Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva
Ano de defesa: | 2022 |
---|---|
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/1/27036 |
Resumo: | In this work, a sample preparation method was developed using the dispersive liquidliquid microextraction (DLLME) for the Cu extraction and pre-concentration in beer, followed by the determination by flame atomic absorption spectrometry (F AAS). Unlike the conventional DLLME, where a dispersive solvent and an extraction solvent are mixed, only the extracting solvent was injected into the beer. For the DLLME optimization for Cu extraction, some parameters such as type of extracting solvent and its volume, sample volume, pH, concentration of sodium diethyldithiocarbamate as a complexing agent and the viability of ultrasound in the dispersion were evaluated. After optimization, the external calibration curve was linear between 5 and 100 µg L-¹ Cu, with a limit of quantification of 9,1 µg L-¹ . Accuracy was evaluated for 3 samples and the results were compared with those obtained after microwave-assisted sample digestion and subsequent Cu determination by inductively coupled plasma mass spectrometry and inductively coupled plasma optical emission spectrometry. The method was applied to 7 beer samples and the Cu concentration ranged from 20,6 and 58,8 µg L -¹ . Accuracy was also evaluated by analyte spike, which ranged from 92 to 116%, with relative standard deviation from 3 to 16%. The proposed method for the Cu extraction and pre-concentration from beer by DLLME and quantification by F AAS proved to be suitable in terms of linearity, accuracy and precision, presenting as positive aspects the speed, simplicity of operation and low reagents consumption. |
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Biblioteca Digital de Teses e Dissertações do UFSM |
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2022-11-22T12:03:05Z2022-11-22T12:03:05Z2022-09-21http://repositorio.ufsm.br/handle/1/27036In this work, a sample preparation method was developed using the dispersive liquidliquid microextraction (DLLME) for the Cu extraction and pre-concentration in beer, followed by the determination by flame atomic absorption spectrometry (F AAS). Unlike the conventional DLLME, where a dispersive solvent and an extraction solvent are mixed, only the extracting solvent was injected into the beer. For the DLLME optimization for Cu extraction, some parameters such as type of extracting solvent and its volume, sample volume, pH, concentration of sodium diethyldithiocarbamate as a complexing agent and the viability of ultrasound in the dispersion were evaluated. After optimization, the external calibration curve was linear between 5 and 100 µg L-¹ Cu, with a limit of quantification of 9,1 µg L-¹ . Accuracy was evaluated for 3 samples and the results were compared with those obtained after microwave-assisted sample digestion and subsequent Cu determination by inductively coupled plasma mass spectrometry and inductively coupled plasma optical emission spectrometry. The method was applied to 7 beer samples and the Cu concentration ranged from 20,6 and 58,8 µg L -¹ . Accuracy was also evaluated by analyte spike, which ranged from 92 to 116%, with relative standard deviation from 3 to 16%. The proposed method for the Cu extraction and pre-concentration from beer by DLLME and quantification by F AAS proved to be suitable in terms of linearity, accuracy and precision, presenting as positive aspects the speed, simplicity of operation and low reagents consumption.Neste trabalho foi desenvolvido um método de preparo de amostras empregando a microextração líquido-líquido dispersiva (DLLME) para a extração e pré-concentração de Cu em cerveja, seguido da determinação por espectrometria de absorção atômica com chama (F AAS). Diferente da DLLME convencional, onde é feita a mistura entre um solvente dispersor e um solvente extrator, foi feita a injeção apenas do solvente extrator na cerveja. Para a otimização da DLLME visando a extração de Cu, foram avaliados alguns parâmetros como tipo de solvente extrator e seu volume, volume de amostra, pH, concentração do dietilditiocarbamato de sódio como complexante e a viabilidade do ultrassom na dispersão. Após a otimização das condições da DLLME, a curva de calibração externa foi linear entre 5 e 100 µg L -¹ de Cu, com limite de quantificação de 9,1 µg L-¹ . A exatidão do método proposto foi avaliada para 3 amostras e os resultados foram comparados com os obtidos após decomposição assistida por micro-ondas e posterior determinação de Cu por espectrometria de massa com plasma indutivamente acoplado e por espectrometria de emissão óptica com plasma indutivamente acoplado. O método foi aplicado para 7 amostras de cerveja e a concentração de Cu variou entre 20,6 e 58,8 µg L -¹ . A exatidão também foi avaliada utilizando ensaio de recuperação, variando entre 92 e 116%, com desvio padrão relativo entre 3 e 16%. O método de extração e pré-concentração de Cu em cerveja por DLLME e quantificação por F AAS mostrou-se adequado em termos de linearidade, exatidão e precisão, apresentando como aspectos positivos a rapidez, simplicidade de operação e baixo consumo de reagentes.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/openAccessDLLMECobreCervejaF AASPreparo de amostrasCopperBeerSample preparationCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersivaDetermination of copper in beer by flame atomic absorption spectrometry after dispersive liquid-liquid microextractioninfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisDuarte, Fábio Andreihttp://lattes.cnpq.br/3503633944419329Flores, Éder Lisandro de MoraesRosa, Francisco Cunha dahttp://lattes.cnpq.br/1963768847542028Silveira, Jader Rodrigo Kappaun da100600000000600600600600600218323ac-81fc-4a7a-93bc-4536cd06202fd2848028-94a6-4037-98a1-264507c7bc4f44b2e8e0-9f59-4bfc-9a22-9662db92dac80f018176-85de-47fb-9e02-7396866abd6freponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUÍMICA_2022_SILVEIRA_JADER.pdfDIS_PPGQUÍMICA_2022_SILVEIRA_JADER.pdfDissertação de Mestradoapplication/pdf1002239http://repositorio.ufsm.br/bitstream/1/27036/1/DIS_PPGQU%c3%8dMICA_2022_SILVEIRA_JADER.pdf16e6413d7ecf8014ae20015d10288affMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/27036/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/27036/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/270362022-11-22 09:03:05.914oai:repositorio.ufsm.br:1/27036TElDRU7Dh0EgREUgRElTVFJJQlVJw4fDg08gTsODTy1FWENMVVNJVkEKCkNvbSBhIGFwcmVzZW50YcOnw6NvIGRlc3RhIGxpY2Vuw6dhLCB2b2PDqiAobyBhdXRvciAoZXMpIG91IG8gdGl0dWxhciBkb3MgZGlyZWl0b3MgZGUgYXV0b3IpIGNvbmNlZGUgw6AgVW5pdmVyc2lkYWRlCkZlZGVyYWwgZGUgU2FudGEgTWFyaWEgKFVGU00pIG8gZGlyZWl0byBuw6NvLWV4Y2x1c2l2byBkZSByZXByb2R1emlyLCAgdHJhZHV6aXIgKGNvbmZvcm1lIGRlZmluaWRvIGFiYWl4byksIGUvb3UKZGlzdHJpYnVpciBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gKGluY2x1aW5kbyBvIHJlc3VtbykgcG9yIHRvZG8gbyBtdW5kbyBubyBmb3JtYXRvIGltcHJlc3NvIGUgZWxldHLDtG5pY28gZQplbSBxdWFscXVlciBtZWlvLCBpbmNsdWluZG8gb3MgZm9ybWF0b3Mgw6F1ZGlvIG91IHbDrWRlby4KClZvY8OqIGNvbmNvcmRhIHF1ZSBhIFVGU00gcG9kZSwgc2VtIGFsdGVyYXIgbyBjb250ZcO6ZG8sIHRyYW5zcG9yIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbwpwYXJhIHF1YWxxdWVyIG1laW8gb3UgZm9ybWF0byBwYXJhIGZpbnMgZGUgcHJlc2VydmHDp8Ojby4KClZvY8OqIHRhbWLDqW0gY29uY29yZGEgcXVlIGEgVUZTTSBwb2RlIG1hbnRlciBtYWlzIGRlIHVtYSBjw7NwaWEgYSBzdWEgdGVzZSBvdQpkaXNzZXJ0YcOnw6NvIHBhcmEgZmlucyBkZSBzZWd1cmFuw6dhLCBiYWNrLXVwIGUgcHJlc2VydmHDp8Ojby4KClZvY8OqIGRlY2xhcmEgcXVlIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyDDqSBvcmlnaW5hbCBlIHF1ZSB2b2PDqiB0ZW0gbyBwb2RlciBkZSBjb25jZWRlciBvcyBkaXJlaXRvcyBjb250aWRvcwpuZXN0YSBsaWNlbsOnYS4gVm9jw6ogdGFtYsOpbSBkZWNsYXJhIHF1ZSBvIGRlcMOzc2l0byBkYSBzdWEgdGVzZSBvdSBkaXNzZXJ0YcOnw6NvIG7Do28sIHF1ZSBzZWphIGRlIHNldQpjb25oZWNpbWVudG8sIGluZnJpbmdlIGRpcmVpdG9zIGF1dG9yYWlzIGRlIG5pbmd1w6ltLgoKQ2FzbyBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gY29udGVuaGEgbWF0ZXJpYWwgcXVlIHZvY8OqIG7Do28gcG9zc3VpIGEgdGl0dWxhcmlkYWRlIGRvcyBkaXJlaXRvcyBhdXRvcmFpcywgdm9jw6oKZGVjbGFyYSBxdWUgb2J0ZXZlIGEgcGVybWlzc8OjbyBpcnJlc3RyaXRhIGRvIGRldGVudG9yIGRvcyBkaXJlaXRvcyBhdXRvcmFpcyBwYXJhIGNvbmNlZGVyIMOgIFVGU00Kb3MgZGlyZWl0b3MgYXByZXNlbnRhZG9zIG5lc3RhIGxpY2Vuw6dhLCBlIHF1ZSBlc3NlIG1hdGVyaWFsIGRlIHByb3ByaWVkYWRlIGRlIHRlcmNlaXJvcyBlc3TDoSBjbGFyYW1lbnRlCmlkZW50aWZpY2FkbyBlIHJlY29uaGVjaWRvIG5vIHRleHRvIG91IG5vIGNvbnRlw7pkbyBkYSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gb3JhIGRlcG9zaXRhZGEuCgpDQVNPIEEgVEVTRSBPVSBESVNTRVJUQcOHw4NPIE9SQSBERVBPU0lUQURBIFRFTkhBIFNJRE8gUkVTVUxUQURPIERFIFVNIFBBVFJPQ8ONTklPIE9VCkFQT0lPIERFIFVNQSBBR8OKTkNJQSBERSBGT01FTlRPIE9VIE9VVFJPIE9SR0FOSVNNTyBRVUUgTsODTyBTRUpBIEEgVUZTTQosIFZPQ8OKIERFQ0xBUkEgUVVFIFJFU1BFSVRPVSBUT0RPUyBFIFFVQUlTUVVFUiBESVJFSVRPUyBERSBSRVZJU8ODTyBDT01PClRBTULDiU0gQVMgREVNQUlTIE9CUklHQcOHw5VFUyBFWElHSURBUyBQT1IgQ09OVFJBVE8gT1UgQUNPUkRPLgoKQSBVRlNNIHNlIGNvbXByb21ldGUgYSBpZGVudGlmaWNhciBjbGFyYW1lbnRlIG8gc2V1IG5vbWUgKHMpIG91IG8ocykgbm9tZShzKSBkbyhzKQpkZXRlbnRvcihlcykgZG9zIGRpcmVpdG9zIGF1dG9yYWlzIGRhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbywgZSBuw6NvIGZhcsOhIHF1YWxxdWVyIGFsdGVyYcOnw6NvLCBhbMOpbSBkYXF1ZWxhcwpjb25jZWRpZGFzIHBvciBlc3RhIGxpY2Vuw6dhLgoKBiblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-11-22T12:03:05Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva |
dc.title.alternative.eng.fl_str_mv |
Determination of copper in beer by flame atomic absorption spectrometry after dispersive liquid-liquid microextraction |
title |
Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva |
spellingShingle |
Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva Silveira, Jader Rodrigo Kappaun da DLLME Cobre Cerveja F AAS Preparo de amostras Copper Beer Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva |
title_full |
Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva |
title_fullStr |
Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva |
title_full_unstemmed |
Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva |
title_sort |
Determinação de cobre em cerveja por espectrometria de absorção atômica com chama após microextração líquido-líquido dispersiva |
author |
Silveira, Jader Rodrigo Kappaun da |
author_facet |
Silveira, Jader Rodrigo Kappaun da |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/3503633944419329 |
dc.contributor.referee1.fl_str_mv |
Flores, Éder Lisandro de Moraes |
dc.contributor.referee2.fl_str_mv |
Rosa, Francisco Cunha da |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/1963768847542028 |
dc.contributor.author.fl_str_mv |
Silveira, Jader Rodrigo Kappaun da |
contributor_str_mv |
Duarte, Fábio Andrei Flores, Éder Lisandro de Moraes Rosa, Francisco Cunha da |
dc.subject.por.fl_str_mv |
DLLME Cobre Cerveja F AAS Preparo de amostras |
topic |
DLLME Cobre Cerveja F AAS Preparo de amostras Copper Beer Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Copper Beer Sample preparation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, a sample preparation method was developed using the dispersive liquidliquid microextraction (DLLME) for the Cu extraction and pre-concentration in beer, followed by the determination by flame atomic absorption spectrometry (F AAS). Unlike the conventional DLLME, where a dispersive solvent and an extraction solvent are mixed, only the extracting solvent was injected into the beer. For the DLLME optimization for Cu extraction, some parameters such as type of extracting solvent and its volume, sample volume, pH, concentration of sodium diethyldithiocarbamate as a complexing agent and the viability of ultrasound in the dispersion were evaluated. After optimization, the external calibration curve was linear between 5 and 100 µg L-¹ Cu, with a limit of quantification of 9,1 µg L-¹ . Accuracy was evaluated for 3 samples and the results were compared with those obtained after microwave-assisted sample digestion and subsequent Cu determination by inductively coupled plasma mass spectrometry and inductively coupled plasma optical emission spectrometry. The method was applied to 7 beer samples and the Cu concentration ranged from 20,6 and 58,8 µg L -¹ . Accuracy was also evaluated by analyte spike, which ranged from 92 to 116%, with relative standard deviation from 3 to 16%. The proposed method for the Cu extraction and pre-concentration from beer by DLLME and quantification by F AAS proved to be suitable in terms of linearity, accuracy and precision, presenting as positive aspects the speed, simplicity of operation and low reagents consumption. |
publishDate |
2022 |
dc.date.accessioned.fl_str_mv |
2022-11-22T12:03:05Z |
dc.date.available.fl_str_mv |
2022-11-22T12:03:05Z |
dc.date.issued.fl_str_mv |
2022-09-21 |
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/1/27036 |
url |
http://repositorio.ufsm.br/handle/1/27036 |
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 |
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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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