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Master's Dissertation
DOI
https://doi.org/10.11606/D.64.2009.tde-10122009-151257
Document
Author
Full name
Jéssica Correia Ramella
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
Piracicaba, 2009
Supervisor
Committee
Rosias, Maria Fernanda Georgina Gine (President)
Miranda, Carlos Eduardo Saraiva
Veiga, Márcia Andreia Mesquita Silva da
Title in Portuguese
Comparação das metodologias de extração no ponto nuvem e extração em fase sólida para a determinação de cádmio em amostras de águas
Keywords in Portuguese
1-(2-Tiazolilazo)-2-naftol
Amostras de águas
Cádmio
Extração em fase sólida
Extração no ponto nuvem
O,O-Dietilditiofosfato
Pré-concentração
Abstract in Portuguese
Apresenta-se a comparação de duas metodologias para pré-concentração e determinação de Cd em amostras de águas estuarinas e água de mar. As metodologias comparadas foram a extração líquido-líquido no ponto nuvem e a extração por retenção dos analitos em fase sólida. Em ambos os métodos houve necessidade de formação de complexos de Cd previamente à extração. Dois agentes complexantes foram testados o O-O dietilditiofosfato (DDTP), e 1-(2- tiazolilazo)-2-naftol (TAN). A extração no ponto nuvem foi realizada utilizando o surfactante não iônico octil fenoxipolietoxietanol (Triton X-114) que à temperatura de '40 graus'C forma uma fase micelar viscosa de volume reduzido. Após separação das micelas, estas foram dissolvidas em solução de ácido nítrico facilitando a análise por ICP OES. A pré-concentração em fase sólida por retenção dos íons complexados foi realizada colocando-se uma coluna de Amberlite XAD 4 em sistema em fluxo. Foram ajustadas as vazões de carregamento da coluna e eluição de forma a aumentar os fatores de pré-concentração. Os volumes das soluções finais foram de 2 mL de forma a obter resultados em triplicata na análise por ICP OES. A quantificação foi efetuada pelo método das adições de padrão. Os dois procedimentos foram comparados considerando as eficiências relativas de pré-concentração, a facilidade para efetuar os procedimentos e a percentagem de recuperação das medidas
Title in English
Comparison of methodologies for cloud point extraction and solid phase extraction for determination of cadmium in water samples
Keywords in English
1-(2-Thiazolylazo)-2-naphthol
Cadmium
Cloud point extraction
O,O-Diethyl dithiophosphate
Pre-concentration
Samples of water
Solid phase extraction
Abstract in English
Two methodologies for determination of Cd in estuarine and seawater samples were studied. The methodologies for pre-concentration of analytes by surfactant-mediated cloud point extraction and solid phase retention in a resin column were compared. In both cases the prior formation of Cd ions complexes with O,O-diethyldithiophosphate (DDTP) and 1-(2-thiazolylazo)-2-naphtol (TAN) was carried out. The Cloud point extraction was attained with the non ionic surfactant ctylphenoxypolyethoxyethanol (Triton X-114) at '40 graus'C . The reduced volume of surfactant micelles was easily separated and dissolved using the solution containing nitric acid which facilitate the analysis by ICP OES. The solid phase pre-concentration was performed by retention of the complexed ions in the Amberlite XAD 4 resin column in a flow scheme. The flow-rates for sample loading and elution were adjusted to increase the preconcentration factor. The final volumes collected of 2 mL were further analyzed in triplicate by ICP OES. Quantification was performed by the standard addition method. Both pre-concentration procedures were compared considering the relative efficiencies, the complexity of procedures and recovery percent of results
 
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Errata_JCRAMELLA.pdf (10.46 Kbytes)
Publishing Date
2009-12-14
 
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