Department of Chemistry, University of Girona, Girona, Spain.
Anal Chim Acta. 2013 Jul 5;786:8-15. doi: 10.1016/j.aca.2013.05.006. Epub 2013 May 13.
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.
在本研究中，考虑到全反射 X 射线光谱法 (TXRF) 的微量分析能力，我们探索了中空纤维液相微萃取 (HF-LPME) 和分散液相微萃取 (DLLME) 与 TXRF 结合用于测定水中低浓度无机 Sb 形态的可能性。对于上述每种 LPME 配置，都仔细评估了影响 Sb 萃取的实验参数，但特别是适当的样品制备过程（反射载体上的沉积体积和干燥模式）和随后 TXRF 分析的测量条件。对于在低 μg L(-1)范围内测定 Sb(III)和 Sb(V)，最佳的分析策略是在 TXRF 分析之前应用 DLLME 模式。所开发的方法成功应用于不同类型加标水样中无机 Sb 形态的测定。
