Simultaneous analysis of 237Np and Pu isotopes in environmental samples by ICP-SF-MS coupled with automated sequential injection system

Simultaneous analysis of 237Np and Pu isotopes in environmental samples by ICP-SF-MS coupled with automated sequential injection system
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DOI:
10.1039/b400034j
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发表时间:
2004-01-01
影响因子:
3.4
通讯作者:
Lee, KJ
Lee, KJ
中科院分区:
化学2区
文献类型:
--
作者:
Kim, CS;Kim, CK;Lee, KJ

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采用扇形场电感耦合等离子体质谱(ICP-SF-MS)检测器和自动顺序注射(SI)分离系统,建立了Np-237、Pu-239和Pu-240的同时分析方法。这些锕系元素的化学纯化进行了一个锕系元素特异性的萃取色谱树脂,TEVA-Spec,在自动SI系统。Np和Pu在TEVA-Spec上的类似化学行为通过在5 M HNO 3中用抗坏血酸处理后的回收试验来证实。TEVA-Spec保持其可重复使用性,提供高且一致的化学回收率,并在连续分析9个重复样品期间显示出对Np和Pu的良好选择性和低记忆效应。用标准参考物质验证了SI系统提纯Np-237和Pu同位素的化学回收率高(>90%),准确度和重复性可靠。Np-237、Pu-239和Pu-240的检出限分别为2.5、2.1和0.42 fg ml(-1),这使得分析土壤和沉积物样品中低至1 g的这些核素成为可能。除上样前需要的制备过程外,所有化学净化均由程控SI系统自动进行,并在1小时内完成,其中包括ICP-SF-MS测量。该方法已成功应用于土壤、沉积物和生物样品中Np-237和Pu的环境水平分析。
A simultaneous analytical method for Np-237, Pu-239 and Pu-240 has been developed using sector field inductively coupled plasma mass spectrometry (ICP-SF-MS) detection combined with an automated sequential injection ( SI) separation system. The chemical purification of these actinides was carried out on an actinide-specific extraction chromatographic resin, TEVA-Spec, in an automated SI system. The similar chemical behaviors of Np and Pu on TEVA-Spec was confirmed by recovery test after treating with ascorbic acid in 5 M HNO3. TEVA-Spec maintained its re-usability, giving high and consistent chemical recovery, and showed good selectivity for Np and Pu and a low memory effect during the consecutive analysis of nine replicate samples. The high chemical recovery (>90%), reliable accuracy and repeatability of Np-237 and Pu isotope purification using the SI system were proved using standard reference materials. Low detection limits of 2.5, 2.1 and 0.42 fg ml(-1) were obtained for Np-237, Pu-239 and Pu-240, respectively, which make it possible to analyze these nuclides in samples of soil and sediment as low as 1 g. With the exception of the preparation process required prior to loading a sample, all chemical purifications were carried out automatically by the programmed SI system, and were completed within 1 hour, which included measurement by ICP-SF-MS. This method was successfully applied to the analysis of the environmental levels of Np-237 and Pu in soil, sediment and in biological samples.