Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas
Ano de defesa: | 2018 |
---|---|
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/1/18731 |
Resumo: | In order to volatilize analytes from inorganic samples, additives such as microcrystalline cellulose have been applied. The cellulose is burnt and the heat generated helps to volatilize the analytes of the matrix being, later, recovered by the absorber solution. In the present work, a method was proposed for the volatilization of As, Cd, Hg and Pb in barium sulfate (BaSO4) using microwave-induced combustion (MIC) and subsequent element determination by inductively coupled plasma mass spectrometry (ICP-MS). BaSO4 samples were mixed with microcrystalline cellulose, homogenized and pressed into tablets. The following parameters related to the combustion procedure were evaluated: sample mass (300 to 700 mg), cellulose mass (300 to 900 mg), NH4Cl mass (300 to 600 mg), absorbing solution (3, 5, 7 and 14 mol L -1 of HNO3 and 25, 50 and 100% of inverse aqua regia) and reflux step (5 and 15 min). Reference values were obtained by using acid extraction method assisted by microwave radiation (MAE), using inverse aqua regia as the extractive solution. In addition, three steps of extractions were performed to ensure complete a extraction of the analytes. The most suitable condition for the volatilization method was 300 mg of sample, 600 mg of microcrystalline cellulose and 500 mg of NH4Cl, reflux for 5 min and a mixture of 5.5 mol L -1 of HNO3 with 1.5 mol L -1 HCl. In this condition the extracts presented a colorless appearance and a concentration of Ba at least 250 times lower then those when compared to MAE, thus avoiding problems of calibration of the spectrometer and formation of salt deposits in the cones of ICP-MS equipment. Thus, the main advantage of the proposed method is the separation of the analytes from the matrix, minimizing interferences in the determination step. In addition, when compared to the MAE method, the proposed methodology has the advantage of avoiding the use of concentrated acids for the preparation of BaSO4 samples. The quantification limits for As, Cd, Pb and Hg were 0.012; 0.001; 0.033 and 0.009 μg g -1, respectively (considering 300 mg of BaSO4 sample). Due to the unavailability of BaSO4 certified reference material or similar matrices, analyte addition assays were performed to assess the accuracy (95%). |
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2019-10-31T18:12:13Z2019-10-31T18:12:13Z2018-07-25http://repositorio.ufsm.br/handle/1/18731In order to volatilize analytes from inorganic samples, additives such as microcrystalline cellulose have been applied. The cellulose is burnt and the heat generated helps to volatilize the analytes of the matrix being, later, recovered by the absorber solution. In the present work, a method was proposed for the volatilization of As, Cd, Hg and Pb in barium sulfate (BaSO4) using microwave-induced combustion (MIC) and subsequent element determination by inductively coupled plasma mass spectrometry (ICP-MS). BaSO4 samples were mixed with microcrystalline cellulose, homogenized and pressed into tablets. The following parameters related to the combustion procedure were evaluated: sample mass (300 to 700 mg), cellulose mass (300 to 900 mg), NH4Cl mass (300 to 600 mg), absorbing solution (3, 5, 7 and 14 mol L -1 of HNO3 and 25, 50 and 100% of inverse aqua regia) and reflux step (5 and 15 min). Reference values were obtained by using acid extraction method assisted by microwave radiation (MAE), using inverse aqua regia as the extractive solution. In addition, three steps of extractions were performed to ensure complete a extraction of the analytes. The most suitable condition for the volatilization method was 300 mg of sample, 600 mg of microcrystalline cellulose and 500 mg of NH4Cl, reflux for 5 min and a mixture of 5.5 mol L -1 of HNO3 with 1.5 mol L -1 HCl. In this condition the extracts presented a colorless appearance and a concentration of Ba at least 250 times lower then those when compared to MAE, thus avoiding problems of calibration of the spectrometer and formation of salt deposits in the cones of ICP-MS equipment. Thus, the main advantage of the proposed method is the separation of the analytes from the matrix, minimizing interferences in the determination step. In addition, when compared to the MAE method, the proposed methodology has the advantage of avoiding the use of concentrated acids for the preparation of BaSO4 samples. The quantification limits for As, Cd, Pb and Hg were 0.012; 0.001; 0.033 and 0.009 μg g -1, respectively (considering 300 mg of BaSO4 sample). Due to the unavailability of BaSO4 certified reference material or similar matrices, analyte addition assays were performed to assess the accuracy (95%).Para que seja possível volatilizar os analitos de amostras inorgânicas, aditivos como a celulose microcristalina têm sido utilizados. Esta entra em combustão e o calor gerado ajuda a volatilizar os analitos da matriz sendo, posteriormente, retidos pela solução absorvedora. No presente trabalho foi proposto um método para a volatilização de As, Cd, Hg e Pb em sulfato de bário (BaSO4) empregando a combustão iniciada por micro-ondas (MIC) e posterior determinação elementar por espectrometria de massa com plasma indutivamente acoplado (ICP-MS). As amostras de BaSO4 foram misturadas com celulose microcristalina, homogeneizadas e prensadas na forma de comprimidos. Os seguintes parâmetros relacionados ao procedimento de combustão foram avaliados: massa de amostra (300 a 700 mg), massa de celulose (300 a 900 mg), massa de NH4Cl (300 a 600 mg), solução absorvedora (HNO3 3, 5, 7 e 14,4 mol L-1 e água régia invertida 25, 50 e 100%) e etapa de refluxo (5 e 15 min). Valores de referência foram obtidos empregando o método de extração ácida assistida por radiação micro-ondas (MAE), utilizando água régia invertida como solução extratora. Adicionalmente, foram realizadas extrações sequenciais para garantir a extração completa dos analitos. A condição mais adequada para o método de volatilização foi empregando 300 mg de amostra, 600 mg de celulose microcristalina e 500 mg de NH4Cl, refluxo de 5 min e uma mistura de 5,5 mol L-1 de HNO3 com 1,5 mol L-1 de HCl. Nessa condição os extratos obtidos apresentaram aspecto incolor e uma concentração de Ba pelo menos 250 vezes menor quando comparada aos extratos obtidos por MAE, evitando assim problemas de calibração do espectrômetro e formação de depósitos de sais nos cones do equipamento de ICP-MS. Desta forma, pode-se destacar como principal vantagem do método proposto a separação dos analitos da matriz, minimizando interferências na etapa de determinação. Além disso, quando comparado ao método de MAE, a metodologia proposta possui a vantagem de dispensar o uso de ácidos concentrados para o preparo de amostras de BaSO4. Os limites de quantificação para As, Cd, Pb e Hg foram 0,012; 0,001; 0,033 e 0,009 μg g-1, respectivamente (considerando 300 mg de amostra de BaSO4). Devido à indisponibilidade de material de referência certificado de amostra de BaSO4 ou matrizes semelhantes, ensaios de adição de analito foram realizados para avaliação da exatidão (95%).Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade 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/openAccessCombustão iniciada por micro-ondasProdutos farmacêuticosImpurezas elementaresPreparo de amostraSulfato de bárioUSPBarium sulfateElemental impuritiesMicrowave-induced combustionSample preparationCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondasVolatilization of elemental impurities in barium sulfate employing microwave-induced combustion for further determination by ICP-MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Barin, Juliano Smaniotohttp://lattes.cnpq.br/7545847424095994http://lattes.cnpq.br/9374513172714873Carvalho, Gabriel Severo de100600000000600a9c2788c-7913-4d7b-92e1-3429800ac0286ac6cc94-08c9-428f-b4c3-a608a0b35f46d879840d-dd75-40ca-b31c-925512af4b42reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2018_CARVALHO_GABRIEL.pdfDIS_PPGQUIMICA_2018_CARVALHO_GABRIEL.pdfDissertação de Mestradoapplication/pdf3339835http://repositorio.ufsm.br/bitstream/1/18731/1/DIS_PPGQUIMICA_2018_CARVALHO_GABRIEL.pdf2fff321be4866519a129573f04665addMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas |
dc.title.alternative.eng.fl_str_mv |
Volatilization of elemental impurities in barium sulfate employing microwave-induced combustion for further determination by ICP-MS |
title |
Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas |
spellingShingle |
Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas Carvalho, Gabriel Severo de Combustão iniciada por micro-ondas Produtos farmacêuticos Impurezas elementares Preparo de amostra Sulfato de bário USP Barium sulfate Elemental impurities Microwave-induced combustion Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas |
title_full |
Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas |
title_fullStr |
Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas |
title_full_unstemmed |
Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas |
title_sort |
Determinação de impurezas elementares em sulfato de bário por ICP-MS após volatilização empregando combustão iniciada por micro-ondas |
author |
Carvalho, Gabriel Severo de |
author_facet |
Carvalho, Gabriel Severo de |
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 |
Barin, Juliano Smanioto |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/7545847424095994 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/9374513172714873 |
dc.contributor.author.fl_str_mv |
Carvalho, Gabriel Severo de |
contributor_str_mv |
Flores, Érico Marlon de Moraes Barin, Juliano Smanioto |
dc.subject.por.fl_str_mv |
Combustão iniciada por micro-ondas Produtos farmacêuticos Impurezas elementares Preparo de amostra Sulfato de bário USP |
topic |
Combustão iniciada por micro-ondas Produtos farmacêuticos Impurezas elementares Preparo de amostra Sulfato de bário USP Barium sulfate Elemental impurities Microwave-induced combustion Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Barium sulfate Elemental impurities Microwave-induced combustion Sample preparation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In order to volatilize analytes from inorganic samples, additives such as microcrystalline cellulose have been applied. The cellulose is burnt and the heat generated helps to volatilize the analytes of the matrix being, later, recovered by the absorber solution. In the present work, a method was proposed for the volatilization of As, Cd, Hg and Pb in barium sulfate (BaSO4) using microwave-induced combustion (MIC) and subsequent element determination by inductively coupled plasma mass spectrometry (ICP-MS). BaSO4 samples were mixed with microcrystalline cellulose, homogenized and pressed into tablets. The following parameters related to the combustion procedure were evaluated: sample mass (300 to 700 mg), cellulose mass (300 to 900 mg), NH4Cl mass (300 to 600 mg), absorbing solution (3, 5, 7 and 14 mol L -1 of HNO3 and 25, 50 and 100% of inverse aqua regia) and reflux step (5 and 15 min). Reference values were obtained by using acid extraction method assisted by microwave radiation (MAE), using inverse aqua regia as the extractive solution. In addition, three steps of extractions were performed to ensure complete a extraction of the analytes. The most suitable condition for the volatilization method was 300 mg of sample, 600 mg of microcrystalline cellulose and 500 mg of NH4Cl, reflux for 5 min and a mixture of 5.5 mol L -1 of HNO3 with 1.5 mol L -1 HCl. In this condition the extracts presented a colorless appearance and a concentration of Ba at least 250 times lower then those when compared to MAE, thus avoiding problems of calibration of the spectrometer and formation of salt deposits in the cones of ICP-MS equipment. Thus, the main advantage of the proposed method is the separation of the analytes from the matrix, minimizing interferences in the determination step. In addition, when compared to the MAE method, the proposed methodology has the advantage of avoiding the use of concentrated acids for the preparation of BaSO4 samples. The quantification limits for As, Cd, Pb and Hg were 0.012; 0.001; 0.033 and 0.009 μg g -1, respectively (considering 300 mg of BaSO4 sample). Due to the unavailability of BaSO4 certified reference material or similar matrices, analyte addition assays were performed to assess the accuracy (95%). |
publishDate |
2018 |
dc.date.issued.fl_str_mv |
2018-07-25 |
dc.date.accessioned.fl_str_mv |
2019-10-31T18:12:13Z |
dc.date.available.fl_str_mv |
2019-10-31T18:12:13Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/18731 |
url |
http://repositorio.ufsm.br/handle/1/18731 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
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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 |
dc.source.none.fl_str_mv |
reponame:Biblioteca Digital de Teses e Dissertações do UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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Universidade Federal de Santa Maria (UFSM) |
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institution |
UFSM |
reponame_str |
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collection |
Biblioteca Digital de Teses e Dissertações do UFSM |
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