Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, Iran.
Talanta. 2010 Apr 15;81(1-2):309-13. doi: 10.1016/j.talanta.2009.12.004. Epub 2009 Dec 16.
A new method of solidified floating organic drop microextraction, based on ultrasound-dispersion prior to flame atomic absorption spectrometry was successfully used for separation and enrichment of trace amounts of palladium in aqueous samples. In this method, palladium (II) was extracted into the fine droplets of 1-undecanol after chelate formation with the water soluble ligand, ammonium pyrrolidinedithiocarbamate. The fine droplets of 1-undecanol were made and dispersed as a cloud in the aqueous sample with the help of ultrasonic waves. Several variable factors that influence the extraction and complex formation, such as pH, concentration of ammonium pyrrolidinedithiocarbamate, sonication time, centrifuging time, type and volume of the extracting solvent were optimized. Under the optimized conditions, a detection limit of 0.60 ng mL(-1) and a good relative standard deviation of +/-2% at 10 ng mL(-1) were obtained (n=7). The proposed method was applied to well water, tap water, wastewater and synthetic samples and spiked recoveries were in the range of 97-105%. The results showed that solidified floating organic drop microextraction based on ultrasound-dispersion combined with flame atomic absorption spectrometry was a rapid, simple, sensitive, low cost, minimum organic solvent consumption and efficient analytical method for the separation and determination of trace amounts of palladium ion.
一种新的固态浮动有机液滴微萃取方法，基于超声分散前火焰原子吸收光谱法，成功地用于分离和富集水样中的痕量钯。在该方法中，钯（II）与水溶性配体吡咯烷二硫代氨基甲酸盐形成螯合物后被萃取到 1-十一醇的细小液滴中。在超声波的帮助下，1-十一醇的细小液滴被制成并分散在水样中形成云状。优化了影响萃取和络合形成的几个变量因素，如 pH 值、吡咯烷二硫代氨基甲酸盐的浓度、超声时间、离心时间、萃取溶剂的类型和体积。在优化条件下，可得到 0.60ng/mL 的检测限和 10ng/mL 时 2%的良好相对标准偏差（n=7）。该方法应用于井水、自来水、废水和合成样品，加标回收率在 97-105%范围内。结果表明，基于超声分散的固态浮动有机液滴微萃取结合火焰原子吸收光谱法是一种快速、简单、灵敏、低成本、有机溶剂消耗最少且高效的分析方法，用于分离和测定痕量钯离子。
