An automatic countercurrent liquid–liquid micro-extraction system coupled with atomic absorption spectrometry for metal determination

• Solvent microextraction based on countercurrent flow for metal preconcentration.
• Automatic sequential injection countercurrent platform coupled with FAAS.
• Design and study of a flow-through extraction chamber.
• Organic solvents heavier or lighter than water can be easily used.
• Determination of lead in water samples.

A novel and versatile automatic sequential injection countercurrent liquid–liquid microextraction (SI-CC-LLME) system coupled with atomic absorption spectrometry (FAAS) is presented for metal determination. The extraction procedure was based on the countercurrent flow of aqueous and organic phases which takes place into a newly designed lab made microextraction chamber. A noteworthy feature of the extraction chamber is that it can be utilized for organic solvents heavier or lighter than water. The proposed method was successfully demonstrated for on-line lead determination and applied in environmental water samples using an amount of 120 μL of chloroform as extractant and ammonium diethyldithiophosphate as chelating reagent. The effect of the major experimental parameters including the volume of extractant, as well as the flow rate of aqueous and organic phases were studied and optimized. Under the optimum conditions for 6 mL sample consumption an enhancement factor of 130 was obtained. The detection limit was 1.5 μg L−1 and the precision of the method, expressed as relative standard deviation (RSD) was 2.7% at 40.0 μg L−1 Pb(II) concentration level. The proposed method was evaluated by analyzing certified reference materials and spiked environmental water samples.

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