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Master's Dissertation
DOI
https://doi.org/10.11606/D.11.1982.tde-20210918-212036
Document
Author
Full name
Arquimedes Lavorenti
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
Piracicaba, 1981
Supervisor
Title in Portuguese
A determinação de selênio por fluorimetria
Keywords in Portuguese
DETERMINAÇÃO
FLUOROMETRIA
SELÊNIO
Abstract in Portuguese
Foi desenvolvido um método fluorimétrico para a determinação de selênio em amostras vegetais e soro de sangue. O método empregou inicialmente o radioisótopo <sup>75</sup>Se para atingir as condições analíticas de determinação. Foram estudados três processos de digestão de amostras e alguns fatores relativos à metodologia. Com o processo de digestão nítrico-perclórica, cerca de 40 amostras podem ser analisadas diariamente com relativa facilidade. Foi adicionado HCl (1+9) ao digerido e submetido ao banho-maria a 90°C por 30 minutos. O procedimento analítico básico consistiu na reação do selênio com 2,3-diaminonaftaleno (DAN) 4 x 10<sup>-3</sup>M a pH 2 durante 60 minutos a 70°C e extração do complexo Se-DAN com ciclohexano. O método proposto apresentou um coeficiente de variação em torno de 9%, uma recuperação média superior a 90% e uma exatidão considerada excelente.
Title in English
Selenium determination by fluorimetry
Abstract in English
A fluorimetric method was developed to determine selenium both in vegetal samples and blood serum. The method consists of a radioisotope <sup>75</sup>Se initially in order to optimize the determination of analytical conditions. Three samples digestion processes were studied and also some factors related to methodology. Thanks to the nitric-percloric digestion process, around 40 samples can be analyzed daily in a relatively easy way. HCl (1+9) was added to the digested material and submitted to water-bath at 90°C during 30 minutes. The basic analytical process consisted of the selenium reaction with 2,3- diaminonaphthalene (DAN) 4 x 10<sup>-3</sup>M at 2 pH during 60 minutes at 70°C and extraction of Se-DAN complex with cyclohexane. The proposed method showed a coefficient of variation of about 9%, an average recovery superior to 90% and excellent accuracy.
 
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Publishing Date
2021-09-18
 
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