Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS)
Ano de defesa: | 2004 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
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/1/26992 |
Resumo: | The purpose of this study was to develop a system for solid sampling analysis by flame atomic absorption spectrometry (SSA-FAAS), which would allow the use of higher sample mass when compared to other devices reported in the literature. The proposed system was made in quartz and two sample introduction procedures have been developed: samples were put in paper capsules or it was prepared as pastilles using agar as an agglutinate. Cadmium determination in biological samples was chosen for the demonstration of potential of this system, and calibration procedures was made using biological certified reference materials. Cadmium determination was made using an atomic absorption spectrometer with deuterium background corrector, using an air + acetylene flame, and a singleslot burner. The results were compared to those obtained by electrothermal atomic absorption spectrometry (ET AAS), after acid decomposition of the samples. Better results were obtained with the agar pastille samples. In this case, it was possible to use up to 21 mg of sample with the proposed system. Background signals were always below 0.08. The limit of quantification (LQ) was typically 37 ng g-1, one order of magnitude lower than those reported using other devices for SSA-FAAS. Using samples in paper capsules, the LQ was deteriorated due to the impurity of the paper (LQ = 750 ng g-1). No significant differences (P < 0.05) in the results were observed comparing the proposed procedure and conventional procedures using ET AAS. The sensitivities (based on the characteristic mass) were 0.34 and 0.19 ng using paper capsules and pastille procedures, respectively. The relative standard deviation was below 8%, and no memory effects were observed during the analytically useful lifetime of the quartz cell (ca. 1000 determinations). Thus, the developed system can be proposed for cadmium determination in biological samples by SSA-FAAS. |
id |
UFSM_6fadd5225e207581d8bd298d95d0ea9c |
---|---|
oai_identifier_str |
oai:repositorio.ufsm.br:1/26992 |
network_acronym_str |
UFSM |
network_name_str |
Biblioteca Digital de Teses e Dissertações do UFSM |
repository_id_str |
|
spelling |
2022-11-18T13:48:11Z2022-11-18T13:48:11Z2004-02-12http://repositorio.ufsm.br/handle/1/26992The purpose of this study was to develop a system for solid sampling analysis by flame atomic absorption spectrometry (SSA-FAAS), which would allow the use of higher sample mass when compared to other devices reported in the literature. The proposed system was made in quartz and two sample introduction procedures have been developed: samples were put in paper capsules or it was prepared as pastilles using agar as an agglutinate. Cadmium determination in biological samples was chosen for the demonstration of potential of this system, and calibration procedures was made using biological certified reference materials. Cadmium determination was made using an atomic absorption spectrometer with deuterium background corrector, using an air + acetylene flame, and a singleslot burner. The results were compared to those obtained by electrothermal atomic absorption spectrometry (ET AAS), after acid decomposition of the samples. Better results were obtained with the agar pastille samples. In this case, it was possible to use up to 21 mg of sample with the proposed system. Background signals were always below 0.08. The limit of quantification (LQ) was typically 37 ng g-1, one order of magnitude lower than those reported using other devices for SSA-FAAS. Using samples in paper capsules, the LQ was deteriorated due to the impurity of the paper (LQ = 750 ng g-1). No significant differences (P < 0.05) in the results were observed comparing the proposed procedure and conventional procedures using ET AAS. The sensitivities (based on the characteristic mass) were 0.34 and 0.19 ng using paper capsules and pastille procedures, respectively. The relative standard deviation was below 8%, and no memory effects were observed during the analytically useful lifetime of the quartz cell (ca. 1000 determinations). Thus, the developed system can be proposed for cadmium determination in biological samples by SSA-FAAS.Este estudo teve por objetivo principal o desenvolvimento de um sistema para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS), para permitir a utilização massas maiores de amostra que às utilizadas em outros sistemas atualmente descritos na literatura. O sistema proposto foi confeccionado em quartzo, e, dois procedimentos de introdução das amostras foram investigados: o encapsulamento das amostras em papel e a produção de pastilhas das amostras utilizando ágar como aglutinante. A determinação de cádmio em amostras biológicas foi escolhida para demonstrar a potencialidade deste sistema e, o procedimento de calibração foi desenvolvido com materiais de referência certificados. As determinações de cádmio foram feitas em espectrômetro de absorção atômica, com chama ar + acetileno, empregando um queimador do tipo monofenda e corretor de fundo com fonte de deutério. Os resultados foram comparados aos obtidos por espectrometria de absorção atômica com atomização eletrotérmica (ET AAS), após decomposição ácida das amostras. Os melhores resultados foram obtidos com amostras na forma de pastilhas com ágar, permitindo a introdução de até 21 mg de amostra no sistema. O fundo foi sempre inferior a 0,08. O limite de quantificação (LQ) foi tipicamente de 37 ng g-¹, dez vezes melhor do que o obtido por outros métodos descritos para SSA-FAAS. O procedimento de encapsulamento das amostras em papel apresentou um pior LQ (750 ng g-¹), devido à contaminação do papel utilizado. Não foram observadas diferenças significativas (P < 0,05) entre os resultados obtidos pelo sistema proposto e procedimentos convencionais de determinação por ET AAS. A sensibilidades (massa característica) obtida foi 0,34 ng e 0,19 ng para os procedimentos de encapsulamento com papel e pastilhas de amostra com ágar, respectivamente. O sistema desenvolvido apresentou desvio padrão relativo inferior a 8%, e ausência de efeito de memória durante a vida útil da cela de quartzo (aproximadamente 1000 determinações). Desta forma, este sistema pode ser proposto para a determinação de cádmio em amostras biológicas por SSA-FAAS.porUniversidade 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/openAccessAnálise direta de sólidosAnálise direta de sólidosCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAProcedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS)Procedures for cadmium determination for solid sampling analysis by flame atomic absorption spectrometry (SSA-FAAS)info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Martins, Ayrton FigueiredoWelz, Bernhard WelzKorn, Maria das Graças AndradeDressler, Valderi Luizhttp://lattes.cnpq.br/2604778196819181Costa, Adilson Ben da100600000000600600600600600600600a9c2788c-7913-4d7b-92e1-3429800ac0287a918d90-c070-47ed-a230-48116fa43baf9a4069fd-90ad-4736-915e-d1e19bfe4b08642fe705-ad8b-4c58-a76e-89aea62ecbee24b107f4-e0eb-493f-99dc-cdc23b819e76041d14df-2bfb-4de7-ba28-c81b80787eaereponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2004_COSTA_ADILSON.pdfTES_PPGQUÍMICA_2004_COSTA_ADILSON.pdfTese de Doutoradoapplication/pdf1126997http://repositorio.ufsm.br/bitstream/1/26992/1/TES_PPGQU%c3%8dMICA_2004_COSTA_ADILSON.pdfdc2ec9eaadcd328686405eed6d33f4ceMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/26992/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/26992/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/269922022-11-18 10:48:11.861oai:repositorio.ufsm.br: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 Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-11-18T13:48:11Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS) |
dc.title.alternative.eng.fl_str_mv |
Procedures for cadmium determination for solid sampling analysis by flame atomic absorption spectrometry (SSA-FAAS) |
title |
Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS) |
spellingShingle |
Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS) Costa, Adilson Ben da Análise direta de sólidos Análise direta de sólidos CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS) |
title_full |
Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS) |
title_fullStr |
Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS) |
title_full_unstemmed |
Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS) |
title_sort |
Procedimentos para a determinação de cádmio para análise de amostras sólidas por espectrometria de absorção atômica com chama (SSA-FAAS) |
author |
Costa, Adilson Ben da |
author_facet |
Costa, Adilson Ben da |
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 |
Martins, Ayrton Figueiredo |
dc.contributor.referee2.fl_str_mv |
Welz, Bernhard Welz |
dc.contributor.referee3.fl_str_mv |
Korn, Maria das Graças Andrade |
dc.contributor.referee4.fl_str_mv |
Dressler, Valderi Luiz |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/2604778196819181 |
dc.contributor.author.fl_str_mv |
Costa, Adilson Ben da |
contributor_str_mv |
Flores, Érico Marlon de Moraes Martins, Ayrton Figueiredo Welz, Bernhard Welz Korn, Maria das Graças Andrade Dressler, Valderi Luiz |
dc.subject.por.fl_str_mv |
Análise direta de sólidos Análise direta de sólidos |
topic |
Análise direta de sólidos Análise direta de sólidos CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The purpose of this study was to develop a system for solid sampling analysis by flame atomic absorption spectrometry (SSA-FAAS), which would allow the use of higher sample mass when compared to other devices reported in the literature. The proposed system was made in quartz and two sample introduction procedures have been developed: samples were put in paper capsules or it was prepared as pastilles using agar as an agglutinate. Cadmium determination in biological samples was chosen for the demonstration of potential of this system, and calibration procedures was made using biological certified reference materials. Cadmium determination was made using an atomic absorption spectrometer with deuterium background corrector, using an air + acetylene flame, and a singleslot burner. The results were compared to those obtained by electrothermal atomic absorption spectrometry (ET AAS), after acid decomposition of the samples. Better results were obtained with the agar pastille samples. In this case, it was possible to use up to 21 mg of sample with the proposed system. Background signals were always below 0.08. The limit of quantification (LQ) was typically 37 ng g-1, one order of magnitude lower than those reported using other devices for SSA-FAAS. Using samples in paper capsules, the LQ was deteriorated due to the impurity of the paper (LQ = 750 ng g-1). No significant differences (P < 0.05) in the results were observed comparing the proposed procedure and conventional procedures using ET AAS. The sensitivities (based on the characteristic mass) were 0.34 and 0.19 ng using paper capsules and pastille procedures, respectively. The relative standard deviation was below 8%, and no memory effects were observed during the analytically useful lifetime of the quartz cell (ca. 1000 determinations). Thus, the developed system can be proposed for cadmium determination in biological samples by SSA-FAAS. |
publishDate |
2004 |
dc.date.issued.fl_str_mv |
2004-02-12 |
dc.date.accessioned.fl_str_mv |
2022-11-18T13:48:11Z |
dc.date.available.fl_str_mv |
2022-11-18T13:48:11Z |
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 |
http://repositorio.ufsm.br/handle/1/26992 |
url |
http://repositorio.ufsm.br/handle/1/26992 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 600 |
dc.relation.authority.fl_str_mv |
a9c2788c-7913-4d7b-92e1-3429800ac028 7a918d90-c070-47ed-a230-48116fa43baf 9a4069fd-90ad-4736-915e-d1e19bfe4b08 642fe705-ad8b-4c58-a76e-89aea62ecbee 24b107f4-e0eb-493f-99dc-cdc23b819e76 041d14df-2bfb-4de7-ba28-c81b80787eae |
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 |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Biblioteca Digital de Teses e Dissertações do UFSM |
collection |
Biblioteca Digital de Teses e Dissertações do UFSM |
bitstream.url.fl_str_mv |
http://repositorio.ufsm.br/bitstream/1/26992/1/TES_PPGQU%c3%8dMICA_2004_COSTA_ADILSON.pdf http://repositorio.ufsm.br/bitstream/1/26992/2/license_rdf http://repositorio.ufsm.br/bitstream/1/26992/3/license.txt |
bitstream.checksum.fl_str_mv |
dc2ec9eaadcd328686405eed6d33f4ce 4460e5956bc1d1639be9ae6146a50347 2f0571ecee68693bd5cd3f17c1e075df |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 |
repository.name.fl_str_mv |
Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
_version_ |
1793240150521675776 |