Preconcentration of lead complexed with O,O-diethyl-dithiophosphate by column solid-phase extraction using different sorbents in a flow injection system coupled to a flame atomic absorption spectrometer

A comparative study of C-18 immobilized on silica, activated carbon and a p olyurethane foam, as sorbents for Pb complexed with O,O-diethyl-dithiophosp hate in a flow injection preconcentration system is reported. The complex w as formed in 1.0 M HCl medium and processed in a simple system using a peri staltic pump, a manual injector-commutator and a mini-column filled with th e sorbent. Using ethanol as eluent, the richest 150-mul fraction was collec ted and measured (after discarding 150, 200 and 0 mul for the activated car bon, foam and C-18, respectively) by flame atomic absorption spectrometry. The optimum concentration of the complexing agent was 0.05%, m/v for C-18 a nd 0.2% m/v for the activated carbon and the polyurethane foam. The best sa mple loading Row rate was 4.0 mi min (-1) for the activated carbon and 2.0 mi min (-1) for C-18, and the polyurethane foam, while the best elution Row rate was 1.0 mi min(-1) (activated carbon) and 0.6 mi min (-1) (C-18 and f oam). It was found that beyond a certain loading sample volume, for a const ant analyte mass, the signal decreased. The maximum loading sample volume, for a constant analyte mass, before the signal started to decrease, was 50 mi for the activated carbon and 150 mi for the other materials. By processi ng 25 mi, the enrichment factors were 23, 55 and 166 for the activated carb on, foam and C-18, respectively. The best limit of detection (3 sigma) was 0.3 mug l(-1) for the C-18 (1.2 mug l(-1) for the foam and 3 mug l(-1) for the activated carbon). As shown, the C-18 has a much superior retention per formance in comparison to the other two materials. (C) 2001 Elsevier Scienc e B.V. All rights reserved.