Laboratoire de radioécologie, Département de chimie, Université Laval, 1045 Avenue de la Médecine, Québec, QC, G1V 0A6, Canada.
Laboratoire de radioécologie, Département de chimie, Université Laval, 1045 Avenue de la Médecine, Québec, QC, G1V 0A6, Canada.
Appl Radiat Isot. 2021 Feb;168:109549. doi: 10.1016/j.apradiso.2020.109549. Epub 2020 Dec 4.
This study presents a novel cloud point extraction (CPE) methodology for the separation and enrichment of polonium-210 prior to alpha-spectrometric quantification in water, urine and digested samples. The extractive behaviour of diglycolamide-based ligands towards Po by CPE was determined and optimised in various acidic conditions. The extraction efficiency and selectivity of the CPE systems depend greatly on the choice of the extracting agent and acidic conditions. The thorough optimisation of those specific parameters has led to the development of a suitable cloud point extraction system for the determination of polonium-210 at ultra-trace levels compatible with alpha-spectrometry. To facilitate this coupling, a back-extraction procedure was optimised and performed on the surfactant-rich phase to enable the spontaneous deposition of polonium-210 onto a silver disk; this also avoids making the matrix transfer step mandatory due to the presence of a nitric medium. Method detection and quantification limits of 3.5 and 12 mBq L, respectively, were determined by alpha spectrometry. The robustness of the proposed methodology was demonstrated by the determination of polonium ions concentration in various environmental and biological samples and solid certified reference materials.
本研究提出了一种新的浊点萃取（CPE）方法，用于在水、尿液和消化样品中进行α-光谱定量之前分离和富集钋-210。在各种酸性条件下，确定了基于二甘醇酰胺的配体对 Po 的萃取行为，并对其进行了优化。CPE 体系的萃取效率和选择性在很大程度上取决于萃取剂和酸性条件的选择。对这些特定参数的彻底优化导致开发了一种适用于超痕量水平的钋-210 测定的浊点萃取系统，该系统与α-光谱法兼容。为了便于这种耦合，优化并执行了富表面活性剂相的反萃取程序，以促使钋-210 自发沉积到银盘上；这也避免了由于存在硝酸介质而必须进行基质转移步骤。通过α 光谱法确定了方法的检测限和定量限分别为 3.5 和 12 mBq·L。通过测定各种环境和生物样品及固体认证参考物质中的钋离子浓度，证明了所提出方法的稳健性。
