Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry

Detalhes bibliográficos
Autor(a) principal: Ramalhosa, Elsa
Data de Publicação: 2001
Outros Autores: Río-Segade, Susana, Pereira, Eduarda, Vale, Carlos, Duarte, Armando
Tipo de documento: Artigo
Idioma: eng
Título da fonte: Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
Texto Completo: http://hdl.handle.net/10198/3941
Resumo: A simple and rapid procedure for methylmercury extraction from sediments based on microwave-assisted alkaline digestion with methanolic potassium hydroxide was optimized on parameters such as microwave power, extraction time and sample size. Organomercury species were extracted with dichloromethane in hydrochloric acid medium and back-extracted into ultra-pure water. The sediment extracts were injected into an analytical system composed of high-performance liquid chromatography-ultraviolet-post-column oxidation-cold vapour-atomic fluorescence spectrometry (HPLC-UV-PCO-CV-AFS) for methylmercury determination. Quantitative methylmercury recoveries were obtained when 0.15 g of sediment were suspended into 6 mi of 25% m/v methanolic potassium hydroxide and the slurry was exposed to microwave irradiation at 84 W for 2 min. The detection limit of proposed method was 12 ng g(-1) while the relative standard deviation was less than 5%. The method was validated by the analysis of two sediment certified reference materials and the methylmercury concentrations found were in good agreement (95% confidence level) with the certified values.
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spelling Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometryMethylmercuryMicrowave-assisted extractionHPLC-CV-AFSA simple and rapid procedure for methylmercury extraction from sediments based on microwave-assisted alkaline digestion with methanolic potassium hydroxide was optimized on parameters such as microwave power, extraction time and sample size. Organomercury species were extracted with dichloromethane in hydrochloric acid medium and back-extracted into ultra-pure water. The sediment extracts were injected into an analytical system composed of high-performance liquid chromatography-ultraviolet-post-column oxidation-cold vapour-atomic fluorescence spectrometry (HPLC-UV-PCO-CV-AFS) for methylmercury determination. Quantitative methylmercury recoveries were obtained when 0.15 g of sediment were suspended into 6 mi of 25% m/v methanolic potassium hydroxide and the slurry was exposed to microwave irradiation at 84 W for 2 min. The detection limit of proposed method was 12 ng g(-1) while the relative standard deviation was less than 5%. The method was validated by the analysis of two sediment certified reference materials and the methylmercury concentrations found were in good agreement (95% confidence level) with the certified values.The Royal Society of ChemistryBiblioteca Digital do IPBRamalhosa, ElsaRío-Segade, SusanaPereira, EduardaVale, CarlosDuarte, Armando2011-04-04T15:40:49Z20012001-01-01T00:00:00Zinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleapplication/pdfhttp://hdl.handle.net/10198/3941engRamalhosa, Elsa; Río-Segade, Susana; Pereira, Eduarda; Vale, Carlos; Duarte, Armando (2001). Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry. Journal of Analytical Atomic Spectrometry. ISSN 0267-9477. 16:6, p. 643-6470267-947710.1039/b101229finfo:eu-repo/semantics/openAccessreponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãoinstacron:RCAAP2023-11-21T10:09:37Zoai:bibliotecadigital.ipb.pt:10198/3941Portal AgregadorONGhttps://www.rcaap.pt/oai/openaireopendoar:71602024-03-19T22:56:31.461033Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãofalse
dc.title.none.fl_str_mv Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry
title Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry
spellingShingle Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry
Ramalhosa, Elsa
Methylmercury
Microwave-assisted extraction
HPLC-CV-AFS
title_short Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry
title_full Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry
title_fullStr Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry
title_full_unstemmed Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry
title_sort Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry
author Ramalhosa, Elsa
author_facet Ramalhosa, Elsa
Río-Segade, Susana
Pereira, Eduarda
Vale, Carlos
Duarte, Armando
author_role author
author2 Río-Segade, Susana
Pereira, Eduarda
Vale, Carlos
Duarte, Armando
author2_role author
author
author
author
dc.contributor.none.fl_str_mv Biblioteca Digital do IPB
dc.contributor.author.fl_str_mv Ramalhosa, Elsa
Río-Segade, Susana
Pereira, Eduarda
Vale, Carlos
Duarte, Armando
dc.subject.por.fl_str_mv Methylmercury
Microwave-assisted extraction
HPLC-CV-AFS
topic Methylmercury
Microwave-assisted extraction
HPLC-CV-AFS
description A simple and rapid procedure for methylmercury extraction from sediments based on microwave-assisted alkaline digestion with methanolic potassium hydroxide was optimized on parameters such as microwave power, extraction time and sample size. Organomercury species were extracted with dichloromethane in hydrochloric acid medium and back-extracted into ultra-pure water. The sediment extracts were injected into an analytical system composed of high-performance liquid chromatography-ultraviolet-post-column oxidation-cold vapour-atomic fluorescence spectrometry (HPLC-UV-PCO-CV-AFS) for methylmercury determination. Quantitative methylmercury recoveries were obtained when 0.15 g of sediment were suspended into 6 mi of 25% m/v methanolic potassium hydroxide and the slurry was exposed to microwave irradiation at 84 W for 2 min. The detection limit of proposed method was 12 ng g(-1) while the relative standard deviation was less than 5%. The method was validated by the analysis of two sediment certified reference materials and the methylmercury concentrations found were in good agreement (95% confidence level) with the certified values.
publishDate 2001
dc.date.none.fl_str_mv 2001
2001-01-01T00:00:00Z
2011-04-04T15:40:49Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/article
format article
status_str publishedVersion
dc.identifier.uri.fl_str_mv http://hdl.handle.net/10198/3941
url http://hdl.handle.net/10198/3941
dc.language.iso.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv Ramalhosa, Elsa; Río-Segade, Susana; Pereira, Eduarda; Vale, Carlos; Duarte, Armando (2001). Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry. Journal of Analytical Atomic Spectrometry. ISSN 0267-9477. 16:6, p. 643-647
0267-9477
10.1039/b101229f
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 The Royal Society of Chemistry
publisher.none.fl_str_mv The Royal Society of Chemistry
dc.source.none.fl_str_mv reponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação
instacron:RCAAP
instname_str Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação
instacron_str RCAAP
institution RCAAP
reponame_str Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
collection Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
repository.name.fl_str_mv Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação
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