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Doctoral Thesis
DOI
https://doi.org/10.11606/T.46.2006.tde-20092006-125755
Document
Author
Full name
Luciana Bagdeve de Oliveira dos Santos
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2006
Supervisor
Committee
Masini, Jorge Cesar (President)
Abate, Gilberto
Cavicchioli, Andrea
Tavares, Marina Franco Maggi
Zanoni, Maria Valnice Boldrin
Title in Portuguese
Desenvolvimento de metodologias para determinação de resíduos de atrazina em solos e águas naturais empregando técnicas eletroanalíticas.
Keywords in Portuguese
águas naturais/análise
atrazina
resíduos/determinação
solo/análise
Abstract in Portuguese
Esta tese descreve o desenvolvimento de metodologias eletroanalíticas, em especial a voltametria de onda quadrada com o eletrodo de gota pendente de Hg, para determinação de atrazina em águas de rios do Estados de São Paulo e em amostras de solo. A exatidão das metodologias foi avaliada por comparação com HPLC e estudos de recuperação. Inicialmente desenvolveu-se o método em modo estático, no qual a maior sensibilidade foi obtida em pH 2 e freqüência de 400 Hz, com limites de detecção e determinação de 2 e 10 microgramas L-1, respectivamente. O estudo do comportamento eletroquímico revelou que a atrazina comporta-se reversivelmente em altas freqüências de onda quadrada. Dentre os metabólitos da atrazina, a desetilatrazina e desiosopropilatrazina, também são eletroativas nas condições estudadas, sendo possíveis interferentes, ao contrário da hidroxiatrazina e didealquilatrazina. Sistemas em fluxo contínuo e de injeção seqüencial foram desenvolvidos para determinação de atrazina em extrato de solo e águas naturais, bem como em estudos de adsorção. Em águas, os limites de detecção e determinação obtidos por injeção seqüencial foram de 4,5 e 15 microgramas L-1. Estudos de adsorção revelaram que atrazina liga-se mais fortemente a solos em meios ácidos. As metodologias em fluxo permitiram um significativo aumento da velocidade analítica e economia de reagentes, automatizando as determinações.
Title in English
Development of methodologies for determination of residues of atrazine in soil and natural waters employing electroanalytical techniques.
Keywords in English
atrazine
natural water/analysis
residues/determination
soil/analysis
Abstract in English
This thesis describes the development of electroanalytical methodologies, especially the square wave voltammetry with the hanging mercury drop electrode, for determination of the herbicide atrazine in river waters of the São Paulo state and soil samples. The accuracy of the methodologies was evaluated by comparison with HPLC and recovery studies. Initially, a stationary method was developed, in which the highest sensitivity was attained at pH 2 and at frequency of 400 Hz, with detection and quantification limits of 2 and 10 micrograms L-1, respectively. The electrochemical behavior of atrazine was reversible at the higher square wave frequencies. Among the atrazine metabolites, deethylatrazine and deisopropylatrazine are also electroactive under the studied conditions, being possible interferences, contrary to hydroxyatrazine and didealkylatrazine. Continuous flow and sequential injection systems were developed for determination of atrazine in soil extracts and natural waters, as well as in adsorption studies. In waters, the detection and quantification limits attained by sequential injection were 4.5 and 15 micrograms L-1. Adsorption studies showed that atrazine binds more strongly to soil in acidic media. The flow analysis methodologies lead to significant increase in the sampling throughput and reagent saving, automating the determinations.
 
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Publishing Date
2006-12-05
 
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