02272naa a2200253 a 450000100080000000500110000800800410001910000180006024501580007826000090023652014950024565000110174065000120175165300310176365300240179465300140181865300130183270000190184570000280186470000240189270000190191670000160193577300670195110155242017-07-26 2004 bl uuuu u00u1 u #d1 aMALTEZ, H. F. aA comparative study of homemade C18 and commercial C18 sorbents for preconcentration of lead by minicolumn solid phase extraction.h[electronic resource] c2004 aA comparative study of commercial C18 chemically immobilized on silica and homemade C18, as sorbents for Pb complexed with O,O-diethyl-dithiophosphate (DDTP) in a flow injection preconcentration system is reported. The homemade C18 sorbent was obtained by sorption of poly(methyloctadecylsiloxane) (PMODS) on the silica support followed by immobilization using thermal treatment. The method follows the concept of green chemistry, since there are no toxic residues after synthesis. The complexed Pb was formed in 1.0molL-1 HCl medium and retained on the minicolumn filled with the sorbents. The elution was carried out using ethanol, and the richest 210µL fraction was collected and analyzed by flame atomic absorption spectrometry. Chemical and flow variables were optimized for each sorbent. The results demonstrated that the performance of the proposed homemade C18 sorbent for preconcentration of Pb complexed with DDTP is very similar to commercial C18 chemically bonded on silica. By processing 25mL, the enrichment factors were 129 and 125 for commercial C18 and homemade C18, respectively. The limit of detection for commercial and homemade C18 was 0.2µgL-1 and 0.6µgL-1, respectively. The relative standard deviation (RSD) was lower than 1.2% for both sorbents for a Pb concentration of 100µgL-1. The method was also applied successfully to the analysis of water samples, and the accuracy was tested by recovery measurements on spiked samples and biological reference material. aChumbo aMétodo aExtração em fase sólida aPré-concentração aResíduos aTécnica1 aMELO, L. F. C.1 aQUEIROZ, S. C. do N. de1 aJARDIM, I. C. S. F.1 aCURTIUS, A. J.1 aCARASEK, E. tMicrochimica Acta, Viennagv. 144, n. 1-3, p.17-21, jan. 2004.