Abstract A simple microanalytical method for trace elemental determinations in plutonium (Pu) solution samples was developed using Energy Dispersive X- Ray Fluorescence (EDXRF) spectrometry. A very small sample volume (200 μL) of Pu solution was taken for analysis and the major matrix Pu was separated using the extractant, Tri n-Butyl Phosphate (TBP), in 4 M HNO3 medium. Aliquot of 5 μL of the aqueous phase containing only the trace elements were deposited on a thin transparent mylar film inside the PVC (Poly Vinyl Chloride) EDXRF sample container and dried in ambient atmosphere inside a radioactive fume hood. After drying, the container was sealed with PVC lids. Two pure Pu solutions spiked with different trace elements having concentration of 6.25 and 23.25 μg/mL, were analyzed with RSD (Relative Standard Deviation) of 6.6 and 4.2% (1 σ, n = 3), and the average deviation from the expected values calculated on the basis of sample preparation were 8.9 and 6.6%, respectively. The developed methodology requires small amount of sample, extractant, and therefore generates less radioanalytical waste. Moreover, due to the requirement of small amount of sample, sealed inside a PVC container, the measurements could be carried out in ambient atmosphere without putting the instrument inside glove box. Further, the simple instrumentation of EDXRF, made this methodology very much ideal for the routine analysis of plutonium based samples.

中文翻译：

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使用能量色散 X 射线荧光测定钚样品中痕量元素的简单微量分析方法

摘要 使用能量色散 X 射线荧光 (EDXRF) 光谱法开发了一种用于测定钚 (Pu) 溶液样品中痕量元素的简单微量分析方法。取少量样品 (200 μL) 的 Pu 溶液进行分析，使用萃取剂磷酸三正丁酯 (TBP) 在 4 M HNO3 介质中分离主要基质 Pu。将仅含有微量元素的 5 μL 水相的等分试样沉积在 PVC（聚氯乙烯）EDXRF 样品容器内的透明聚酯薄膜上，并在放射性通风橱内的环境大气中干燥。干燥后，用PVC盖密封容器。两种添加不同痕量元素且浓度分别为 6.25 和 23.25 μg/mL 的纯 Pu 溶液的 RSD（相对标准偏差）分别为 6.6% 和 4.2% (1 σ, n = 3)，与基于样品制备计算的预期值的平均偏差分别为 8.9% 和 6.6%。开发的方法需要少量的样品、萃取剂，因此产生的放射性分析废物较少。此外，由于样品量少，需要密封在PVC容器内，因此无需将仪器放入手套箱内即可在环境大气中进行测量。此外，EDXRF 的简单仪器使这种方法非常适合对基于钚的样品进行常规分析。由于样品量小，密封在PVC容器内，无需将仪器放入手套箱内，即可在常压环境下进行测量。此外，EDXRF 的简单仪器使这种方法非常适合对基于钚的样品进行常规分析。由于样品量小，密封在PVC容器内，无需将仪器放入手套箱内，即可在常压环境下进行测量。此外，EDXRF 的简单仪器使这种方法非常适合对基于钚的样品进行常规分析。