In-vessel headspace liquid-phase microextraction

A new mode of headspace liquid-phase microextraction termed in-vessel headspace liquid-phase microextraction (IV-HS-LPME) has been developed. A plastic vessel was used as a holder for an extraction phase. Problems with drop stability, limitations in the stirring speed, and too little volume of the acceptor phase have been completely eliminated. The proposed approach is fully compatible with ordinary instruments and microcuvettes used in spectrophotometry. The potential of the method was evaluated by determining the iodide concentration in various samples. Iodide in the donor phase was converted to volatile I₂ by oxidation with 1 mmol L^-1 K₂Cr₂O₇. The reaction mixture was agitated on a magnetic stirrer for 30 min at a stirring speed of 1200 rpm. A 1% (w/v) aqueous solution of KI was used as the acceptor phase. The absorbance of the I₃^- ion formed in the acceptor phase was measured in a 50 μL microcuvette at 350 nm. For the case of extraction from 10 mL donor solution into 50 μL of acceptor phase, the calibration graph is linear in the range of 20-400 μg L^-1 (as I^-) with a detection limit of 6 μg L^-1. The developed method has a high precision comparable to conventional spectrophotometric methods (0.6-1.5%). The extraction efficiency obtained in the optimal conditions was 10.5%. The distribution constants for equilibria between the donor solution and the headspace and between the headspace and the acceptor solution are 0.8 ± 0.1 and 16 ± 2, respectively. The developed method was successfully applied to determine the iodine content in natural waters, medicines and algae.