Institute of Chemistry and Technical Electrochemistry, Poznan University of Technology, Piotrowo 3, 60-965 Poznań, Poland.
Talanta. 2013 Oct 15;115:178-83. doi: 10.1016/j.talanta.2013.04.063. Epub 2013 May 2.
In situ synthesis of ionic liquid extractant for dispersive liquid-liquid microextraction (in situ IL DLLME) combined with electrothermal atomic absorption spectrometry (ET AAS) for determination of copper in water samples was developed. Analytical signals were obtained without the back-extraction of copper from the IL phase prior to its determination by AAS. Some essential parameters of the microextraction and detection techniques such as the pH of sample solution, volume of components for in situ synthesis, matrix interferences and main parameters of graphite furnace atomizer have been studied. Under optimal conditions, high extraction efficiency for copper was achieved for the extraction of 0.7 µg L(-1) in 10.0 mL of sample solution employing 8 μL of 1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (HmimNTf2) as the extraction solvent. The detection limit was found as 0.004 µg L(-1) with an enrichment factor of 200. The relative standard deviation (RSD) for seven replicate measurements of 0.7 µg L(-1) in sample solution was 4%. The accuracy of the proposed method was evaluated by analysis of the Certified Reference Materials: NIST SRM 2709 (San Joaquin Soil), NBS SRM 2704 (Buffalo River Sediment), NRCC DOLT-2 (Dogfish Liver) and NIST SRM 1643e (Trace Element in Water). The measured copper contents in the reference materials were in satisfactory agreement with the certified values. The method was successfully applied to analysis of the tap, lake and mineral water samples.
发展了一种将离子液体萃取剂原位合成(原位 IL-DLLME)与电热原子吸收光谱法(ET AAS)相结合,用于水样中铜的测定。在通过 AAS 测定之前,无需将铜从 IL 相中反萃取出来,即可获得分析信号。研究了微萃取和检测技术的一些重要参数,如样品溶液的 pH 值、原位合成的组分体积、基体干扰以及石墨炉原子化器的主要参数。在最佳条件下,采用 8 μL 1-己基-3-甲基咪唑双[(三氟甲基)磺酰基]亚胺(HmimNTf2)作为萃取溶剂,从 10.0 mL 样品溶液中萃取 0.7 µg L(-1)的铜时,可获得较高的萃取效率。检测限为 0.004 µg L(-1),富集因子为 200。在样品溶液中 0.7 µg L(-1) 的七个重复测量的相对标准偏差(RSD)为 4%。通过对 NIST SRM 2709(圣华金土壤)、NBS SRM 2704(布法罗河沉积物)、NRCC DOLT-2(狗鲨肝)和 NIST SRM 1643e(水中微量元素)等标准参考物质的分析,评估了该方法的准确性。所测标准参考物质中的铜含量与证书值相符。该方法成功应用于自来水、湖水和矿泉水样品的分析。