Manzoori Jamshid L, Amjadi Mohammad, Abulhassani Jafar
Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.
Anal Chim Acta. 2009 Jun 30;644(1-2):48-52. doi: 10.1016/j.aca.2009.04.029. Epub 2009 May 3.
An improved single drop microextraction procedure was developed for the preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry. Ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6], was used as an alternative to volatile organic solvents for extraction. Lead was complexed with ammonium pyrroldinedithiocarbamate (APDC) and extracted into a 7-microL ionic liquid drop. The extracted complex was directly injected into the graphite furnace. Several variables affecting microextraction efficiency and ETAAS signal, such as pyrolysis and atomization temperature, pH, APDC concentration, extraction time, drop volume and stirring rate were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enhancement factor were 0.015 microg L(-1) and 76, respectively. The relative standard deviation (RSD) for five replicate determinations of 0.2 microg L(-1) Pb was 5.2%. The developed method was validated by the analysis of certified reference materials and applied successfully to the determination of lead in several real samples.
开发了一种改进的单滴微萃取方法,用于在电热原子吸收光谱法测定铅之前对其进行预富集。离子液体1-丁基-3-甲基咪唑六氟磷酸盐[C4MIM][PF6]被用作挥发性有机溶剂的替代品进行萃取。铅与吡咯烷二硫代氨基甲酸铵(APDC)络合,并被萃取到7微升的离子液体滴中。萃取的络合物直接注入石墨炉。研究并优化了影响微萃取效率和电热原子吸收光谱信号的几个变量,如热解温度、原子化温度、pH值、APDC浓度、萃取时间、液滴体积和搅拌速率。在最佳实验条件下,检测限(3s)和富集因子分别为0.015微克/升和76。对0.2微克/升铅进行五次重复测定的相对标准偏差(RSD)为5.2%。通过对有证标准物质的分析验证了所开发的方法,并成功应用于多个实际样品中铅的测定。