Determination of chromium(VI) and lead in water samples by on-line sorption preconcentration coupled with flame atomic absorption spectrometry using a PCTFE-beads packed column

Abstract

A new time-based flow injection on-line solid phase extraction method for chromium(VI) and lead determination using flame atomic absorption spectrometry was developed. The use of hydrophobic poly-chlorotrifluoroethylene (PCTFE)-beads as absorbent in on-line preconcentration system was evaluated. Effective formation of ammonium pyrrolidine dithiocarbamate complexes and subsequently retention in PCTFE packed column, was achieved in pH range 1.0–1.6 and 1.5–3.2 for Cr(VI) and Pb(II) ions, respectively. The sorbed analyte was efficiently eluted with isobutyl-methyl-ketone for on-line FAAS determination. The proposed packing material exhibited excellent chemical and mechanical resistance, fast kinetics for adsorption of Cr(VI) and Pb(II) permitting the use of high sample flow rates at least up to 15 mL min −1 without loss of retention efficiency. For a preconcentration time of 90 s, the sample frequency was 30 h −1, the enhancement factor was 94 and 220, the detection limit was 0.4 and 1.2 μg L −1, while the precision (R.S.D.) was 1.8% (at 5 μg L −1) and 2.1% (at 30 μg L −1) for chromium(VI) and lead, respectively. The applicability and the accuracy of the developed method were estimated by the analysis spiked water samples and certified reference material NIST-CRM 1643d (Trace elements in water) and NIST-SRM 2109 (chromium(VI) speciation in water).