Qiao Jixin, Hou Xiaolin, Roos Per, Miró Manuel
Radiation Research Division, Risø National Laboratory for Sustainable Energy, NUK-202, Technical University of Denmark, DK-4000 Roskilde, Denmark.
Anal Chem. 2009 Oct 1;81(19):8185-92. doi: 10.1021/ac901395e.
This article presents an automated method for the rapid determination of 239Pu and 240Pu in various environmental samples. The analytical method involves the in-line separation of Pu isotopes using extraction chromatography (TEVA) implemented in a sequential injection (SI) network followed by detection of isolated analytes with inductively coupled plasma mass spectrometry (ICP-MS). The method has been devised for the determination of Pu isotopes at environmentally relevant concentrations, whereby it has been successfully applied to the analyses of large volumes/amounts of samples, for example, 100-200 g of soil and sediment, 20 g of seaweed, and 200 L of seawater following analyte preconcentration. The investigation of the separation capability of the assembled SI system revealed that up to 200 g of soil or sediment can be treated using a column containing about 0.70 g of TEVA resin. The analytical results of Pu isotopes in the reference materials showed good agreement with the certified or reference values at the 0.05 significance level. Chemical yields of Pu ranged from 80 to 105%, and the decontamination factors for uranium, thorium, mercury and lead were all above 10(4). The duration of the in-line extraction chromatographic run was <1.5 h, and the proposed setup was able to handle up to 20 samples (14 mL each) in a fully automated mode using a single chromatographic column. The SI manifold is thus suitable for rapid and automated determination of Pu isotopes in environmental risk assessment and emergency preparedness scenarios.
本文介绍了一种用于快速测定各种环境样品中239Pu和240Pu的自动化方法。该分析方法包括使用在顺序注射(SI)网络中实施的萃取色谱法(TEVA)在线分离Pu同位素,然后用电感耦合等离子体质谱法(ICP-MS)检测分离出的分析物。该方法旨在测定环境相关浓度下的Pu同位素,已成功应用于大量样品的分析,例如,在分析物预浓缩后,可对100 - 200克土壤和沉积物、20克海藻以及200升海水进行分析。对组装的SI系统分离能力的研究表明,使用含有约0.70克TEVA树脂的柱子可处理多达200克土壤或沉积物。参考物质中Pu同位素的分析结果在0.05显著水平下与认证值或参考值显示出良好的一致性。Pu的化学产率在80%至105%之间,铀、钍、汞和铅的去污因子均高于10⁴。在线萃取色谱运行时间<1.5小时,所提出的装置能够使用单个色谱柱以全自动模式处理多达20个样品(每个14毫升)。因此,SI流路适用于环境风险评估和应急准备场景中Pu同位素的快速自动化测定。