Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único
Ano de defesa: | 2021 |
---|---|
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: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/24658 |
Resumo: | In this work, microwave-induced combustion in disposable vessel (MIC-DV) was evaluated for the decomposition of fish tissue for the subsequent determination of As, Cd, Cr, Cu, Mn, Pb, Se and V by inductively coupled plasma mass spectrometry (ICP-MS) and Hg in a flow injection system with cold vapor generation coupled with inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS). In addition, a chemical vapor generation system in a disposable vessel (DV-CVG) was proposed, coupled with ICP-MS and atomic absorption spectrometry (AAS) techniques for the determination of Hg. For the development of the method using MIC-DV, the following parameters were evaluated: composition of the absorbing solution (HNO3 and HCl), concentration of HNO3 as an absorbing solution (0.25, 0.5, 1, 3, 5, 7 and 14.4 mol L-¹), sample mass (10, 15, 20, 25 and 30 mg), absorbing solution volume (1, 3, 5 and 7 mL) and successive digestion cycles (2 and 3 times). For the ignition of the sample in the MIC-DV, 40 μL of NH4NO3 10 mol L-¹ were pipetted into a filter paper disc, which was positioned in the quartz holder and the set was inserted in disposable vessel. Before closing, the vessel were purged with O2 for 60 s at a flow rate of 4 L min-¹ and inserted into the microwave oven for irradiation for 30 s. After decomposition by MIC-DV, the digested were stored in a refrigerator until quantification. The results obtained by MIC-DV were compared with those obtained by the methods of microwave-induced combustion (MIC) and microwave assisted wet decomposition (MAWD). The proposed method was applied to 5 samples of fish tissue and to the certified reference material (CRM) of fish liver (DOLT 4) under the following optimized conditions: 5 mL of 0.5 mol L-¹ of HNO3 as an absorbing solution using 10 mg of sample mass with one combustion. Considering the system developed for the determination of Hg (DV-CVG), it uses only the lid of the disposable vessel itself with four holes, which were necessary for the introduction of HCl, NaBH4, carrier gas and for carrying the gas phase from inside the vessel to the determination technique. This system was coupled with the ICP-MS and AAS technique, being called DV-CVG-ICP-MS and DV-CVG-AAS. The agreement for the elements As, Cd, Cr, Hg, Mn, Se and V in the 5 samples and CRM evaluated after the decomposition by MIC-DV, did not show significant difference (ANOVA) when compared with the reference methods and certified values. The MIC-DV limits of quantification (LOQs) for As, Cd, Cr, Hg, Mn, Pb, Se and V were 0.02, 0.05, 0.50, 0.10, 0.19, 0, 7, 0.18, 0.02 μg g-¹, respectively. For As, Cd and Hg, the LOQs were below the maximum limit required by MERCOSUL for fish tissue. The DV-CVG-ICP-MS that uses the adapted cover presented a lower LOQ when compared to the FI-CVG-ICP-MS used as a reference. The LOQs of the system with the adapted lid coupled to ICP-MS and AAS were 0.025 and 1.2 μg g-¹ respectively. Both the MIC-DV method and the DV-CVG systems developed in this work, presented low cost (disregarding the technique used), simplicity of operation, safety for the operator, reduced use of reagents and used for the quality control of inorganic contaminants such as As, Cd, Cr, Hg, Mn, Se and V. |
id |
UFSM-20_e4543794fe69000e0ca70e00185784b5 |
---|---|
oai_identifier_str |
oai:repositorio.ufsm.br:1/24658 |
network_acronym_str |
UFSM-20 |
network_name_str |
Manancial - Repositório Digital da UFSM |
repository_id_str |
|
spelling |
2022-06-08T11:34:46Z2022-06-08T11:34:46Z2021-02-15http://repositorio.ufsm.br/handle/1/24658In this work, microwave-induced combustion in disposable vessel (MIC-DV) was evaluated for the decomposition of fish tissue for the subsequent determination of As, Cd, Cr, Cu, Mn, Pb, Se and V by inductively coupled plasma mass spectrometry (ICP-MS) and Hg in a flow injection system with cold vapor generation coupled with inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS). In addition, a chemical vapor generation system in a disposable vessel (DV-CVG) was proposed, coupled with ICP-MS and atomic absorption spectrometry (AAS) techniques for the determination of Hg. For the development of the method using MIC-DV, the following parameters were evaluated: composition of the absorbing solution (HNO3 and HCl), concentration of HNO3 as an absorbing solution (0.25, 0.5, 1, 3, 5, 7 and 14.4 mol L-¹), sample mass (10, 15, 20, 25 and 30 mg), absorbing solution volume (1, 3, 5 and 7 mL) and successive digestion cycles (2 and 3 times). For the ignition of the sample in the MIC-DV, 40 μL of NH4NO3 10 mol L-¹ were pipetted into a filter paper disc, which was positioned in the quartz holder and the set was inserted in disposable vessel. Before closing, the vessel were purged with O2 for 60 s at a flow rate of 4 L min-¹ and inserted into the microwave oven for irradiation for 30 s. After decomposition by MIC-DV, the digested were stored in a refrigerator until quantification. The results obtained by MIC-DV were compared with those obtained by the methods of microwave-induced combustion (MIC) and microwave assisted wet decomposition (MAWD). The proposed method was applied to 5 samples of fish tissue and to the certified reference material (CRM) of fish liver (DOLT 4) under the following optimized conditions: 5 mL of 0.5 mol L-¹ of HNO3 as an absorbing solution using 10 mg of sample mass with one combustion. Considering the system developed for the determination of Hg (DV-CVG), it uses only the lid of the disposable vessel itself with four holes, which were necessary for the introduction of HCl, NaBH4, carrier gas and for carrying the gas phase from inside the vessel to the determination technique. This system was coupled with the ICP-MS and AAS technique, being called DV-CVG-ICP-MS and DV-CVG-AAS. The agreement for the elements As, Cd, Cr, Hg, Mn, Se and V in the 5 samples and CRM evaluated after the decomposition by MIC-DV, did not show significant difference (ANOVA) when compared with the reference methods and certified values. The MIC-DV limits of quantification (LOQs) for As, Cd, Cr, Hg, Mn, Pb, Se and V were 0.02, 0.05, 0.50, 0.10, 0.19, 0, 7, 0.18, 0.02 μg g-¹, respectively. For As, Cd and Hg, the LOQs were below the maximum limit required by MERCOSUL for fish tissue. The DV-CVG-ICP-MS that uses the adapted cover presented a lower LOQ when compared to the FI-CVG-ICP-MS used as a reference. The LOQs of the system with the adapted lid coupled to ICP-MS and AAS were 0.025 and 1.2 μg g-¹ respectively. Both the MIC-DV method and the DV-CVG systems developed in this work, presented low cost (disregarding the technique used), simplicity of operation, safety for the operator, reduced use of reagents and used for the quality control of inorganic contaminants such as As, Cd, Cr, Hg, Mn, Se and V.Neste trabalho a combustão iniciada por micro-ondas em frascos descartáveis (MIC-DV) foi avaliada para a decomposição de tecido de peixe para a posterior determinação de As, Cd, Cr, Cu, Mn, Pb, Se e V por espectrometria de massa com plasma indutivamente acoplado (ICP-MS) e Hg em sistema de injeção em fluxo com geração de vapor frio acoplado a espectrometria de massa com plasma indutivamente acoplado (FI-CVG-ICP-MS). Adicionalmente, foi proposto um sistema de geração química de vapor em frasco único (DV-CVG) acoplado as técnicas de ICP-MS e espectrometria de absorção atômica (AAS) para a determinação de Hg. Para o desenvolvimento do método empregando a MIC-DV, foram avaliados os seguintes parâmetros: composição da solução absorvedora (HNO3 e HCl), concentração de HNO3 como solução absorvedora (0,25, 0,5, 1, 3, 5, 7 e 14,4 mol L-¹), massa de amostra (10, 15, 20, 25 e 30 mg), volume de solução absorvedora (1, 3, 5 e 7 mL) e ciclos sucessivos de combustão (2 e 3 vezes). Para a ignição da amostra na MIC-DV, foram pipetados 40 μL de NH4NO3 10 mol L-¹ em disco de papel filtro, o qual foi posicionado no suporte de quartzo e o conjunto foi inserido nos frascos descartáveis. Antes do fechamento, os frascos foram purgados com O2 durante 60 s com vazão de 4 L min-¹ e submetidos a irradiação da micro-ondas por 30 s. Após a decomposição por MIC-DV, os digeridos foram armazenados em geladeira até a quantificação. Os resultados obtidos por MIC-DV foram comparados com os obtidos pelos métodos da combustão iniciada por micro-ondas (MIC) e decomposição por via úmida assistida por micro-ondas (MAWD). O método proposto foi aplicado para 5 amostras de tecido de peixe e para o material de referência certificado (CRM) de fígado de peixe (DOLT4) nas seguintes condições otimizadas: 5 mL de 0,5 mol L-¹ de HNO3 como solução absorvedora usando 10 mg de massa de amostra com uma queima. Considerando o sistema desenvolvido para a determinação de Hg (DV-CVG), este utiliza apenas a tampa do próprio frasco descartável com quatro orifícios, os quais foram necessários para a introdução de HCl, NaBH4, gás de arraste e para o carreamento da fase gasosa de dentro do frasco até a técnica de determinação. Este sistema foi acoplado à técnica de ICP-MS e AAS, sendo chamado de DV-CVG-ICP-MS e DV-CVG-AAS. A concordância para os elementos As, Cd, Cr, Hg, Mn, Se e V nas 5 amostras e CRM avaliados após a decomposição por MIC-DV, não apresentaram diferença significativa (ANOVA) quando comparados com os métodos de referência e valores certificados. Os limites de quantificação (LQs) da MIC-DV para As, Cd, Cr, Hg, Mn, Pb, Se e V foram 0,02, 0,05, 0,50, 0,10, 0,19, 0,7, 0,18, 0,02 μg g-¹, respectivamente. Para As, Cd e Hg, os LQs foram inferiores ao limite máximo exigido pelo MERCOSUL para tecido de peixe. A DV-CVG-ICP-MS que utiliza a tampa adaptada apresentou LQ inferior quando comparado com o FI-CVG-ICP-MS usado como referência. Os LQs do sistema com a tampa adaptada acoplado a ICP-MS e AAS foram de 0,025 e 1,2 μg g-¹ respectivamente. Tanto o método da MIC-DV quanto os sistemas DV-CVG desenvolvidos neste trabalho, apresentaram baixo custo (desconsiderando a técnica utilizada), simplicidade de operação, segurança para o operador, uso reduzido de reagentes e utilizados para o controle de qualidade de contaminantes inorgânicos como As, Cd, Cr, Hg, Mn, Se e V.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/openAccessMIC-DVPeixeFrasco únicoDV-CVG-ICP-MSDV-CVG-AASFishSingle vesselCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAvaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco únicoEvaluation of MIC-DV for decomposition of fish tissue and system development for cold vapor generation in disposable vesselinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Bolzan, Rodrigo CordeiroDuarte, Fábio AndreiBarin, Juliano SmaniotoRodrigues, Luiz FredericoMortari, Sergio Robertohttp://lattes.cnpq.br/0617212620483345Pardinho, Renan Buque100600000000600600600600600600600600a9c2788c-7913-4d7b-92e1-3429800ac028d95fe6ca-aa5d-4323-ba0e-ff6e1407ed3caeaf2656-6542-4955-b951-a92cd5517da5bedaf96e-f8fc-48ca-820e-6559530109cb91851857-1b47-4140-8705-5c9a23daaf4deb5f6555-ee67-449a-ab4f-ae56ae8070f3ebb296a1-1569-43d1-8946-7cc7e3bec814reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2021_PARDINHO_RENAN.pdfTES_PPGQUÍMICA_2021_PARDINHO_RENAN.pdfTese de Doutoradoapplication/pdf1792425http://repositorio.ufsm.br/bitstream/1/24658/1/TES_PPGQU%c3%8dMICA_2021_PARDINHO_RENAN.pdfc0b9f4c4d5c989668fa13767c0fb37d6MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/24658/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/24658/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/246582022-06-08 08:34:46.498oai:repositorio.ufsm.br:1/24658TElDRU7Dh0EgREUgRElTVFJJQlVJw4fDg08gTsODTy1FWENMVVNJVkEKCkNvbSBhIGFwcmVzZW50YcOnw6NvIGRlc3RhIGxpY2Vuw6dhLCB2b2PDqiAobyBhdXRvciAoZXMpIG91IG8gdGl0dWxhciBkb3MgZGlyZWl0b3MgZGUgYXV0b3IpIGNvbmNlZGUgw6AgVW5pdmVyc2lkYWRlCkZlZGVyYWwgZGUgU2FudGEgTWFyaWEgKFVGU00pIG8gZGlyZWl0byBuw6NvLWV4Y2x1c2l2byBkZSByZXByb2R1emlyLCAgdHJhZHV6aXIgKGNvbmZvcm1lIGRlZmluaWRvIGFiYWl4byksIGUvb3UKZGlzdHJpYnVpciBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gKGluY2x1aW5kbyBvIHJlc3VtbykgcG9yIHRvZG8gbyBtdW5kbyBubyBmb3JtYXRvIGltcHJlc3NvIGUgZWxldHLDtG5pY28gZQplbSBxdWFscXVlciBtZWlvLCBpbmNsdWluZG8gb3MgZm9ybWF0b3Mgw6F1ZGlvIG91IHbDrWRlby4KClZvY8OqIGNvbmNvcmRhIHF1ZSBhIFVGU00gcG9kZSwgc2VtIGFsdGVyYXIgbyBjb250ZcO6ZG8sIHRyYW5zcG9yIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbwpwYXJhIHF1YWxxdWVyIG1laW8gb3UgZm9ybWF0byBwYXJhIGZpbnMgZGUgcHJlc2VydmHDp8Ojby4KClZvY8OqIHRhbWLDqW0gY29uY29yZGEgcXVlIGEgVUZTTSBwb2RlIG1hbnRlciBtYWlzIGRlIHVtYSBjw7NwaWEgYSBzdWEgdGVzZSBvdQpkaXNzZXJ0YcOnw6NvIHBhcmEgZmlucyBkZSBzZWd1cmFuw6dhLCBiYWNrLXVwIGUgcHJlc2VydmHDp8Ojby4KClZvY8OqIGRlY2xhcmEgcXVlIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyDDqSBvcmlnaW5hbCBlIHF1ZSB2b2PDqiB0ZW0gbyBwb2RlciBkZSBjb25jZWRlciBvcyBkaXJlaXRvcyBjb250aWRvcwpuZXN0YSBsaWNlbsOnYS4gVm9jw6ogdGFtYsOpbSBkZWNsYXJhIHF1ZSBvIGRlcMOzc2l0byBkYSBzdWEgdGVzZSBvdSBkaXNzZXJ0YcOnw6NvIG7Do28sIHF1ZSBzZWphIGRlIHNldQpjb25oZWNpbWVudG8sIGluZnJpbmdlIGRpcmVpdG9zIGF1dG9yYWlzIGRlIG5pbmd1w6ltLgoKQ2FzbyBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gY29udGVuaGEgbWF0ZXJpYWwgcXVlIHZvY8OqIG7Do28gcG9zc3VpIGEgdGl0dWxhcmlkYWRlIGRvcyBkaXJlaXRvcyBhdXRvcmFpcywgdm9jw6oKZGVjbGFyYSBxdWUgb2J0ZXZlIGEgcGVybWlzc8OjbyBpcnJlc3RyaXRhIGRvIGRldGVudG9yIGRvcyBkaXJlaXRvcyBhdXRvcmFpcyBwYXJhIGNvbmNlZGVyIMOgIFVGU00Kb3MgZGlyZWl0b3MgYXByZXNlbnRhZG9zIG5lc3RhIGxpY2Vuw6dhLCBlIHF1ZSBlc3NlIG1hdGVyaWFsIGRlIHByb3ByaWVkYWRlIGRlIHRlcmNlaXJvcyBlc3TDoSBjbGFyYW1lbnRlCmlkZW50aWZpY2FkbyBlIHJlY29uaGVjaWRvIG5vIHRleHRvIG91IG5vIGNvbnRlw7pkbyBkYSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gb3JhIGRlcG9zaXRhZGEuCgpDQVNPIEEgVEVTRSBPVSBESVNTRVJUQcOHw4NPIE9SQSBERVBPU0lUQURBIFRFTkhBIFNJRE8gUkVTVUxUQURPIERFIFVNIFBBVFJPQ8ONTklPIE9VCkFQT0lPIERFIFVNQSBBR8OKTkNJQSBERSBGT01FTlRPIE9VIE9VVFJPIE9SR0FOSVNNTyBRVUUgTsODTyBTRUpBIEEgVUZTTQosIFZPQ8OKIERFQ0xBUkEgUVVFIFJFU1BFSVRPVSBUT0RPUyBFIFFVQUlTUVVFUiBESVJFSVRPUyBERSBSRVZJU8ODTyBDT01PClRBTULDiU0gQVMgREVNQUlTIE9CUklHQcOHw5VFUyBFWElHSURBUyBQT1IgQ09OVFJBVE8gT1UgQUNPUkRPLgoKQSBVRlNNIHNlIGNvbXByb21ldGUgYSBpZGVudGlmaWNhciBjbGFyYW1lbnRlIG8gc2V1IG5vbWUgKHMpIG91IG8ocykgbm9tZShzKSBkbyhzKQpkZXRlbnRvcihlcykgZG9zIGRpcmVpdG9zIGF1dG9yYWlzIGRhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbywgZSBuw6NvIGZhcsOhIHF1YWxxdWVyIGFsdGVyYcOnw6NvLCBhbMOpbSBkYXF1ZWxhcwpjb25jZWRpZGFzIHBvciBlc3RhIGxpY2Vuw6dhLgoKRepositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132022-06-08T11:34:46Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único |
dc.title.alternative.eng.fl_str_mv |
Evaluation of MIC-DV for decomposition of fish tissue and system development for cold vapor generation in disposable vessel |
title |
Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único |
spellingShingle |
Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único Pardinho, Renan Buque MIC-DV Peixe Frasco único DV-CVG-ICP-MS DV-CVG-AAS Fish Single vessel CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único |
title_full |
Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único |
title_fullStr |
Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único |
title_full_unstemmed |
Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único |
title_sort |
Avaliação da MIC-DV para a decomposição de tecido de peixe e desenvolvimento de sistema para geração de vapor frio em frasco único |
author |
Pardinho, Renan Buque |
author_facet |
Pardinho, Renan Buque |
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.advisor-co1.fl_str_mv |
Bolzan, Rodrigo Cordeiro |
dc.contributor.referee1.fl_str_mv |
Duarte, Fábio Andrei |
dc.contributor.referee2.fl_str_mv |
Barin, Juliano Smanioto |
dc.contributor.referee3.fl_str_mv |
Rodrigues, Luiz Frederico |
dc.contributor.referee4.fl_str_mv |
Mortari, Sergio Roberto |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/0617212620483345 |
dc.contributor.author.fl_str_mv |
Pardinho, Renan Buque |
contributor_str_mv |
Flores, Érico Marlon de Moraes Bolzan, Rodrigo Cordeiro Duarte, Fábio Andrei Barin, Juliano Smanioto Rodrigues, Luiz Frederico Mortari, Sergio Roberto |
dc.subject.por.fl_str_mv |
MIC-DV Peixe Frasco único DV-CVG-ICP-MS DV-CVG-AAS |
topic |
MIC-DV Peixe Frasco único DV-CVG-ICP-MS DV-CVG-AAS Fish Single vessel CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Fish Single vessel |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, microwave-induced combustion in disposable vessel (MIC-DV) was evaluated for the decomposition of fish tissue for the subsequent determination of As, Cd, Cr, Cu, Mn, Pb, Se and V by inductively coupled plasma mass spectrometry (ICP-MS) and Hg in a flow injection system with cold vapor generation coupled with inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS). In addition, a chemical vapor generation system in a disposable vessel (DV-CVG) was proposed, coupled with ICP-MS and atomic absorption spectrometry (AAS) techniques for the determination of Hg. For the development of the method using MIC-DV, the following parameters were evaluated: composition of the absorbing solution (HNO3 and HCl), concentration of HNO3 as an absorbing solution (0.25, 0.5, 1, 3, 5, 7 and 14.4 mol L-¹), sample mass (10, 15, 20, 25 and 30 mg), absorbing solution volume (1, 3, 5 and 7 mL) and successive digestion cycles (2 and 3 times). For the ignition of the sample in the MIC-DV, 40 μL of NH4NO3 10 mol L-¹ were pipetted into a filter paper disc, which was positioned in the quartz holder and the set was inserted in disposable vessel. Before closing, the vessel were purged with O2 for 60 s at a flow rate of 4 L min-¹ and inserted into the microwave oven for irradiation for 30 s. After decomposition by MIC-DV, the digested were stored in a refrigerator until quantification. The results obtained by MIC-DV were compared with those obtained by the methods of microwave-induced combustion (MIC) and microwave assisted wet decomposition (MAWD). The proposed method was applied to 5 samples of fish tissue and to the certified reference material (CRM) of fish liver (DOLT 4) under the following optimized conditions: 5 mL of 0.5 mol L-¹ of HNO3 as an absorbing solution using 10 mg of sample mass with one combustion. Considering the system developed for the determination of Hg (DV-CVG), it uses only the lid of the disposable vessel itself with four holes, which were necessary for the introduction of HCl, NaBH4, carrier gas and for carrying the gas phase from inside the vessel to the determination technique. This system was coupled with the ICP-MS and AAS technique, being called DV-CVG-ICP-MS and DV-CVG-AAS. The agreement for the elements As, Cd, Cr, Hg, Mn, Se and V in the 5 samples and CRM evaluated after the decomposition by MIC-DV, did not show significant difference (ANOVA) when compared with the reference methods and certified values. The MIC-DV limits of quantification (LOQs) for As, Cd, Cr, Hg, Mn, Pb, Se and V were 0.02, 0.05, 0.50, 0.10, 0.19, 0, 7, 0.18, 0.02 μg g-¹, respectively. For As, Cd and Hg, the LOQs were below the maximum limit required by MERCOSUL for fish tissue. The DV-CVG-ICP-MS that uses the adapted cover presented a lower LOQ when compared to the FI-CVG-ICP-MS used as a reference. The LOQs of the system with the adapted lid coupled to ICP-MS and AAS were 0.025 and 1.2 μg g-¹ respectively. Both the MIC-DV method and the DV-CVG systems developed in this work, presented low cost (disregarding the technique used), simplicity of operation, safety for the operator, reduced use of reagents and used for the quality control of inorganic contaminants such as As, Cd, Cr, Hg, Mn, Se and V. |
publishDate |
2021 |
dc.date.issued.fl_str_mv |
2021-02-15 |
dc.date.accessioned.fl_str_mv |
2022-06-08T11:34:46Z |
dc.date.available.fl_str_mv |
2022-06-08T11:34:46Z |
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/1/24658 |
url |
http://repositorio.ufsm.br/handle/1/24658 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 600 600 |
dc.relation.authority.fl_str_mv |
a9c2788c-7913-4d7b-92e1-3429800ac028 d95fe6ca-aa5d-4323-ba0e-ff6e1407ed3c aeaf2656-6542-4955-b951-a92cd5517da5 bedaf96e-f8fc-48ca-820e-6559530109cb 91851857-1b47-4140-8705-5c9a23daaf4d eb5f6555-ee67-449a-ab4f-ae56ae8070f3 ebb296a1-1569-43d1-8946-7cc7e3bec814 |
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: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/1/24658/1/TES_PPGQU%c3%8dMICA_2021_PARDINHO_RENAN.pdf http://repositorio.ufsm.br/bitstream/1/24658/2/license_rdf http://repositorio.ufsm.br/bitstream/1/24658/3/license.txt |
bitstream.checksum.fl_str_mv |
c0b9f4c4d5c989668fa13767c0fb37d6 4460e5956bc1d1639be9ae6146a50347 2f0571ecee68693bd5cd3f17c1e075df |
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_ |
1794524382428659712 |