Analytical capabilities of two-phase hollow- ber liquid phase microextraction fortrace multielement determination in aqueous samples by means of portable totalre ection X-ray instrumentation

Liquid phase microextraction (LPME) procedures have been widely used in combination with atomic andemission spectroscopic techniques for the isolation and preconcentration of trace elements. However, its applicationin combination with total re ection X-ray spectrometry (TXRF) is still scarce. In this paper, we evaluate the possi-bilities and drawbacks of a two-phase hollow ber LPME procedure in combination with TXRF for the simultaneousdetermination of trace amounts of Cr, Ni, Cu, Zn, Pb, and Cd in aqueous samples.After extraction of the analytes by using the optimum conditions (sample volume: 25 mL, complexing agent:APDC, organic solvent: hexylbenzene, extraction time: 2 h, extraction speed: 660 rpm), 10 L of the preconcentratedsample was deposited on a preheated quartz re ector, dried on a hot plate at 80◦C, and analyzed by TXRF. Using suchconditions, limits of detection lower than 3 g L1were obtained for all metals.In spite of LODs improvement in comparison with the direct analysis of the aqueous samples (up to a factor of100), precision of the results was not optimal (RSD 20%). This fact may be related to the use of a low volatility solventas extractant phase that hampers the later TXRF analysis.

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