Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento
Ano de defesa: | 2016 |
---|---|
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: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/17621 |
Resumo: | In this study a sample preparation method using ultrasound-assisted extraction (UAE) for further determination of As, Cd, Cr, Ni and Pb in soil and sediment by inductively coupled plasma mass spectrometry (ICP-MS) was proposed. Elemental characterization was performed after microwave-assisted digestion (MAD), as recommended by methods 3051A and 3052 of United States Environmental Protection Agency (EPA). The digest was used for determination of Cd, Cr, Ni and Pb by ICP-MS and As was determined by graphite furnace atomic absorption spectrometry (GF AAS). These results were used as reference values during optimization of proposed UAE method. For UAE, three different ultrasound systems (bath, cup horn and probes) were evaluated and the optimization of analytes extraction was carried out using the soil sample. Some variables such as extraction time, temperature, amplitude, frequency, sample mass and extraction solutions were investigated. Initially, univariate experiments were applied in order to determine which variables presents higher influence on extraction efficiency. However, due to the high number of variables and the difficulty to found a compromise extraction condition for all analytes, the application of a multivariate factorial design was required. In this sense, three types of factorial design were applied: 25-1 fractional factorial design, 23 full factorial design and the central composite design (CCD), varying temperature, sample mass, extraction solution, sonication time and amplitude as variables. These experiments were applied in cup horn systems (130 and 750 W). For bath systems, a mapping with aluminum foil was performed. The frequency of baths was also evaluated for all equipments and the baths with 100 and 200 W were selected to apply the 23 factorial design and CCD. After the optimization, the experiments were carried out for analytes extraction in order to evaluate the precision and accuracy of the proposed method. Thus, using the ultrasonic bath of 200 W and 35 kHz, the method was applied to soil and sediment samples and four certified reference materials (CRMs). For determination of As, Cd, Cr, Ni and Pb in soil, sediment and CRMs (except Cr in sediment ant CRMs) by ICP-MS, no statistical difference (Student t-test, p < 0,05) was observed comparing to reference method. The UAE method was also compared with extraction by mechanical stirring and better extraction efficiency was observed for UAE method. In order to check the effects of ultrasound on the surface of samples, they were also characterized by scanning electron microscopy before and after UAE. The limits of detection of the proposed method for the determination of As, Cd, Cr, Ni and Pb by ICP-MS were 75, 2, 174, 156 and 24 ng g-1, respectively. |
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2019-07-30T22:12:47Z2019-07-30T22:12:47Z2016-03-10http://repositorio.ufsm.br/handle/1/17621In this study a sample preparation method using ultrasound-assisted extraction (UAE) for further determination of As, Cd, Cr, Ni and Pb in soil and sediment by inductively coupled plasma mass spectrometry (ICP-MS) was proposed. Elemental characterization was performed after microwave-assisted digestion (MAD), as recommended by methods 3051A and 3052 of United States Environmental Protection Agency (EPA). The digest was used for determination of Cd, Cr, Ni and Pb by ICP-MS and As was determined by graphite furnace atomic absorption spectrometry (GF AAS). These results were used as reference values during optimization of proposed UAE method. For UAE, three different ultrasound systems (bath, cup horn and probes) were evaluated and the optimization of analytes extraction was carried out using the soil sample. Some variables such as extraction time, temperature, amplitude, frequency, sample mass and extraction solutions were investigated. Initially, univariate experiments were applied in order to determine which variables presents higher influence on extraction efficiency. However, due to the high number of variables and the difficulty to found a compromise extraction condition for all analytes, the application of a multivariate factorial design was required. In this sense, three types of factorial design were applied: 25-1 fractional factorial design, 23 full factorial design and the central composite design (CCD), varying temperature, sample mass, extraction solution, sonication time and amplitude as variables. These experiments were applied in cup horn systems (130 and 750 W). For bath systems, a mapping with aluminum foil was performed. The frequency of baths was also evaluated for all equipments and the baths with 100 and 200 W were selected to apply the 23 factorial design and CCD. After the optimization, the experiments were carried out for analytes extraction in order to evaluate the precision and accuracy of the proposed method. Thus, using the ultrasonic bath of 200 W and 35 kHz, the method was applied to soil and sediment samples and four certified reference materials (CRMs). For determination of As, Cd, Cr, Ni and Pb in soil, sediment and CRMs (except Cr in sediment ant CRMs) by ICP-MS, no statistical difference (Student t-test, p < 0,05) was observed comparing to reference method. The UAE method was also compared with extraction by mechanical stirring and better extraction efficiency was observed for UAE method. In order to check the effects of ultrasound on the surface of samples, they were also characterized by scanning electron microscopy before and after UAE. The limits of detection of the proposed method for the determination of As, Cd, Cr, Ni and Pb by ICP-MS were 75, 2, 174, 156 and 24 ng g-1, respectively.Neste trabalho foi proposto um método de preparo de amostra empregando a extração assistida por ultrassom (UAE) para posterior determinação de As, Cd, Cr, Ni e Pb em solo e sedimento por espectrometria de massa com plasma indutivamente acoplado (ICP-MS). A caracterização elementar foi feita após digestão assistida por radiação micro-ondas (MAD), de acordo com o procedimento proposto nos métodos 3051A e 3052 da Agência de Proteção Ambiental dos Estados Unidos (EPA). A determinação de Cd, Cr, Ni e Pb nos digeridos por MAD foi feita por ICP-MS e a determinação de As foi feita por espectrometria de absorção atômica com forno de grafite (GF AAS). Estes resultados foram utilizados como referência para o método proposto. A UAE foi avaliada empregando três diferentes sistemas de ultrassom, banho, cup horn e sonda. Cabe destacar que as otimizações foram feitas somente com a amostra de solo. Diferentes variáveis foram estudadas, tais como tempo, temperatura, amplitude, frequência, massa de amostra e soluções extratoras. Inicialmente, foram aplicados ensaios univariados com o objetivo de verificar quais variáveis apresentavam maior influência nos sistemas. Entretanto, devido ao grande número de variáveis e da dificuldade em encontrar uma condição de extração similar para todos os analitos, foi necessária a aplicação de um planejamento multivariado. Nesse sentido, foram aplicados três tipos de delineamento: delineamento fatorial fracionado 25-1, fatorial completo 23 e o delineamento composto central rotacional (DCCR), utilizando como variáveis temperatura, massa de amostra, solução extratora, tempo de sonicação e amplitude. Essas avaliações foram aplicadas para os sistemas de cup horn de 130 e 750 W. Para os sistemas de banhos, foi feito mapeamento com papel alumínio, bem como a avaliação das frequências e os banhos de 100 e 200 W foram selecionados para aplicação do planejamento fatorial 23 e DCCR. Após otimizada a melhor condição para extração dos analitos, foram feitos experimentos nesta condição, de forma a avaliar a precisão e a exatidão do método. Utilizando o banho ultrassônico de 200 W e 35 kHz, o método foi aplicado para solo e sedimento e para quatro materiais de referência certificados (CRMs). Os resultados para As, Cd, Cr, Ni e Pb em solo, sedimento e CRMs (com exceção de Cr no sedimento e CRMs), após determinação por ICP-MS, não apresentaram diferença significativa (teste t-student, p < 0,05) quando comparados com os valores de referência obtido pelos métodos de comparação. A UAE foi também comparada com extração por agitação mecânica e mostrou melhor eficiência na extração dos analitos. A fim de verificar os efeitos provocados pelo ultrassom na superfície dos sólidos as amostras foram caracterizadas por microscopia eletrônica de varredura (MEV), antes e após a UAE. Os limites de detecção do método proposto para As, Cd, Cr, Ni e Pb por ICP-MS foram de 75, 2, 174, 156 e 24 ng g-1, respectivamente.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/openAccessUltrassomSolosSedimentosQuímicaQuímica analíticaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAvaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimentoinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisDuarte, Fábio Andreihttp://lattes.cnpq.br/3503633944419329Flores, Éder Lisandro de Moraeshttp://lattes.cnpq.br/1947122730060457Barin, Juliano Smaniotohttp://lattes.cnpq.br/7545847424095994http://lattes.cnpq.br/2739532786356266Dalla Vecchia, Paula100600000000600218323ac-81fc-4a7a-93bc-4536cd06202fa4d50395-496f-4c14-858a-82e322f21a6544b2e8e0-9f59-4bfc-9a22-9662db92dac891851857-1b47-4140-8705-5c9a23daaf4dreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento |
title |
Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento |
spellingShingle |
Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento Dalla Vecchia, Paula Ultrassom Solos Sedimentos Química Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento |
title_full |
Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento |
title_fullStr |
Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento |
title_full_unstemmed |
Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento |
title_sort |
Avaliação de diferentes sistemas de extração assistida por ultrassom para determinação de As, Cd, Cr, Ni e Pb em solo e sedimento |
author |
Dalla Vecchia, Paula |
author_facet |
Dalla Vecchia, Paula |
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.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/1947122730060457 |
dc.contributor.referee2.fl_str_mv |
Barin, Juliano Smanioto |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/7545847424095994 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/2739532786356266 |
dc.contributor.author.fl_str_mv |
Dalla Vecchia, Paula |
contributor_str_mv |
Duarte, Fábio Andrei Flores, Éder Lisandro de Moraes Barin, Juliano Smanioto |
dc.subject.por.fl_str_mv |
Ultrassom Solos Sedimentos Química Química analítica |
topic |
Ultrassom Solos Sedimentos Química Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this study a sample preparation method using ultrasound-assisted extraction (UAE) for further determination of As, Cd, Cr, Ni and Pb in soil and sediment by inductively coupled plasma mass spectrometry (ICP-MS) was proposed. Elemental characterization was performed after microwave-assisted digestion (MAD), as recommended by methods 3051A and 3052 of United States Environmental Protection Agency (EPA). The digest was used for determination of Cd, Cr, Ni and Pb by ICP-MS and As was determined by graphite furnace atomic absorption spectrometry (GF AAS). These results were used as reference values during optimization of proposed UAE method. For UAE, three different ultrasound systems (bath, cup horn and probes) were evaluated and the optimization of analytes extraction was carried out using the soil sample. Some variables such as extraction time, temperature, amplitude, frequency, sample mass and extraction solutions were investigated. Initially, univariate experiments were applied in order to determine which variables presents higher influence on extraction efficiency. However, due to the high number of variables and the difficulty to found a compromise extraction condition for all analytes, the application of a multivariate factorial design was required. In this sense, three types of factorial design were applied: 25-1 fractional factorial design, 23 full factorial design and the central composite design (CCD), varying temperature, sample mass, extraction solution, sonication time and amplitude as variables. These experiments were applied in cup horn systems (130 and 750 W). For bath systems, a mapping with aluminum foil was performed. The frequency of baths was also evaluated for all equipments and the baths with 100 and 200 W were selected to apply the 23 factorial design and CCD. After the optimization, the experiments were carried out for analytes extraction in order to evaluate the precision and accuracy of the proposed method. Thus, using the ultrasonic bath of 200 W and 35 kHz, the method was applied to soil and sediment samples and four certified reference materials (CRMs). For determination of As, Cd, Cr, Ni and Pb in soil, sediment and CRMs (except Cr in sediment ant CRMs) by ICP-MS, no statistical difference (Student t-test, p < 0,05) was observed comparing to reference method. The UAE method was also compared with extraction by mechanical stirring and better extraction efficiency was observed for UAE method. In order to check the effects of ultrasound on the surface of samples, they were also characterized by scanning electron microscopy before and after UAE. The limits of detection of the proposed method for the determination of As, Cd, Cr, Ni and Pb by ICP-MS were 75, 2, 174, 156 and 24 ng g-1, respectively. |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-03-10 |
dc.date.accessioned.fl_str_mv |
2019-07-30T22:12:47Z |
dc.date.available.fl_str_mv |
2019-07-30T22:12:47Z |
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/1/17621 |
url |
http://repositorio.ufsm.br/handle/1/17621 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
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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UFSM |
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