Radiochemistry Division, Bhabha Atomic Research Centre, Mumbai-400 085, India.
Radiochemistry Division, Bhabha Atomic Research Centre, Mumbai-400 085, India.
J Chromatogr A. 2021 Apr 12;1642:462037. doi: 10.1016/j.chroma.2021.462037. Epub 2021 Mar 4.
Two solid phase extraction resins (SPER) were prepared by impregnating solutions of two diglycolamide-functionalized calix[4]arenes in 10% isodecanol in n-dodecane into Chromosorb W, as the stationary phase. While SPER-I contained n-propyl functionalized calix[4]arene, SPER-II contained the calix[4]arene with isopentyl groups at the carboxamide nitrogen atoms. The SPERs were characterized by SEM, TGA, FTIR, etc. and were used for the batch uptake of neptunium(IV) from nitric acid feed solutions. While the uptake of Np(IV) was extremely high with SPER-I (K: 47,544 at 3 M nitric acid, ca. 8% extractant loading), SPER-II displayed a significantly lower extraction efficiency (K: 13,724 under identical conditions) as indicated by the batch uptake studies. Sorption isotherm studies were carried out which indicated good fitting to the Langmuir model suggesting uptake conforming to monolayer sorption. Fitting to the D-R isotherm model conformed to a chemisorption model. Column studies were also carried out and the elution profiles, obtained with solutions of oxalic acid and nitric acid indicated very sharp peaks suggesting that the column can be used for the separation of Np(IV) from acidic radioactive feeds.
两种固相萃取树脂（SPER）是通过将两种二甘醇酰胺功能化杯[4]芳烃在 10%异癸醇中的溶液浸渍到 Chromosorb W 中作为固定相来制备的。SPER-I 中含有正丙基功能化杯[4]芳烃，而 SPER-II 中则含有在羧酰胺氮原子上带有异戊基的杯[4]芳烃。SPER 用 SEM、TGA、FTIR 等进行了表征，并用于从硝酸进料溶液中批量吸附镎（IV）。虽然 SPER-I 对 Np（IV）的吸附非常高（在 3 M 硝酸中，K：47,544，约 8%的萃取剂负载量），但批次吸附研究表明 SPER-II 的萃取效率明显较低（在相同条件下，K：13,724）。进行了吸附等温线研究，表明其很好地符合 Langmuir 模型，表明吸附符合单层吸附。拟合到 D-R 等温线模型符合化学吸附模型。还进行了柱研究，用草酸和硝酸溶液获得的洗脱曲线表明非常尖锐的峰，表明该柱可用于从酸性放射性进料中分离 Np（IV）。
