Method for analyzing trace plutonium content in large amount of uranium in nuclear fuel aftertreatment process

An analysis method and nuclear fuel technology, applied in the field of analytical chemistry, can solve the problems of large sample consumption, complicated separation process, and long operation time, and achieve the effects of improving analysis sensitivity, reducing sample volume, and reducing analysis errors

Inactive Publication Date: 2020-07-31
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Summary
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AI Technical Summary

Problems solved by technology

The pretreatment process of the separation of uranium and plutonium in this method includes adsorption, rinsing, elution and other processes, the process is complicated, and the pretreatment of a single sample takes 2-4 hours; the sample consumption is large, requiring 5-50ml; the sample with low plutonium concentration , in the process of adsorption, leaching and elution of ion exchange, some plutonium will be lost, resulting in low analysis results (see: Li Lili, Li Jinying, Zhao Yonggang, etc. Separation of trace plutonium in uranium matrix[J]. Nuclear Chemistry and Radiation Chemistry, 2007,29(3):135-140.)
[0006] Therefore, the above methods have the disadvantages of large analysis error, large sampling volume, complicated separation process and long operation time when analyzing nuclear fuel reprocessing process samples.

Method used

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Embodiment 1

[0029] (1) Take 5ml simulated sample (the uranium concentration is 50g / L, the plutonium concentration is 5.12×10 -8 g / L), add 1.2ml10mol / L nitric acid to make the solution acidity reach 2mol / L;

[0030] (2) Add 0.05ml 1mol / L sodium nitrite solution, mix well and let stand for 2 minutes to oxidize plutonium to tetravalent;

[0031] (3) Add 0.5mol / LTTA-xylene solution 0.5ml of extractant to extract Pu(IV) for 10min, centrifuge for 2min at 3000 rpm, discard the water phase, and realize the separation of uranium and plutonium;

[0032] (4) Wash the organic phase three times with 1mol / L nitric acid, each washing for 5 minutes, to elute a small amount of uranium entrained in the organic phase;

[0033] (5) Get 0.1ml of the organic phase and dilute it to 2.5ml with isopropanol, analyze the plutonium concentration with ICP-MS equipped with organic sampling system drawn, the organic sampling system was fed with oxygen), and the analyzed plutonium concentration was 5.26×10 -8 g / L, th...

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Abstract

The invention belongs to the technical field of analytical chemistry, and relates to a method for analyzing trace plutonium content in a large amount of uranium in a nuclear fuel aftertreatment process. The analysis method sequentially comprises the following steps: (1) taking a sample with a certain volume, and adding concentrated nitric acid to adjust the concentration of nitric acid to 1-2 mol/L; (2) adding a sodium nitrite solution into the sample, uniformly mixing and standing for a period of time; (3) adding an extraction agent into the sample for extraction, performing centrifugal separation, removing a water phase, and retaining an organic phase; (4) washing the organic phase with a washing solution for 2-5 times, removing the water phase after each washing, and retaining the organic phase; and (5) diluting the organic phase with isopropanol, and analyzing the diluted organic phase with ICP-MS provided with an organic sample injection system. By utilizing the method for analyzing the trace plutonium content in the large amount of uranium in the nuclear fuel post-treatment process, the trace plutonium content in the large amount of uranium in the nuclear fuel post-treatmentprocess can be simply, conveniently, quickly and accurately analyzed with less required sample amount and little interference.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry and relates to a method for analyzing trace plutonium content in a large amount of uranium in a nuclear fuel reprocessing process. Background technique [0002] Nuclear fuel reprocessing has very strict requirements on the control of plutonium in uranium products. In the uranium product of the reprocessing process, the concentration of uranium is tens of grams per liter, and the ratio of uranium to plutonium exceeds 1×10 9 , a large amount of uranium to a trace amount 239 Pu analysis is very disturbing. To accurately measure the concentration of plutonium in the sample solution, it is necessary to undergo a strict pretreatment process for the separation of uranium and plutonium, so that uranium and plutonium can be separated. Therefore, a good pretreatment process for the separation of uranium and plutonium is the key to the accuracy of the analytical data. However, there are many ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N1/28G01N1/38G01N1/34G01N27/626
CPCG01N27/626G01N1/28G01N1/38G01N1/34
Inventor 丛海峰苏哲肖松涛
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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