.8, 0.25 e 3.0 mg g-1, respectively. Additionally, the same MIC procedure was applied for food sample digestion for further iodine determination by ICP-MS. Using MIC technique the LOD for iodine by ICP-MS was 0.001 mg g-1 and the agreement with certified values for iodine in food were higher than 96% for all analyzed samples.Conselho Nacional de Desenvolvimento Científico e TecnológicoO método de combustão iniciada por microondas (MIC) foi aplicado para a decomposição de carvão e coque de petróleo para posterior determinação de Br, Cl, F e I por cromatografia de íons (IC). Foram decompostas até 500 mg de amostra usando 20 bar de oxigênio e os analitos foram absorvidos em água ou soluções de 10 a 50 mmol l-1 de (NH4)2CO3. Uma etapa de refluxo foi aplicada para aumentar a eficiência de absorção dos analitos. A exatidão do procedimento proposto foi avaliada para Br, Cl, F e I usando material de referência certificado (CRM) de carvão e coque de petróleo e, também, por meio de ensaios de recuperação. Para Br, Cl e F as concordâncias com os valores certificados foram de 96 a 103% usando 50 mmol l-1 de (NH4)2CO3 como solução absorvedora e aplicando a etapa de refluxo. Para I, a recuperação foi superior a 97%. Bromo, Cl e I também foram determinados por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) e espectrometria de massa com plasma indutivamente acoplado (ICP-MS) e F foi determinado por eletrodo íon seletivo (ISE). As concordâncias com os valores determinados por IC foram superiores a 95% para todos os analitos. O procedimento foi comparado, também, com procedimentos de decomposição por via úmida e de extração dos halogênios utilizando diferentes soluções extratoras. Contudo, os resultados foram sempre inferiores aos obtidos empregando MIC. A temperatura atingida durante a combustão de carvão e coque de petróleo foi superior a 1350 e 1500 ºC, respectivamente. O teor de carbono residual (RCC) nos digeridos foi inferior a 1%. Usando MIC podem ser decompostas simultaneamente até oito amostras e, uma única solução absorvedora pode ser utilizada para todos os halogênios em ambas as matrizes. Os limites de detecção (LODs, 3s, n=10) por IC foram 2,5, 0,8, 0,25 e 3,0 mg g-1 para Br, Cl, F e I, respectivamente. Adicionalmente, o mesmo procedimento por MIC, foi aplicado para a decomposição de amostras de alimentos para a determinação subseqüente de I por ICP-MS. Usando o método de decomposição por MIC, o LOD obtido para I por ICP-MS foi de 0,001 mg g-1 e a concordância com os valores certificados para I em amostras de alimentos foi superior a 96%.Universidade Federal de Santa MariaBRQuímicaUFSMPrograma de Pós-Graduação em QuímicaFlores, Érico Marlon de Moraeshttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4782125T8Krug, Francisco Joséhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4783058Y5Korn, Maria das Gracas Andradehttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4767631E2Zanella, Renatohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9Paniz, José Neri Gottfriedhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4701043Z3Mesko, Márcia Foster2017-05-192017-05-192008-03-14info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfapplication/pdfMESKO, Márcia Foster. Determination of halogens in coal, petroleum coke and food after microwave induced combustion. 2008. 156 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008.http://repositorio.ufsm.br/handle/1/4162ark:/26339/001300000p618porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2017-07-27T16:09:43Zoai:repositorio.ufsm.br:1/4162Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2017-07-27T16:09:43Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas Determination of halogens in coal, petroleum coke and food after microwave induced combustion |
title |
Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas |
spellingShingle |
Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas Mesko, Márcia Foster Química Química analítica Halogênios Combustão Carvão Coque petroquímico Microondas CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas |
title_full |
Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas |
title_fullStr |
Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas |
title_full_unstemmed |
Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas |
title_sort |
Determinação de halogênios em carvão, coque petroquímico e alimentos após combustão iniciada por microondas |
author |
Mesko, Márcia Foster |
author_facet |
Mesko, Márcia Foster |
author_role |
author |
dc.contributor.none.fl_str_mv |
Flores, Érico Marlon de Moraes http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4782125T8 Krug, Francisco José http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4783058Y5 Korn, Maria das Gracas Andrade http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4767631E2 Zanella, Renato http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9 Paniz, José Neri Gottfried http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4701043Z3 |
dc.contributor.author.fl_str_mv |
Mesko, Márcia Foster |
dc.subject.por.fl_str_mv |
Química Química analítica Halogênios Combustão Carvão Coque petroquímico Microondas CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
topic |
Química Química analítica Halogênios Combustão Carvão Coque petroquímico Microondas CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The microwave-induced combustion (MIC) method was applied for coal and petroleum coke digestion for further determination of bromine, chlorine, fluorine and iodine by ion chromatography (IC). Samples (up to 500 mg) were combusted at 20 bar of oxygen and analytes were absorbed either in water or (NH4)2CO3 (10 to 50 mmol l-1) solutions. A reflux step was applied to improve analyte absorption. Accuracy was evaluated for Br, Cl, F and I using coal and coke certified reference materials as well as using spike recoveries. For Br, Cl and F the agreement was from 96 to 103% using 50 mmol l-1 (NH4)2CO3 as absorbing solution and reflux step. For I, recoveries were higher than 97%. Bromine, Cl and I were also determined in MIC digests by inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma optical emission spectrometry (ICP OES), and F by ion selective electrode (ISE) with agreement higher than 95% to the values obtained using IC. The procedure was also compared with wet digestion procedure for coal and petroleum coke, as well as with procedures of extraction using different solutions. Neverthless, the results were always lower than those obtained using MIC. Temperature during combustion was higher than 1350 and 1500 ºC for coal and petroleum coke, respectively, and the residual carbon content was lower than 1%. Using MIC technique up to eight samples may be simultaneously processed and a single absorbing solution may be suitable for all analytes and determination techniques. The limits of detection (LODs, 3s) using the proposed MIC-IC method were 2.5, 0.8, 0.25 e 3.0 mg g-1, respectively. Additionally, the same MIC procedure was applied for food sample digestion for further iodine determination by ICP-MS. Using MIC technique the LOD for iodine by ICP-MS was 0.001 mg g-1 and the agreement with certified values for iodine in food were higher than 96% for all analyzed samples. |
publishDate |
2008 |
dc.date.none.fl_str_mv |
2008-03-14 2017-05-19 2017-05-19 |
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 |
MESKO, Márcia Foster. Determination of halogens in coal, petroleum coke and food after microwave induced combustion. 2008. 156 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008. http://repositorio.ufsm.br/handle/1/4162 |
dc.identifier.dark.fl_str_mv |
ark:/26339/001300000p618 |
identifier_str_mv |
MESKO, Márcia Foster. Determination of halogens in coal, petroleum coke and food after microwave induced combustion. 2008. 156 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008. ark:/26339/001300000p618 |
url |
http://repositorio.ufsm.br/handle/1/4162 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Química UFSM Programa de Pós-Graduação em Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Química UFSM Programa de Pós-Graduação em Química |
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 |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
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1815172374718316544 |