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引用本文:   汪伟, 李志明, 徐江, 周国庆, 粟永阳, 吴艳敏, 韦冠一, 方随, 王文亮. 激光剥蚀-多接收电感耦合等离子体质谱法测定含钚颗粒物中240Pu/239Pu比值. 分析化学, 2017, 45(11): 1719-1726. doi:  10.11895/j.issn.0253-3820.171028 [复制]

Citation:   WANG Wei, LI Zhi-Ming, XU Jiang, ZHOU Guo-Qing, SU Yong-Yang, WU Yan-Min, WEI Guan-Yi, FANG Sui, WANG Wen-Liang. Determination of 240Pu/239Pu in Plutonium-containing Particle by Laser Ablation Multiple Collector Inductively Coupled Plasma Mass Spectrometry. Chinese Journal of Analytical Chemistry, 2017, 45(11): 1719-1726. doi: 10.11895/j.issn.0253-3820.171028 [复制]

激光剥蚀-多接收电感耦合等离子体质谱法测定含钚颗粒物中240Pu/239Pu比值

通讯作者:  李志明, YQ250003@nint.ac.cn

收稿日期: 2017-06-22

接受日期: 2017-09-10

出版日期: 2017-11-20

基金项目: 本文系科技部重大仪器专项资助项目(No.2012YQ250003)

Determination of 240Pu/239Pu in Plutonium-containing Particle by Laser Ablation Multiple Collector Inductively Coupled Plasma Mass Spectrometry

Corresponding author:  LI Zhi-Ming, YQ250003@nint.ac.cn

Received Date:  2017-06-22

Accepted Date:  2017-09-10

Published Date:  2017-11-20

Fund Project:  This work was supproted by the National key Foundation for Exploring Scientific Instrumet of China (No. 2012YQ250003)

为高精度、准确地获取含钚颗粒物中具有核保障监督意义和核取证价值的钚同位素比值,建立了激光剥蚀-多接收电感耦合等离子体质谱(LA-MC-ICP-MS)测定含钚颗粒物中240Pu/239Pu的分析方法。采用检漏、安装排风罩和擦拭剥蚀池内壁等方式有效降低激光剥蚀产物沾污实验室和危及人身安全的潜在风险。联用扫描电迁移率粒径谱仪(SMPS)与激光剥蚀-多接收器等离子体质谱(LA-MC-ICP-MS)研究了激光剥蚀玻璃基体标样产生气溶胶的分布特性,结果表明,剥蚀产物的主要粒径是40~500 nm,应尽量采用水平管道连接激光剥蚀进样系统与MC-ICP-MS,含钚颗粒物分析后剥蚀池持续吹扫时间应大于15 min。采用外标归一化法离线校正质量分馏效应和离子计数器检测效率,建立了含钚颗粒物中240Pu/239Pu的LA-MC-ICP-MS分析方法,固定束斑直径30μm、脉冲重复率5 Hz、剥蚀时间5 s,调节能量密度使含钚颗粒物模拟样品中239Pu的信号强度分别达2×104cps和2×105 cps,本方法对240Pu/239Pu测量的相对实验标准不确定度小于1.4%(n=6),测量结果与参考值的相对偏差小于4.7%,仪器调试时间和单个样品测量时间分别为9.0和0.5 h。含钚颗粒物模拟样品分析结果表明,本方法精度高、结果准确、分析速度快,可满足核保障监督、禁产核查和核取证中含钚颗粒物直接分析的需求。

关键词:   钚颗粒物, 240Pu/239Pu比值, 激光剥蚀-多接收电感耦合等离子体质谱
Key words:   Plutonium particles, 240Pu/239Pu ratio, Laser ablation multiple collector inductively coupled plasma mass spectrometry
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激光剥蚀-多接收电感耦合等离子体质谱法测定含钚颗粒物中240Pu/239Pu比值

汪伟, 李志明, 徐江, 周国庆, 粟永阳, 吴艳敏, 韦冠一, 方随, 王文亮

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