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浊点萃取后激光诱导热透镜光谱法测定痕量钯。

Laser induced-thermal lens spectrometry after cloud point extraction for the determination of trace amounts of palladium.

机构信息

Department of Analytical Chemistry, Chemistry & Chemical Engineering Research Center of Iran, PO Box 14335-186, Tehran, Iran.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2009 Oct 15;74(3):761-6. doi: 10.1016/j.saa.2009.08.013. Epub 2009 Aug 13.

Abstract

Cloud point extraction (CPE) in combination with thermal lens spectrometry (TLS) has been developed for the preconcentration and determination of palladium. TLS and CPE methods have good matching conditions for the combination because TLS is a suitable method for the analysis of low volume samples obtained after CPE. Palladium was complexed with 1-(2-pyridylazo)-2-naphthol (PAN) as a complexing agent in an aqueous medium and concentrated by octylphenoxypolyethoxyethanol (Triton X-114) as a surfactant. After the phase separation at 60 degrees C based on the cloud point extraction of the mixture, the surfactant-rich phase was dried and the remaining phase was dissolved using 20 microL of carbon tetrachloride. The obtained solution was introduced into a quartz microcell and the analyte was determined by laser induced-thermal lens spectrometry (LI-TLS). The single-laser TLS was used as a sensitive method for the determination of palladium-PAN complex in 20 microL of the sample. Under optimum conditions, the analytical curve was linear for the concentration range of 0.3-60 ng mL(-1) and the detection limit was 0.04 ng mL(-1). The enhancement factor of 460 was achieved for 10 mL samples containing the analyte and relative standard deviations were lower than 5%. The developed method was successfully applied to the extraction and determination of palladium in water samples.

摘要

浊点萃取(CPE)结合热透镜光谱法(TLS)已被开发用于钯的预浓缩和测定。TLS 和 CPE 方法具有良好的组合条件,因为 TLS 是分析 CPE 后获得的低体积样品的合适方法。钯与 1-(2-吡啶偶氮)-2-萘酚(PAN)在水介质中络合,并通过辛基酚聚氧乙烯醚(Triton X-114)作为表面活性剂浓缩。在基于混合物浊点萃取的 60°C 下进行相分离后,将富含表面活性剂的相干燥,并使用 20 μL 四氯化碳溶解剩余相。所得溶液被引入石英微池,并通过激光诱导热透镜光谱法(LI-TLS)测定分析物。单激光 TLS 被用作测定 20 μL 样品中钯-PAN 络合物的灵敏方法。在最佳条件下,分析曲线在 0.3-60ng mL(-1)浓度范围内呈线性,检测限为 0.04ng mL(-1)。对于含有分析物的 10 mL 样品,实现了 460 的增强因子,相对标准偏差低于 5%。所开发的方法成功地应用于水样中钯的提取和测定。

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