NDLI: Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

Content Provider	Scientific Electronic Library Online (SciELO)
Author	Andrada, Daniel Pinto, Frederico G. Magalhães, Cristina Gonçalves Nunes, Berta R. Franco, Milton B. Silva, José Bento Borba da
Abstract	The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ET AAS). Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 µL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO3 1% v/v and 0.02% v/v of cetil trimethyl ammonium chloride (CTAC) were prepared directly in the autosampler cups and placed into the graphite furnace. For modifiers in solutions 10 µL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 µg), the best pyrolysis and atomization temperatures were 900 and 1600 ºC, respectively, with a characteristic mass of 12 pg (recommended of 10 pg), with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence) for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh) and between 93.9 and 105.2% (Zr+Rh). In both recovery studies, the relative standard deviation (n=3) was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r² higher than 0.99. The limits of detection were 0.7 µg L-1 for serum samples, with Zr+Rh permanent, and 1.0 µg L-1 for urine with iridium permanent.
Related Links	http://www.scielo.br/scielo.php?script=sci_abstract&pid=S0103-50532006000200016&lng=en&nrm=iso http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532006000200016&lng=en&nrm=iso
Starting Page	328
Ending Page	332
Page Count	5
File Format	PDF
ISSN	01035053
DOI	10.1590/S0103-50532006000200016
Journal	Journal of the Brazilian Chemical Society
Issue Number	2
Volume Number	17
Language	English
Publisher	Sociedade Brasileira de Química
Publisher Date	2006-04-01
Publisher Institution	Universidade Federal de Minas Gerais Departamento de Química Centro de Desenvolvimento de Tecnologia Nuclear Laboratório de Absorção Atômica
Publisher Place	Brazil
Access Restriction	Open
Subject Keyword	Electrothermal atomic absorption spectrometry Lead Urine Serum Iridium Iridium plus rhodium Permanent modifier
Content Type	Text
Resource Type	Article
Subject	Chemistry

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