On-line liquid–liquid extraction system using a new phase separator for flame atomic absorption spectrometric determination of ultra-trace cadmium in natural waters

Abstract

A robust flow injection (FI) on-line liquid–liquid extraction (LLE) preconcentration/separation system associated with a newly designed gravitational phase separator, coupled to flame atomic absorption spectrometry (FAAS) was developed. The performance of the system was illustrated for cadmium determination at the μg l −1 level. The non-charged cadmium complex with ammonium pyrrolidine dithiocarbamate (APDC) was extracted on-line into isobutyl methyl ketone (IBMK). The organic phase was effectively separated from a large volume of aqueous phase and is led into a 100 μl loop of an injection valve before its introduction into the nebulizer. The system was optimized and offered good performance characteristics with unlimited life time of phase separator, greater flow rate ratios and improved flexibility, as compared with other solvent extraction preconcentration systems. With a sampling frequency of 33 h −1, the enhancement factor was 155, the detection limit was 0.02 μg l −1, the relative standard deviation was 3.2% at 2.0 μg l −1 Cd concentration level and the calibration curve was linear over the concentration range 0.06–6.0 μg l −1. The accuracy of the proposed method was evaluated by analyzing a certified reference material of water and by recovery measurements on spiked samples. Finally, it was successfully applied to the analysis of tapwater, river and seawater samples.