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

• Published in: Talanta (Oxford) 2001-05, Vol.54 (4), p.687-696
• Main Authors: Quináia, Sueli Pércio, Borba da Silva, José Bento, Ezequiel Rollemberg, Maria do Carmo, Curtius, Adilson José
• Format: Article
• Language: English
• Subjects: Activated Carbon; Analytical chemistry; Atomic absorption spectrometry; C 18 immobilized on silica; Chemistry; Exact sciences and technology; Lead; Polyurethane foam; Preconcentration; Spectrometric and optical methods
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/S0039-9140(01)00326-5

A comparative study of C 18 immobilized on silica, activated carbon and a polyurethane foam, as sorbents for Pb complexed with O,O-diethyl-dithiophosphate in a flow injection preconcentration system is reported. The complex was formed in 1.0 M HCl medium and processed in a simple system using a peristaltic pump, a manual injector–commutator and a mini-column filled with the sorbent. Using ethanol as eluent, the richest 150-μl fraction was collected and measured (after discarding 150, 200 and 0 μl for the activated carbon, 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 and 0.2% m/v for the activated carbon and the polyurethane foam. The best sample loading flow rate was 4.0 ml min −1 for the activated carbon and 2.0 ml min −1 for C 18 and the polyurethane foam, while the best elution flow rate was 1.0 ml min −1 (activated carbon) and 0.6 ml min −1 (C 18 and foam). It was found that beyond a certain loading sample volume, for a constant analyte mass, the signal decreased. The maximum loading sample volume, for a constant analyte mass, before the signal started to decrease, was 50 ml for the activated carbon and 150 ml for the other materials. By processing 25 ml, the enrichment factors were 23, 55 and 166 for the activated carbon, foam and C 18, respectively. The best limit of detection (3σ) was 0.3 μg l −1 for the C 18 (1.2 μg l −1 for the foam and 3 μg l −1 for the activated carbon). As shown, the C 18 has a much superior retention performance in comparison to the other two materials.