Faculty of Science, Department of Chemistry, Trakya University, 22030 Edirne, Turkey.
Environ Sci Pollut Res Int. 2012 Jul;19(6):2428-37. doi: 10.1007/s11356-012-0755-x. Epub 2012 Jan 25.
An online cloud-point extraction (CPE) coupled with flow injection method is developed for the separation and preconcentration of palladium and lead from various matrices using flame atomic absorption spectrometry (FAAS).
The method employs the formation of complexes of the metallic species with dimethylglyoxime, which are subsequently entrapped in the micelles of the surfactant Triton X-114, upon increase of the solution temperature to 60°C and loaded into the flow injection system at a flow rate of 4.6 mL min(-1). The surfactant rich-phase was retained in a minicolumn packed with animal wool at pH 6 and eluted with 1.0 mol L(-1) nitric acid in methanol at a flow rate of 1.1 mL min(-1) directly into the nebulizer of the FAAS. The CPE variables and flow injection conditions affecting the analytical performance of the combined methodology was studied and optimized.
Under the optimized conditions for 25 mL of preconcentrated solution, the enrichment factors were 51 and 44, and the limit of detections were 1.0 and 1.4 ng mL(-1) for palladium and lead, respectively. Finally, the developed method was applied for the determination of palladium and lead in street dust, soil, radiology waste, catalytic converter, and urban aerosol samples.
Cloud-point extraction coupled with flow injection-FAAS was proposed as an effective preconcentration and separation method for Pd and Pb determination in radiology waste, road dust, soil, and urban aerosol samples. The most favorable feature of this method is its much higher selectivity, sensitivity, rapidity, good extraction efficiency, and employs the green chemistry concept, as it does not require the addition of toxic chemicals. In addition, this proposed method gives very low detection limits and good relative standard.
本研究开发了一种在线浊点萃取（CPE）结合流动注射法，用于火焰原子吸收光谱法（FAAS）分离和预浓缩各种基质中的钯和铅。
该方法采用金属物种与二甲基乙二醛形成配合物，然后在溶液温度升高至 60°C 时将其包裹在表面活性剂 Triton X-114 的胶束中，并以 4.6 mL min(-1)的流速载入流动注射系统。在 pH 6 下，富表面活性剂相被保留在填充有动物羊毛的微型柱中，并以 1.1 mL min(-1)的流速用 1.0 mol L(-1)硝酸甲醇洗脱，直接进入 FAAS 的雾化器。研究并优化了影响组合方法分析性能的 CPE 变量和流动注射条件。
在 25 mL 浓缩溶液的最佳条件下，钯和铅的富集因子分别为 51 和 44，检测限分别为 1.0 和 1.4 ng mL(-1)。最后，该方法应用于测定街道灰尘、土壤、放射性废物、催化转化器和城市气溶胶样品中的钯和铅。
提出了浊点萃取结合流动注射-FAAS 作为一种有效的预浓缩和分离方法，用于测定放射性废物、道路灰尘、土壤和城市气溶胶样品中的 Pd 和 Pb。该方法最有利的特点是其更高的选择性、灵敏度、快速性、良好的萃取效率，并采用了绿色化学概念，因为它不需要添加有毒化学品。此外，该方法的检测限非常低，相对标准良好。
