Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS
Ano de defesa: | 2017 |
---|---|
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: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/13873 |
Resumo: | In this work a method for the digestion of high ash content coal (>30%) using a high pressure asher (HPA) system for further determination of platinum group elements (PGEs) by inductively coupled plasma mass spectrometry (ICP-MS) was developed. The efficiency of coal digestion with was evaluated by the residual carbon content (RCC), being evaluated solutions of HNO3 + HCl (3+1, v/v) and (1+1, v/v). About 500 mg of coal were digested in HPA system using 6 mL of HNO3 + HCl (3+1, v/v) and time of heating of 20, 40 and 60 min at 320 ºC. Due to the very low concentrations of these elements in the coal sample used in this work, the coal sample was enriched with PGEs and digested at the same conditions. To evaluate the accuracy, coal was digested by microwave induced combustion (MIC) and also by microwave-assisted wet digestion (MAWD). The MIC procedure was evaluated using 6 mL of HNO3 + HCl (3+1, v/v), (1+1, v/v) and (1+3, v/v) and pellets with 500 mg of coal. The addition of 300 mg of NH4Cl to the coal pellets was also evaluated by the MIC. For the MAWD were used 150 mg of coal and 4.5 mL of 14.4 mol L-1 HNO3, 1.0 mL of 12 mol L-1 HCl and 1.5 mL of 23 mol L-1 HF. During the development of this work, a study of interferences for PGEs (Cu, Hf, Rb, Sr, Y and Zn, possible interferences for 193Ir, 105Pd, 195Pt, 103Rh and 101Ru) was performed. The determination of Os was difficult due to the formation of OsO4 during the digestion process, remaining in the nebulizer chamber of the ICP-MS. Generally, the digestion of enriched coal in HPA system presented satisfactory results when compared with MIC and MAWD. It was possible to digest up to 500 mg of coal with 6 mL of HNO3 + HCl (3+1, v/v) in HPA system. Recoveries between 100 and 127% were obtained for PGEs, except for Os, where errors over 350% were observed. RCC values in coal digested by HPA system were less than 40%. Limits of quantification were between 0.19 and 3.91 ng g-1. |
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2018-07-20T19:20:35Z2018-07-20T19:20:35Z2017-06-03http://repositorio.ufsm.br/handle/1/13873In this work a method for the digestion of high ash content coal (>30%) using a high pressure asher (HPA) system for further determination of platinum group elements (PGEs) by inductively coupled plasma mass spectrometry (ICP-MS) was developed. The efficiency of coal digestion with was evaluated by the residual carbon content (RCC), being evaluated solutions of HNO3 + HCl (3+1, v/v) and (1+1, v/v). About 500 mg of coal were digested in HPA system using 6 mL of HNO3 + HCl (3+1, v/v) and time of heating of 20, 40 and 60 min at 320 ºC. Due to the very low concentrations of these elements in the coal sample used in this work, the coal sample was enriched with PGEs and digested at the same conditions. To evaluate the accuracy, coal was digested by microwave induced combustion (MIC) and also by microwave-assisted wet digestion (MAWD). The MIC procedure was evaluated using 6 mL of HNO3 + HCl (3+1, v/v), (1+1, v/v) and (1+3, v/v) and pellets with 500 mg of coal. The addition of 300 mg of NH4Cl to the coal pellets was also evaluated by the MIC. For the MAWD were used 150 mg of coal and 4.5 mL of 14.4 mol L-1 HNO3, 1.0 mL of 12 mol L-1 HCl and 1.5 mL of 23 mol L-1 HF. During the development of this work, a study of interferences for PGEs (Cu, Hf, Rb, Sr, Y and Zn, possible interferences for 193Ir, 105Pd, 195Pt, 103Rh and 101Ru) was performed. The determination of Os was difficult due to the formation of OsO4 during the digestion process, remaining in the nebulizer chamber of the ICP-MS. Generally, the digestion of enriched coal in HPA system presented satisfactory results when compared with MIC and MAWD. It was possible to digest up to 500 mg of coal with 6 mL of HNO3 + HCl (3+1, v/v) in HPA system. Recoveries between 100 and 127% were obtained for PGEs, except for Os, where errors over 350% were observed. RCC values in coal digested by HPA system were less than 40%. Limits of quantification were between 0.19 and 3.91 ng g-1.Neste trabalho foi desenvolvido um método para a decomposição de carvão mineral com elevado teor de cinzas (>30%) empregando um sistema de decomposição a altas temperaturas e pressões (HPA) para a posterior determinação dos elementos do grupo da platina (PGEs) por espectrometria de massa com plasma indutivamente acoplado (ICP-MS). A eficiência da digestão foi avaliada pelo teor de carbono residual (RCC), sendo estudadas soluções de digestão de HNO3 + HCl (3+1, v/v) e (1+1, v/v). Cerca de 500 mg de carvão foram decompostos em sistema HPA com 6 mL de HNO3 + HCl (3+1, v/v), sendo aplicados tempos de aquecimento de 20, 40 e 60 min a 320 ºC. Devido à baixa concentração desses elementos na amostra empregada neste trabalho, carvão foi enriquecido com PGEs e decomposto nas mesmas condições. Para a avaliação da exatidão, as amostras foram decompostas por combustão iniciada por radiação micro-ondas (MIC) e por decomposição por via úmida assistida por radiação micro-ondas (MAWD), utilizando condições baseadas na literatura. Na MIC foram utilizados 6 mL de HNO3 + HCl (3+1, v/v), (1+1, v/v) e (1+3, v/v) e comprimidos de carvão de 500 mg. A adição de 300 mg de NH4Cl sólido aos comprimidos de carvão também foi avaliada na MIC. Na MAWD foram utilizados 150 mg de carvão e solução de 4,5 mL de HNO3 14,4 mol L-1, 1,0 mL de HCl 12 mol L-1 e 1,5 mL de HF 23 mol L-1. Além do desenvolvimento do método de digestão, foram avaliadas as possíveis interferências para os isótopos de PGEs (Cu, Hf, Rb, Sr, Y e Zn, possíveis interferentes para 193Ir, 105Pd, 195Pt, 103Rh e 101Ru). A determinação de Os foi dificultada pela formação da espécie OsO4 durante a etapa de decomposição, a qual permanece na câmara de nebulização do espectrômetro de ICP-MS durante a etapa de determinação. De modo geral, a decomposição de carvão enriquecido em sistema HPA apresentou resultados satisfatórios quando comparados com a MIC e a MAWD. Foi possível decompor 500 mg de carvão utilizando 6 mL de água régia invertida em sistema HPA. Recuperações entre 100 e 127% foram obtidas para os PGEs, com exceção de Os, que apresentou erros acima de 350%. Os valores de RCC para carvão decomposto em sistema HPA foram menores que 40%. Os limites de quantificação foram de 0,19 a 3,91 ng g-1.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/openAccessQuímicaCarvão mineralAltas temperaturasCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Costa, Adilson Ben dahttp://lattes.cnpq.br/2604778196819181Rodrigues, Luiz Fredericohttp://lattes.cnpq.br/9354290360702855http://lattes.cnpq.br/7503089513286607Giesbrecht, Cristiano Kasdorf100600000000600a9c2788c-7913-4d7b-92e1-3429800ac028f153d4c6-e148-43b5-8861-2c728749d16c8fd7d402-38cb-487a-ae04-60b751dc48d633b68b9e-17df-4982-9a2b-3ab9ad0a1e02reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2017_GIESBRECHT_ CRISTIANO.pdfDIS_PPGQUIMICA_2017_GIESBRECHT_ CRISTIANO.pdfDissertação de Mestradoapplication/pdf6040594http://repositorio.ufsm.br/bitstream/1/13873/1/DIS_PPGQUIMICA_2017_GIESBRECHT_%20CRISTIANO.pdf99601c84fa7525d3957cd952482f8773MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS |
title |
Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS |
spellingShingle |
Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS Giesbrecht, Cristiano Kasdorf Química Carvão mineral Altas temperaturas CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS |
title_full |
Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS |
title_fullStr |
Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS |
title_full_unstemmed |
Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS |
title_sort |
Determinação de elementos do grupo da platina em carvão com alto teor de cinzas por ICP-MS |
author |
Giesbrecht, Cristiano Kasdorf |
author_facet |
Giesbrecht, Cristiano Kasdorf |
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.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/2604778196819181 |
dc.contributor.referee2.fl_str_mv |
Rodrigues, Luiz Frederico |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/9354290360702855 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/7503089513286607 |
dc.contributor.author.fl_str_mv |
Giesbrecht, Cristiano Kasdorf |
contributor_str_mv |
Flores, Érico Marlon de Moraes Costa, Adilson Ben da Rodrigues, Luiz Frederico |
dc.subject.por.fl_str_mv |
Química Carvão mineral Altas temperaturas |
topic |
Química Carvão mineral Altas temperaturas CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work a method for the digestion of high ash content coal (>30%) using a high pressure asher (HPA) system for further determination of platinum group elements (PGEs) by inductively coupled plasma mass spectrometry (ICP-MS) was developed. The efficiency of coal digestion with was evaluated by the residual carbon content (RCC), being evaluated solutions of HNO3 + HCl (3+1, v/v) and (1+1, v/v). About 500 mg of coal were digested in HPA system using 6 mL of HNO3 + HCl (3+1, v/v) and time of heating of 20, 40 and 60 min at 320 ºC. Due to the very low concentrations of these elements in the coal sample used in this work, the coal sample was enriched with PGEs and digested at the same conditions. To evaluate the accuracy, coal was digested by microwave induced combustion (MIC) and also by microwave-assisted wet digestion (MAWD). The MIC procedure was evaluated using 6 mL of HNO3 + HCl (3+1, v/v), (1+1, v/v) and (1+3, v/v) and pellets with 500 mg of coal. The addition of 300 mg of NH4Cl to the coal pellets was also evaluated by the MIC. For the MAWD were used 150 mg of coal and 4.5 mL of 14.4 mol L-1 HNO3, 1.0 mL of 12 mol L-1 HCl and 1.5 mL of 23 mol L-1 HF. During the development of this work, a study of interferences for PGEs (Cu, Hf, Rb, Sr, Y and Zn, possible interferences for 193Ir, 105Pd, 195Pt, 103Rh and 101Ru) was performed. The determination of Os was difficult due to the formation of OsO4 during the digestion process, remaining in the nebulizer chamber of the ICP-MS. Generally, the digestion of enriched coal in HPA system presented satisfactory results when compared with MIC and MAWD. It was possible to digest up to 500 mg of coal with 6 mL of HNO3 + HCl (3+1, v/v) in HPA system. Recoveries between 100 and 127% were obtained for PGEs, except for Os, where errors over 350% were observed. RCC values in coal digested by HPA system were less than 40%. Limits of quantification were between 0.19 and 3.91 ng g-1. |
publishDate |
2017 |
dc.date.issued.fl_str_mv |
2017-06-03 |
dc.date.accessioned.fl_str_mv |
2018-07-20T19:20:35Z |
dc.date.available.fl_str_mv |
2018-07-20T19:20:35Z |
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/1/13873 |
url |
http://repositorio.ufsm.br/handle/1/13873 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
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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 |
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