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A sem-icp-ms method for measuring single particle uranium isotope ratio

A technology of SEM-ICP-MS and isotope ratio, which is applied in the field of nuclear safeguards, can solve the problems of affecting the precision of the measurement results, the stability of the instrument is greatly affected, and the amount of sample processing is not large. Effects with fast processing speed

Inactive Publication Date: 2011-12-21
CHINA INSTITUTE OF ATOMIC ENERGY
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Problems solved by technology

Compared with the analysis of the suspension of uranium particles, the signal obtained after the particle is dissolved and then measured remains stable, but this method takes a long time to dissolve the particle, and the sample processing capacity is not large. ICP-MS uses a single receiver peak jump to measure uranium isotopes The amount of sample required for the ratio is large and the time is long, the stability of the instrument has a great influence on the result, and ultimately affects the precision of the measurement result

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  • A sem-icp-ms method for measuring single particle uranium isotope ratio
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  • A sem-icp-ms method for measuring single particle uranium isotope ratio

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Embodiment Construction

[0015] Below in conjunction with accompanying drawing and specific embodiment the present invention is described in further detail:

[0016] Experimental instrument, utensil and reagent used in the present invention are as follows:

[0017] JSM-6360LV scanning electron microscope (SEM), Japanese JEOL company; Genesis2000XMS energy spectrometer (EDX), American EDAX company; MM3A-EM micromanipulator, German Kleindiek Nanotechnik company; Isoprobe TM Multi-receiver inductively coupled plasma mass spectrometer (MC-ICP-MS), GV Company, UK; ultrapure water device (18.2MΩ·cm), Millipore Company, USA.

[0018] PFA reagent bottle, Zhenghong Plastic Factory, Binhai County, Jiangsu Province; high-purity carbon sheet (diameter 2.4cm, thickness 3mm), American Ernest F.Fullam Company; silicon wafer (5×5mm), Beijing Zhongjing Technology Company; cotton quality wipes (TexWipe TX304, 10cm x 10cm).

[0019] Uranium isotope reference material (U 3 o 8 powder), NBL; HNO 3 (BV-Ⅲ level), Beiji...

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Abstract

The invention discloses a method for measuring the uranium isotope ratio of a single particle by SEM-ICP-MS. The method comprises the following steps: (1) preparation of a uranium particle sample; (2) search, identification and transfer of the uranium particle; (3) Dissolution of uranium particles; (4) determination of uranium isotope ratio, described step (3) is to put the silicon chip with uranium particles into the reagent bottle, add HNO3, heat on the electric heating plate to dissolve the particles, and then add Deionized water is used to adjust the acidity; in the step (4), a multi-receiver inductively coupled plasma mass spectrometer (MC-ICP-MS) is used to simultaneously receive 235U and 238U signals for sample measurement. The invention provides a SEM-ICP-MS method for determining the uranium isotope ratio of a single particle with fast particle dissolution rate, large sample processing capacity, small amount of sample required for measurement, relatively high measurement precision and short measurement time.

Description

technical field [0001] The invention relates to the technical field of nuclear safeguards, in particular to a method for measuring single-particle uranium isotope ratios by SEM-ICP-MS. Background technique [0002] The isotope ratio analysis of single uranium particles is an important technical means for revealing undeclared nuclear activities in the field of nuclear safeguards. FT-TIMS and SIMS are reliable methods for the analysis of single particle isotopes. The FT-TIMS method can easily identify uranium-containing particles and precisely measure the isotope ratio. The disadvantage is that this method needs to irradiate the sample with reactor thermal neutrons, and the overall process is complicated and time-consuming. The SIMS method is suitable for samples with a large number of uranium-containing particles and a sufficiently large particle size. However, in actual samples, there are few uranium-containing particles, and it is time-consuming to find particles, and the ...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/28G01N27/626
Inventor 王晓明李力力张燕朱留超赵永刚
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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