Laboratoire de radioécologie, Département de chimie, Université Laval , 1045 Avenue de la Médecine, Québec, Quebec G1V 0A6, Canada.
Anal Chem. 2013 Nov 5;85(21):10549-55. doi: 10.1021/ac402649v. Epub 2013 Oct 16.
A new cloud point extraction procedure has been developed for the quantification of plutonium(IV) in environmental samples. The separation procedure can be either coupled to inductively coupled plasma mass spectrometry (ICPMS) or α spectrometry for plutonium quantification. The method uses a combination of selective ligand (P,P'-di(2-ethylhexyl) methanediphosphonic acid (H2DEH[MDP])) and micelle shielding by bromine formation to enable quantitative extraction of Pu in highly acidic solutions. Cross-optimization of all parameters (nonionic and ionic surfactant, chelating agent, bromate, bromide, and pH) led to optimal of the extraction conditions. Figures of merit of the method for the detection using α spectrometry and ICPMS are reported (limit of detection, limit of quantification, minimal detectable activity, and recovery). Quantitative extractions (>95%) were obtained for a wide variety of aqueous and digested samples (synthetic urine, wastewater, drinking water, seawater, and soil samples). The method features the first successful coupling between α spectrometry and cloud point extraction and is the first demonstration of CPE suitability with metaborate fusion as a sample preparation approach, techniques used extensively in nuclear industries.
一种新的浊点萃取程序已经被开发出来，用于环境样品中钚（IV）的定量分析。分离程序可以与电感耦合等离子体质谱（ICPMS）或α谱法结合使用，以进行钚的定量分析。该方法使用选择性配体（P，P'-二（2-乙基己基）甲叉二膦酸（H2DEH[MDP]））和溴形成胶束屏蔽的组合，以实现高酸度溶液中钚的定量萃取。对所有参数（非离子和离子表面活性剂、螯合剂、溴酸盐、溴化物和 pH 值）进行交叉优化，以达到最佳萃取条件。报告了使用α谱法和 ICPMS 检测的方法的优点（检测限、定量限、最小可检测活度和回收率）。对各种水相和消解样品（合成尿液、废水、饮用水、海水和土壤样品）进行了定量萃取（>95%）。该方法的特点是首次成功地将α谱法和浊点萃取法结合起来，并且首次证明了浊点萃取法与偏硼酸盐熔融法作为样品制备方法的适用性，后者在核工业中得到了广泛应用。
