Department of Chemistry, University of Missouri, Columbia, MO, 65211, United States.
Department of Chemistry, University of Missouri, Columbia, MO, 65211, United States; Research Reactor, University of Missouri, Columbia, MO, 65211, United States.
Talanta. 2021 Jan 1;221:121622. doi: 10.1016/j.talanta.2020.121622. Epub 2020 Sep 6.
High-temperature ammonium bifluoride (ABF) fusions were evaluated for potential use in rapid dissolution of post-detonation nuclear debris. The ABF fusion was carried out in a Pt crucible which allowed evaluation of higher fusion and evaporation temperatures. The high-temperature ABF fusion dissolution method was evaluated using geological reference materials: USGS QLO-1a Quartz Latite, USGS SDC-1 Mica Schist, and NIST 278 Obsidian Rock. The optimized dissolution method involved a 10 min fusion at 540 °C, a 5 min reflux in 8 M HNO an evaporation at 300 °C and final dilution into 45 mL of 2% (v/v) HNO. The final solution was filtered after heating at 105 °C using a hotblock. This dissolution method was simple, requiring only a hotplate or hotblock, filtered samples were available for ICP-MS analysis or radiochemical separation within 150 min, and was found to have high (>90%) recovery for many isotopes of interest in nuclear forensics applications. U and Pu in the dissolved material was separated using TEVA and UTEVA extraction chromatography columns, a process which resulted in >90% recovery. An irradiated U tracer was spiked into the material prior to dissolution and analyzed for recovery of major fission products and Np. The monitored radionuclides had recoveries of greater than 90%, except for the volatile radioiodine isotopes.
高温氟化铵(ABF)熔融物被评估为用于快速溶解核爆炸后残骸的潜在方法。在 Pt 坩埚中进行 ABF 熔融实验,这使得可以评估更高的熔融和蒸发温度。使用地质参考试样:USGS QLO-1a Quartz Latite、USGS SDC-1 Mica Schist 和 NIST 278 Obsidian Rock 评估了高温 ABF 熔融溶解方法。优化的溶解方法包括在 540°C 下进行 10 分钟熔融、在 8M HNO 中进行 5 分钟回流、在 300°C 下蒸发以及最终稀释至 45mL 2%(v/v)HNO。在 105°C 下加热后,使用热块过滤最终溶液。这种溶解方法简单,只需要热板或热块,过滤后的样品可在 150 分钟内进行 ICP-MS 分析或放射化学分离,并且发现对于核取证应用中许多感兴趣的同位素具有高(>90%)回收率。溶解材料中的 U 和 Pu 使用 TEVA 和 UTEVA 萃取色谱柱进行分离,这一过程导致>90%的回收率。在溶解之前,将辐照的 U 示踪剂掺入材料中,并分析主要裂变产物和 Np 的回收率。监测的放射性核素的回收率均大于 90%,除了挥发性放射性碘同位素。