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~（240）Pu/~（239）Pu比值

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 mi...

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Published in分析化学 Vol. 45; no. 11; pp. 1719 - 1726
Main Author 汪伟 李志明 徐江 周国庆 粟永阳 吴艳敏 韦冠一 方随 王文亮
Format Journal Article
LanguageChinese
Published 西北核技术研究所,西安,710024 2017
Subjects
240Pu/239Pu比值
激光剥蚀-多接收电感耦合等离子体质谱
钚颗粒物
激光剥蚀-多接收电感耦合等离子体质谱
Laser ablation multiple collector inductively coupled plasma mass spectrometry
240Pu/239Pu比值
钚颗粒物
Plutonium particles
240 Pu / 239 Pu ratio
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ISSN0253-3820
DOI10.11895/j.issn.0253-3820.171028

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Summary: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2×105cps,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。
Bibliography:Plutonium particles;240Pu /239Pu ratio; Laser ablation multiple collector inductively coupledplasma mass spectrometry
WANG Wei, LI Zhi-Ming, XU Jiang, ZHOU Guo-Qing, SU Yong-Yang,WU Yan-Min, WEI Guan-Yi, FANG Sui, WANG Wen-Liang（Northwest Institute of Nuclear Technology, Xi忆an 710024, China）
22-1125/O6
The isotopic fingerprints of plutonium are extremely important for nuclear safeguards and nuclear forensics. An analytical method was developed for direct determination of240Pu/239Pu ratio in plutoniumcontaining particles by laser ablation multiple collector inductively coupled plasma mass spectrometry（ LAMC-ICP-MS）. The risk of ablated particles leakage was reduced by leak detection,exhaust hood,and swiping the laser cell. Scanning mobility particle sizer（ SMPS） was used to measure the effect of ablation parameters on the size distribution of ablated particles. The results showed that the majority of ablation material presented as particles from 40-500 nm and the sweep time after laser ablation should be longer t
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.171028