Radiation Research Division, Risø National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde, Denmark.
Anal Chim Acta. 2011 Jan 31;685(2):111-9. doi: 10.1016/j.aca.2010.10.029. Epub 2010 Oct 30.
This paper reports an automated analytical method for rapid determination of plutonium isotopes ((239)Pu and (240)Pu) in environmental solid extracts. Anion exchange chromatographic columns were incorporated in a sequential injection (SI) system to undertake the automated separation of plutonium from matrix and interfering elements. The analytical results most distinctly demonstrated that the crosslinkage of the anion exchanger is a key parameter controlling the separation efficiency. AG 1-×4 type resin was selected as the most suitable sorbent material for analyte separation. Investigation of column size effect upon the separation efficiency revealed that small-sized (2 mL) columns sufficed to handle up to 50 g of environmental soil samples. Under the optimum conditions, chemical yields of plutonium exceeded 90% and the decontamination factors for uranium, thorium and lead ranged from 10(3) to 10(4). The determination of plutonium isotopes in three standard/certified reference materials (IAEA-375 soil, IAEA-135 sediment and NIST-4359 seaweed) and two reference samples (Irish Sea sediment and Danish soil) revealed a good agreement with reference/certified values. The SI column-separation method is straightforward and less labor intensive as compared with batch-wise anion exchange chromatographic procedures. Besides, the automated method features low consumption of ion-exchanger and reagents for column washing and elution, with the consequent decrease in the generation of acidic waste, thus bearing green chemical credentials.
本文报道了一种自动化分析方法,用于快速测定环境固体提取物中的钚同位素((239)Pu 和 (240)Pu)。阴离子交换色谱柱被整合到顺序注射 (SI) 系统中,以实现钚与基质和干扰元素的自动分离。分析结果最明显地表明,阴离子交换剂的交联是控制分离效率的关键参数。AG 1-×4 型树脂被选为最适合分析物分离的吸附材料。考察了柱尺寸对分离效率的影响,结果表明,小尺寸(2 mL)的柱子足以处理多达 50 g 的环境土壤样品。在最佳条件下,钚的化学收率超过 90%,铀、钍和铅的净化因子范围为 10(3)至 10(4)。对三种标准/认证参考物质(IAEA-375 土壤、IAEA-135 沉积物和 NIST-4359 海藻)和两种参考样品(爱尔兰海沉积物和丹麦土壤)中的钚同位素进行测定,结果与参考/认证值吻合良好。与批处理阴离子交换色谱程序相比,SI 柱分离方法简单直接,劳动强度低。此外,自动化方法的特点是离子交换剂和用于柱洗涤和洗脱的试剂消耗低,从而减少了酸性废物的产生,因此具有绿色化学的特点。