Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado
Autor(a) principal: | |
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Data de Publicação: | 2020 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Biblioteca Digital de Teses e Dissertações do UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/23076 |
Resumo: | In this work, pyrohydrolysis was proposed as a sample preparation method for the tungsten volatilization of the silicon carbide (SiC) and subsequent determination by induced coupled plasma optical emission spectroscopy (ICP OES) and mass spectrometry with inductively coupled plasma (ICP-MS). The following parameters were evaluated: the type of pyrohydrolysis reagent, H2O and H2O2 (10 to 50%, v/v), flow rate of the pyrohydrolysis reagent (0.2 a 1.4 mL min-1), type of carrier gas (oxygen and compressed air) and flow of this gas (0.1 a 1.0 L min-1), adding of auxiliary reagent (V2O5, PTFE, NH4Cl e NaCl), reaction time (30 to 180 min), oven temperature (1000 to 1200 °C), sample mass (2.5 to 20 mg) and type of absorbing solution (50% H2O2 or H2O). The use of H2O2 resulted in recoveries of 55% of tungsten, which is greater than when compared to recoveries only with the use of water as a reagent for pyrohydrolysis (30%). In addition, it was necessary to adapt a inlet at the end of the tube using 50% H2O2, where condensation of volatile tungsten species occurs. Without this inlet with 50% H2O2, tungsten was not fully collected, causing lower recoveries, in addition to causing memory effects. The condition that resulted in the best recovery was using 50% H2O2 at a flow rate of 1.2 ml min-1, oxygen flow rate of 0.1 L min-1, without using an auxiliary reagent, at temperature of 1000 ºC, for 60 min of reaction and using H2O as absorbing solution. The results were compared with the reference results of the alkaline fusion method and with the instrumental neutron activation analysis technique and they do not differ significantly (Student's t-test, confidence level of 95%). The proposed method with optimized conditions was applied to samples with different tungsten concentrations. The detection limit was 23 μg g-1 for the ICP OES technique and 2.6 μg g-1 for ICP-MS (estimated for 200 mg of mass). The proposed pyrohydrolysis method proved to be adequate for the determination of tungsten in SiC with minimal use of reagents and generation of waste. |
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2021-11-30T16:42:30Z2021-11-30T16:42:30Z2020-02-26http://repositorio.ufsm.br/handle/1/23076In this work, pyrohydrolysis was proposed as a sample preparation method for the tungsten volatilization of the silicon carbide (SiC) and subsequent determination by induced coupled plasma optical emission spectroscopy (ICP OES) and mass spectrometry with inductively coupled plasma (ICP-MS). The following parameters were evaluated: the type of pyrohydrolysis reagent, H2O and H2O2 (10 to 50%, v/v), flow rate of the pyrohydrolysis reagent (0.2 a 1.4 mL min-1), type of carrier gas (oxygen and compressed air) and flow of this gas (0.1 a 1.0 L min-1), adding of auxiliary reagent (V2O5, PTFE, NH4Cl e NaCl), reaction time (30 to 180 min), oven temperature (1000 to 1200 °C), sample mass (2.5 to 20 mg) and type of absorbing solution (50% H2O2 or H2O). The use of H2O2 resulted in recoveries of 55% of tungsten, which is greater than when compared to recoveries only with the use of water as a reagent for pyrohydrolysis (30%). In addition, it was necessary to adapt a inlet at the end of the tube using 50% H2O2, where condensation of volatile tungsten species occurs. Without this inlet with 50% H2O2, tungsten was not fully collected, causing lower recoveries, in addition to causing memory effects. The condition that resulted in the best recovery was using 50% H2O2 at a flow rate of 1.2 ml min-1, oxygen flow rate of 0.1 L min-1, without using an auxiliary reagent, at temperature of 1000 ºC, for 60 min of reaction and using H2O as absorbing solution. The results were compared with the reference results of the alkaline fusion method and with the instrumental neutron activation analysis technique and they do not differ significantly (Student's t-test, confidence level of 95%). The proposed method with optimized conditions was applied to samples with different tungsten concentrations. The detection limit was 23 μg g-1 for the ICP OES technique and 2.6 μg g-1 for ICP-MS (estimated for 200 mg of mass). The proposed pyrohydrolysis method proved to be adequate for the determination of tungsten in SiC with minimal use of reagents and generation of waste.Neste trabalho foi proposto a piroidrólise como método de preparo de amostras para a volatilização de tungstênio em carbeto de silício (SiC) para sua posterior determinação por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) e espectrometria de massa com plasma indutivamente acoplado (ICP-MS). Para isso, foram avaliados: o tipo de reagente de piroidrólise, H2O e H2O2 (10 a 50%, v/v), vazão do reagente de piroidrólise (0,2 a 1,4 mL min-1), tipo de gás carreador (oxigênio e ar comprimido) e vazão desse gás (0,1 a 1,0 L min-1), a adição de aceleradores (V2O5, PTFE, NH4Cl e NaCl), tempo de reação (30 a 180 minutos), temperatura do forno (1000 a 1200 ºC), massa de amostra (2,5 a 20 mg) e solução absorvedora (H2O2 50% ou H2O). A utilização de H2O2 resultou em recuperações de 55% de tungstênio, sendo essa maior do que quando comparado com recuperações somente com a utilização da água como reagente para a piroidrólise (30%). Ademais, foi necessário adaptar uma entrada de H2O2 50% no final do tubo, onde ocorriam condensações das espécies voláteis de tungstênio. Assim, o tungstênio não era totalmente coletado, causando recuperações inferiores, além de causar efeitos de memória. A condição que resultou na melhor recuperação foi utilizando H2O2 50 % em uma vazão de 1,2 mL min-1, vazão de oxigênio de 0,1 L min-1, sem uso de acelerador, na temperatura de 1000 ºC, por 60 min de reação e utilizando H2O no frasco coletor. Os resultados foram comparados com os resultados de referência do método de fusão alcalina e com a técnica de análise por ativação neutrônica instrumental e os valores adquiridos não se diferenciam significativamente (teste t-student, com nível de confiança de 95%). O método proposto com as condições otimizadas foi aplicado para amostras com diferentes concentrações de tungstênio. O limite de detecção foi de 23 μg g-1 para a técnica de ICP OES e de 2,6 μg g-1 para ICPMS (estimado para massa de 200 mg). O método de piroidrólise proposto mostrou-se adequado para a determinação de tungstênio em SiC com mínimo uso de reagentes e geração de resíduos.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/openAccessCarbeto de silícioPiroidróliseTungstênioPeróxido de hidrogênioSilicon carbidePyrohydrolysisTungstenHydrogen peroxideCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAEmprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acopladoUse of pyrohydrolysis as a method of preparing samples for the determination of tungsten in silicon carbide by techniques based on inductively coupled plasmainfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisMuller, Edson Irineuhttp://lattes.cnpq.br/5994311290376153Mortari, Sérgio RobertoDuarte, Fábio Andreihttp://lattes.cnpq.br/5068762860148399Senger, Caroline Matte1006000000006006006007f625a4e-a794-459f-919f-05a72717620d12085da2-c38c-4528-9560-9170474752f57e27f0ed-3de3-4398-b0a4-87a2c75ba9e97b2cc41c-5584-4228-a9bf-b1eb4d91e1e4reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado |
dc.title.alternative.eng.fl_str_mv |
Use of pyrohydrolysis as a method of preparing samples for the determination of tungsten in silicon carbide by techniques based on inductively coupled plasma |
title |
Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado |
spellingShingle |
Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado Senger, Caroline Matte Carbeto de silício Piroidrólise Tungstênio Peróxido de hidrogênio Silicon carbide Pyrohydrolysis Tungsten Hydrogen peroxide CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado |
title_full |
Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado |
title_fullStr |
Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado |
title_full_unstemmed |
Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado |
title_sort |
Emprego da piroidrólise como método de preparo de amostras para a determinação de tungstênio em carbeto de silício por técnicas baseadas em plasma indutivamente acoplado |
author |
Senger, Caroline Matte |
author_facet |
Senger, Caroline Matte |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Muller, Edson Irineu |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/5994311290376153 |
dc.contributor.referee1.fl_str_mv |
Mortari, Sérgio Roberto |
dc.contributor.referee2.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/5068762860148399 |
dc.contributor.author.fl_str_mv |
Senger, Caroline Matte |
contributor_str_mv |
Muller, Edson Irineu Mortari, Sérgio Roberto Duarte, Fábio Andrei |
dc.subject.por.fl_str_mv |
Carbeto de silício Piroidrólise Tungstênio Peróxido de hidrogênio |
topic |
Carbeto de silício Piroidrólise Tungstênio Peróxido de hidrogênio Silicon carbide Pyrohydrolysis Tungsten Hydrogen peroxide CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Silicon carbide Pyrohydrolysis Tungsten Hydrogen peroxide |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, pyrohydrolysis was proposed as a sample preparation method for the tungsten volatilization of the silicon carbide (SiC) and subsequent determination by induced coupled plasma optical emission spectroscopy (ICP OES) and mass spectrometry with inductively coupled plasma (ICP-MS). The following parameters were evaluated: the type of pyrohydrolysis reagent, H2O and H2O2 (10 to 50%, v/v), flow rate of the pyrohydrolysis reagent (0.2 a 1.4 mL min-1), type of carrier gas (oxygen and compressed air) and flow of this gas (0.1 a 1.0 L min-1), adding of auxiliary reagent (V2O5, PTFE, NH4Cl e NaCl), reaction time (30 to 180 min), oven temperature (1000 to 1200 °C), sample mass (2.5 to 20 mg) and type of absorbing solution (50% H2O2 or H2O). The use of H2O2 resulted in recoveries of 55% of tungsten, which is greater than when compared to recoveries only with the use of water as a reagent for pyrohydrolysis (30%). In addition, it was necessary to adapt a inlet at the end of the tube using 50% H2O2, where condensation of volatile tungsten species occurs. Without this inlet with 50% H2O2, tungsten was not fully collected, causing lower recoveries, in addition to causing memory effects. The condition that resulted in the best recovery was using 50% H2O2 at a flow rate of 1.2 ml min-1, oxygen flow rate of 0.1 L min-1, without using an auxiliary reagent, at temperature of 1000 ºC, for 60 min of reaction and using H2O as absorbing solution. The results were compared with the reference results of the alkaline fusion method and with the instrumental neutron activation analysis technique and they do not differ significantly (Student's t-test, confidence level of 95%). The proposed method with optimized conditions was applied to samples with different tungsten concentrations. The detection limit was 23 μg g-1 for the ICP OES technique and 2.6 μg g-1 for ICP-MS (estimated for 200 mg of mass). The proposed pyrohydrolysis method proved to be adequate for the determination of tungsten in SiC with minimal use of reagents and generation of waste. |
publishDate |
2020 |
dc.date.issued.fl_str_mv |
2020-02-26 |
dc.date.accessioned.fl_str_mv |
2021-11-30T16:42:30Z |
dc.date.available.fl_str_mv |
2021-11-30T16:42:30Z |
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info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/masterThesis |
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masterThesis |
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publishedVersion |
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http://repositorio.ufsm.br/handle/1/23076 |
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http://repositorio.ufsm.br/handle/1/23076 |
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 |
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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 |
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