Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios
Ano de defesa: | 2006 |
---|---|
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
|
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
BR
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/10597 |
Resumo: | In this work it is proposed a method for fluorine (F), bromine (Br) and iodine (I) determination in mineral-feedingstuff after sample decomposition by pyrohydrolysis. Fluoride is determined potentiometrically by means of ion selective electrode (ISE) while Br and I are determined by inductively coupled plasma mass spectrometry (ICP-MS). The sample decomposition is based on heating the sample at ca. of 1100 0C in presence of water vapor and vanadium pentoxide (V2O5) used as accelerator of the pyrohydrolysis reaction. During the heating step the analytes are vaporized and released from the sample and react with water vapor producing HF, HBr and HI. While HF vapor is simply condensed, HBr and HI need to be condensed and then trapped in a basic solution. Parameters like amount of sample + accelerator, gas flow rate (air), decomposition time, kind and concentration of trapping solution (for Br and I) were investigated for sample decomposition by pyrohydrolysis. It was observed that best results are obtained when the amount of sample + accelerator is 1 + 5, the sample decomposition is carried out during 10 min (producing approximately 10 mL of condensed solution) and the gas flow rate is 200 mL min-1. Tetramethylammonium hydroxide (TMAH), ammonium hydroxide (NH4OH) and a mixture of sodium carbonate/sodium bicarbonate (Na2CO3/NaHCO3) were tested as trapping solution for Br and I. Best analyte recoveries were obtained by using a 50 mmol L-1 sodium carbonate/sodium bicarbonate solution. Therefore, the aforementioned conditions were established in the proposed method. The limits of detection (LD) of F, Br and I were 12.0 μg g-1, 0.28 μg g-1 and 0.68 μg g-1, respectively, while the relative standard deviation (RSD) was typically lower than 14%. The method was validated by analyte recovery tests, whose recoveries ranged from 88% to 109%. The method was applied for the determination of F, Br and I in several samples whose concentrations were in the range of 600 to 1800 μg g-1, 26 to 30 μg g-1 and 10 to 58 μg g-1 for F, Br and I, respectively |
id |
UFSM-20_bf52c1af9388c973dd6acbf866d9964c |
---|---|
oai_identifier_str |
oai:repositorio.ufsm.br:1/10597 |
network_acronym_str |
UFSM-20 |
network_name_str |
Manancial - Repositório Digital da UFSM |
repository_id_str |
|
spelling |
2017-05-252017-05-252006-03-10TAFLICK, Ticiane. Halogens determination in mineral supplements after sample decomposition by pyrohydrolysis. 2006. 72 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006.http://repositorio.ufsm.br/handle/1/10597In this work it is proposed a method for fluorine (F), bromine (Br) and iodine (I) determination in mineral-feedingstuff after sample decomposition by pyrohydrolysis. Fluoride is determined potentiometrically by means of ion selective electrode (ISE) while Br and I are determined by inductively coupled plasma mass spectrometry (ICP-MS). The sample decomposition is based on heating the sample at ca. of 1100 0C in presence of water vapor and vanadium pentoxide (V2O5) used as accelerator of the pyrohydrolysis reaction. During the heating step the analytes are vaporized and released from the sample and react with water vapor producing HF, HBr and HI. While HF vapor is simply condensed, HBr and HI need to be condensed and then trapped in a basic solution. Parameters like amount of sample + accelerator, gas flow rate (air), decomposition time, kind and concentration of trapping solution (for Br and I) were investigated for sample decomposition by pyrohydrolysis. It was observed that best results are obtained when the amount of sample + accelerator is 1 + 5, the sample decomposition is carried out during 10 min (producing approximately 10 mL of condensed solution) and the gas flow rate is 200 mL min-1. Tetramethylammonium hydroxide (TMAH), ammonium hydroxide (NH4OH) and a mixture of sodium carbonate/sodium bicarbonate (Na2CO3/NaHCO3) were tested as trapping solution for Br and I. Best analyte recoveries were obtained by using a 50 mmol L-1 sodium carbonate/sodium bicarbonate solution. Therefore, the aforementioned conditions were established in the proposed method. The limits of detection (LD) of F, Br and I were 12.0 μg g-1, 0.28 μg g-1 and 0.68 μg g-1, respectively, while the relative standard deviation (RSD) was typically lower than 14%. The method was validated by analyte recovery tests, whose recoveries ranged from 88% to 109%. The method was applied for the determination of F, Br and I in several samples whose concentrations were in the range of 600 to 1800 μg g-1, 26 to 30 μg g-1 and 10 to 58 μg g-1 for F, Br and I, respectivelyNeste trabalho foi proposto o desenvolvimento de metodologia analítica para a decomposição de suplemento mineral para a determinação de flúor (F) por potenciometria com eletrodo íon seletivo (ISE) e de bromo (Br) e iodo (I) por espectrometria de massa com plasma indutivamente acoplado (ICP-MS). O método consiste na decomposição da amostra por piroidrólise, cujo princípio está baseado no aquecimento da amostra em um reator de quartzo a aproximadamente 1100 ºC, na presença de vapor d água e de um acelerador (V2O5). Os analitos são liberados da amostra e formam seus respectivos ácidos em contado com vapor d água, os quais podem ser simplesmente condensados (no caso do flúor) ou condensados e absorvidos numa solução básica (no caso do bromo e iodo). Para o desenvolvimento da metodologia, foram avaliadas diferentes condições para a decomposição da amostra, dentre elas, a relação amostra + acelerador, a vazão do gás de arraste (ar atmosférico), o tempo de decomposição, a solução absorvedora (para o bromo e iodo) e sua concentração. Foi constatado que as melhores condições de piroidrólise foram mediante o uso de uma relação amostra + acelerador de 1 + 5, tempo de aquecimento de 10 min (o que produz um volume de aproximadamente 10 mL de solução condensada) e vazão do gás de arraste em torno de 200 mL min-1. As soluções absorvedoras testadas foram hidróxido de tetrametilamônio, hidróxido de amônio e carbonato de sódio/bicarbonato de sódio. Melhores recuperações de bromo e iodo foram obtidas com solução de carbonato de sódio/bicarbonato de sódio 50 mmol L-1. Nas condições estabelecidas, os limites de detecção (LD) foram 12,0 μg g-1 de F, 0,28 μg g-1 de Br e 0,68 μg g-1 de I. A metodologia foi validada a partir de testes de recuperação do analito, cujas recuperações ficaram na faixa de 88% a 109%. O método foi aplicado para a determinação dos analitos em suplemento alimentar bovino, onde foi constada a presença de flúor, bromo e iodo na faixa de 600 a 1800, de 26 a 30 e de 10 a 58 μg g-1, respectivamenteapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaPiroidróliseHalogêniosSuplemento mineralPyrohydrolysisHalogensMineral supplementsCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADecomposição de suplemento mineral por piroidrólise para a determinação de halogêniosHalogens determination in mineral supplements after sample decomposition by pyrohydrolysisinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisDressler, Valderi Luizhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4723641Z7Paniz, José Neri Gottfriedhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4701043Z3http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4718179Y5Taflick, Ticiane10060000000040050030030029c59cfe-a489-425c-88a5-18fdf7cbf2580b49319a-064a-4ef1-98f4-50f9074fe5c8f98bfaca-713c-4b52-9a18-7edb1a63f3a1info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALticiane.pdfapplication/pdf1074504http://repositorio.ufsm.br/bitstream/1/10597/1/ticiane.pdffc2bdaf0f17b8bc21b6d97c1d5411b1cMD51TEXTticiane.pdf.txtticiane.pdf.txtExtracted texttext/plain132917http://repositorio.ufsm.br/bitstream/1/10597/2/ticiane.pdf.txt9a482c2923c1d5421c7136f3d840f0adMD52THUMBNAILticiane.pdf.jpgticiane.pdf.jpgIM Thumbnailimage/jpeg5576http://repositorio.ufsm.br/bitstream/1/10597/3/ticiane.pdf.jpg96e05c9da9d720d8030435fa657164b3MD531/105972017-07-25 12:05:06.07oai:repositorio.ufsm.br:1/10597Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132017-07-25T15:05:06Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios |
dc.title.alternative.eng.fl_str_mv |
Halogens determination in mineral supplements after sample decomposition by pyrohydrolysis |
title |
Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios |
spellingShingle |
Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios Taflick, Ticiane Piroidrólise Halogênios Suplemento mineral Pyrohydrolysis Halogens Mineral supplements CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios |
title_full |
Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios |
title_fullStr |
Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios |
title_full_unstemmed |
Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios |
title_sort |
Decomposição de suplemento mineral por piroidrólise para a determinação de halogênios |
author |
Taflick, Ticiane |
author_facet |
Taflick, Ticiane |
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 |
Paniz, José Neri Gottfried |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4701043Z3 |
dc.contributor.authorLattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4718179Y5 |
dc.contributor.author.fl_str_mv |
Taflick, Ticiane |
contributor_str_mv |
Dressler, Valderi Luiz Paniz, José Neri Gottfried |
dc.subject.por.fl_str_mv |
Piroidrólise Halogênios Suplemento mineral |
topic |
Piroidrólise Halogênios Suplemento mineral Pyrohydrolysis Halogens Mineral supplements CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pyrohydrolysis Halogens Mineral supplements |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work it is proposed a method for fluorine (F), bromine (Br) and iodine (I) determination in mineral-feedingstuff after sample decomposition by pyrohydrolysis. Fluoride is determined potentiometrically by means of ion selective electrode (ISE) while Br and I are determined by inductively coupled plasma mass spectrometry (ICP-MS). The sample decomposition is based on heating the sample at ca. of 1100 0C in presence of water vapor and vanadium pentoxide (V2O5) used as accelerator of the pyrohydrolysis reaction. During the heating step the analytes are vaporized and released from the sample and react with water vapor producing HF, HBr and HI. While HF vapor is simply condensed, HBr and HI need to be condensed and then trapped in a basic solution. Parameters like amount of sample + accelerator, gas flow rate (air), decomposition time, kind and concentration of trapping solution (for Br and I) were investigated for sample decomposition by pyrohydrolysis. It was observed that best results are obtained when the amount of sample + accelerator is 1 + 5, the sample decomposition is carried out during 10 min (producing approximately 10 mL of condensed solution) and the gas flow rate is 200 mL min-1. Tetramethylammonium hydroxide (TMAH), ammonium hydroxide (NH4OH) and a mixture of sodium carbonate/sodium bicarbonate (Na2CO3/NaHCO3) were tested as trapping solution for Br and I. Best analyte recoveries were obtained by using a 50 mmol L-1 sodium carbonate/sodium bicarbonate solution. Therefore, the aforementioned conditions were established in the proposed method. The limits of detection (LD) of F, Br and I were 12.0 μg g-1, 0.28 μg g-1 and 0.68 μg g-1, respectively, while the relative standard deviation (RSD) was typically lower than 14%. The method was validated by analyte recovery tests, whose recoveries ranged from 88% to 109%. The method was applied for the determination of F, Br and I in several samples whose concentrations were in the range of 600 to 1800 μg g-1, 26 to 30 μg g-1 and 10 to 58 μg g-1 for F, Br and I, respectively |
publishDate |
2006 |
dc.date.issued.fl_str_mv |
2006-03-10 |
dc.date.accessioned.fl_str_mv |
2017-05-25 |
dc.date.available.fl_str_mv |
2017-05-25 |
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.citation.fl_str_mv |
TAFLICK, Ticiane. Halogens determination in mineral supplements after sample decomposition by pyrohydrolysis. 2006. 72 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10597 |
identifier_str_mv |
TAFLICK, Ticiane. Halogens determination in mineral supplements after sample decomposition by pyrohydrolysis. 2006. 72 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006. |
url |
http://repositorio.ufsm.br/handle/1/10597 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
400 500 300 300 |
dc.relation.authority.fl_str_mv |
29c59cfe-a489-425c-88a5-18fdf7cbf258 0b49319a-064a-4ef1-98f4-50f9074fe5c8 f98bfaca-713c-4b52-9a18-7edb1a63f3a1 |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria |
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 |
BR |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria |
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 |
bitstream.url.fl_str_mv |
http://repositorio.ufsm.br/bitstream/1/10597/1/ticiane.pdf http://repositorio.ufsm.br/bitstream/1/10597/2/ticiane.pdf.txt http://repositorio.ufsm.br/bitstream/1/10597/3/ticiane.pdf.jpg |
bitstream.checksum.fl_str_mv |
fc2bdaf0f17b8bc21b6d97c1d5411b1c 9a482c2923c1d5421c7136f3d840f0ad 96e05c9da9d720d8030435fa657164b3 |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
|
_version_ |
1794524400481992704 |