Rapid determination of lead in water samples by dispersive liquid–liquid microextraction coupled with electrothermal atomic absorption spectrometry

The need for highly reliable methods for the determination of trace and ultratrace elements has been recognized in analytical chemistry and environmental science. A simple and powerful microextraction technique was used for the detection of the lead ultratrace amounts in water samples using the dispersive liquid–liquid microextraction (DLLME), followed by the electrothermal atomic absorption spectrometry (ET AAS). In this microextraction technique, a mixture of 0.50 mL acetone (disperser solvent), containing 35 μL carbon tetrachloride (extraction solvent) and 5 μL diethyldithiophosphoric acid (chelating agent), was rapidly injected by syringe into the 5.00 mL water sample, spiked with lead. In this process, the lead ions reacted with the chelating agent and were extracted into the fine droplets of CCl4. After centrifugation (2 min at 5000 rpm), the fine CCl4 droplets were sedimented at the bottom of the conical test tube (25 ± 1 μL). Then, 20 μL from the sedimented phase, containing the enriched analyte, was determined by ET AAS. The next step was the optimization of various experimental conditions, affecting DLLME, such as the type and the volume of the extraction solvent, the type and the volume of the disperser solvent, the extraction time, the salt effect, pH and the chelating agent amount. Moreover, the effect of the interfering ions on the analytes recovery was also investigated. Under the optimum conditions, the enrichment factor of 150 was obtained from only a 5.00 mL water sample. The calibration graph was linear in the range of 0.05–1 μg L−1 with the detection limit of 0.02 μg L−1. The relative standard deviation (R.S.D.) for seven replicate measurements of 0.50 μg L−1 of lead was 2.5%. The relative lead recoveries in mineral, tap, well and sea water samples at the spiking level of 0.20 and 0.40 μg L−1 varied from 93.5 to 105.0. The characteristics of the proposed method were compared with the cloud point extraction (CPE), the liquid–liquid extraction, the solid phase extraction (SPE), the on-line solid phase extraction (SPE) and the co-precipitation, based on bibliographic data. The main DLLME advantages combined with ET AAS were simplicity of operation, rapidity, low cost, high-enrichment factor, good repeatability, low consumption of extraction solvent, requiring a low sample volume (5.00 mL).