土壤和沉积物中痕量Pu的ICP-MS测量方法研究

辐射防护 ›› 2016, Vol. 36 ›› Issue (5): 265-271.

土壤和沉积物中痕量Pu的ICP-MS测量方法研究

倪有意¹, 卜文庭¹, 胡丹², 许宏², 吴昱城², 郭秋菊¹

1.北京大学物理学院核物理与核技术国家重点实验室,北京 100871;
2.浙江省辐射环境监测站,杭州 310012

收稿日期:2015-02-11 出版日期:2016-09-20 发布日期:2021-11-15
通讯作者: 郭秋菊。E-mail: qjguo@pku.edu.cn
作者简介:倪有意(1992—),男,2014年毕业于北京大学物理学院,现为北京大学物理学院辐射防护与环境保护专业在读博士研究生。E-mail: niyouyi@pku.edu.cn

A method of measurement of ultra-trace level Pu isotopes in soil and sediment samples by ICP-MS

Ni Youyi¹, Bu Wenting¹, Hu Dan², Xu Hong², Wu Yucheng², Guo Qiuju¹

1. State Key Laboratory of Nuclear Physics and Technology, School of Physics, Peking University, Beijing 100871;
2. Radiation Monitoring Technical Center, Zhejiang Province, Hangzhou 310012

Received:2015-02-11 Online:2016-09-20 Published:2021-11-15

摘要/Abstract

摘要： 介绍了一种针对土壤和沉积物样品中Pu核素的ICP-MS测量方法。该方法利用硝酸浸取和两步阴离子交换层析对样品中的Pu进行提纯和除杂,此方法对U的去污因子为1.5×10⁵。在加入了APEX-IR雾化装置和Spiro膜去溶装置后, ICP-MS测量中影响²³⁹Pu和²⁴⁰Pu计数率的²³⁸U多原子离子²³⁸U¹H⁺/²³⁸U和²³⁸U¹H⁺₂/²³⁸U产率分别为3.4×10^-5和7.6×10^-6。将该方法运用在我国环境土壤和沉积物的ICP-MS测量中,可使样品中Pu测量结果的相对误差降低到约千分之一。该方法对²³⁹Pu和²⁴⁰Pu的检测限分别为3.6 fg/mL和 7.3 fg/mL。利用该方法对IAEA-soil-6和NIST-4357两种参考物质进行前处理和ICP-MS测量,结果表明样品中^239+240Pu活度浓度和²⁴⁰Pu/²³⁹Pu同位素原子比与参考值符合,验证了该方法的有效性和准确性。

关键词: 痕量Pu, ICP-MS测量, 阴离子交换层析, 去污因子

Abstract: As a widely accepted method of measuring ultra-trace level Plutonium isotopes in environment samples, the most difficulty and inaccuracy of ICP-MS measurement is from the interference of matrix elements, mainly uranium. In this research, we employed acid digestion and a two-stage anion chromatography for extraction and purification of Pu from soil and sediment samples, which can achieve high decontamination factor of uranium up to 1.5×10⁵. By introducing a APEX-IR sampling system combined with a Spiro membrane desolvation unit, the yields of polyatomic interferences ²³⁸U¹H⁺and ²³⁸U¹H⁺₂, which are the main interferences of ²³⁹Pu and ²⁴⁰Pu, are as low as 3.4×10^-5and 7.6×10^-6, respectively. In case of using this method to analyze the Pu level of Chinese soils and sediments, the relative tolerances of measured results are supposed to be less than millesimal. The detection limit of this method for ²³⁹Pu and ²⁴⁰Pu are respectively 3.6 fg/mL and 7.3 fg/mL. This method is validated by analyzing soil and sediment reference materials IAEA-soil-6 and NIST-4357, both the ^239+240Pu concentration and ²⁴⁰Pu/²³⁹Pu atom ratio correspond well with the certified values.

Key words: Plutonium, ICP-MS, anion chromatography, decontamination factor

中图分类号:

O615.4+5

倪有意, 卜文庭, 胡丹, 许宏, 吴昱城, 郭秋菊. 土壤和沉积物中痕量Pu的ICP-MS测量方法研究[J]. 辐射防护, 2016, 36(5): 265-271.

Ni Youyi, Bu Wenting, Hu Dan, Xu Hong, Wu Yucheng, Guo Qiuju. A method of measurement of ultra-trace level Pu isotopes in soil and sediment samples by ICP-MS[J]. RADIATION PROTECTION, 2016, 36(5): 265-271.

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