Liquid phase microextraction strategies combined with total reflection X-ray spectrometry for the determination of low amounts of inorganic antimony species in waters

• Combination of HF-LPME and DLLME procedures with TXRF.
• Determination of low amounts of inorganic antimony species in waters.
• The detection limit (0.09 μg L−1 Sb) using the DLLME–TXRF system meets legislation requirements.

In the present study, and taking into account the microanalytical capability of total reflection X-ray spectrometry (TXRF), we explored the possibilities of hollow fibre liquid-phase microextraction (HF-LPME) and dispersive liquid–liquid microextraction (DLLME) combined with TXRF for the determination of low amounts of inorganic Sb species in waters.For each of the LPME configurations aforementioned, experimental parameters affecting Sb extraction but specially the proper sample preparation process (deposition volume on the reflective carrier and drying mode) and measurement conditions for subsequent TXRF analysis have been carefully evaluated.The best analytical strategy for the determination of Sb(III) and Sb(V) in the low μg L−1 range was found to be the application of the DLLME mode before TXRF analysis. The developed methodology was successfully applied to the determination of inorganic Sb speciation in different types of spiked water samples.

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