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Analytical method for trace silver in plutonium

An analysis method and trace technology, applied in the direction of material electrochemical variables, can solve the problems of undisclosed operation process and parameter conditions, complex impurity elements, easy hydrolysis of plutonium ions, etc., to reduce the difficulty of radiation protection, simplify operation steps, The effect of high sensitivity

Active Publication Date: 2015-02-11
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the determination of trace silver content in plutonium products has the following characteristics: the impurity elements in plutonium are very complex and there are many interfering elements, and a sharp silver dissolution peak must be formed; plutonium ions are easy to hydrolyze, and the acidity of operation needs to be strictly controlled; It needs to be operated in a glove box, and the protection is difficult. Therefore, the determination of silver in plutonium is very different from other media. The operating process and parameter conditions of applying this method to the determination of trace silver in plutonium are not disclosed in the open literature.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Utilize the method provided by the invention to analyze the silver content in the plutonium, the specific operation steps are as follows:

[0027] (1) After pretreatment of the glassy carbon electrode, in 1×10 -3 mol / L K 3 Fe(CN) 6 -0.2mol / L KNO 3 Test in the solution system to make it satisfy |oxidation potential-reduction potential|≤80mV;

[0028] (2) The glassy carbon electrode is modified with a modifier, the modified glassy carbon electrode is used as the working electrode, the saturated calomel electrode is used as the reference electrode, and the platinum electrode is used as the counter electrode.

[0029] (3) At a temperature of 35°C, add 0.15 mL of plutonium sample solution with a concentration of 10 g / L and 0.3 μg of silver standard solution with 0.05 mol / L HNO 3 -0.05mol / L KNO 3 Dilute to 15mL, apply voltage and record the stripping voltammetry curve, measure the silver content in the sample.

[0030] The mensuration of silver content in the embodiment...

Embodiment 2

[0033] Utilize the method provided by the invention to analyze the silver content in the plutonium, the specific operation steps are as follows:

[0034] (1) The glassy carbon electrode is made of Al 2 o 3 Pretreatment of the suspension, sequentially use Al with a particle size of 0.3 μm and 0.05 μm 2 o 3 The suspension gently polishes the surface of the glassy carbon electrode into a mirror surface according to the direction of "8" at a certain speed, strength, and angle, washes it several times with secondary deionized water, and dries it under infrared light or naturally at room temperature. Dry. After preprocessing, use 1×10 -3 mol / L K 3 Fe(CN) 6 -0.2mol / L KNO 3 The pretreatment effect of the solution is tested, and it is sufficient to satisfy |oxidation potential-reduction potential|≤80mV.

[0035] (2) Use Nafion solution with a mass fraction of 0.06% (ethanol: water = 1:1) to modify the glassy carbon electrode by dipping, that is, insert the electrode vertically ...

Embodiment 3

[0040]The method used in Example 2, the same steps, except that the mass percentage of Nafion solution is 0.09%, and the measurement results are as follows:

[0041] The mensuration of silver content in the embodiment 3 of table 3,

[0042] True value of silver content / μg·L -1

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Abstract

The invention belongs to the technical field of nuclear fuel cycle and discloses an analysis method for trace silver in plutonium. The method comprises the following steps: (1) inspecting the glassy carbon electrode after pretreatment; (2) modifying the glassy carbon electrode with a modifier and using it as a working electrode; An method measures silver content. The method has the characteristics of high sensitivity, strong anti-interference ability, simple instrument structure, and can be directly connected with the glove box.

Description

technical field [0001] The invention belongs to the technical field of nuclear fuel cycle, and in particular relates to an analysis method for trace silver in plutonium. Background technique [0002] In the plutonium purification process, plutonium dioxide needs to be dissolved first. Since plutonium dioxide, especially the plutonium dioxide prepared at high temperature, is an extremely insoluble plutonium compound, conventional dissolution methods such as inorganic acid method and melting method have the characteristics of being difficult to completely dissolve, time-consuming, and labor-intensive. The electrochemical dissolution method is relatively simple, fast and efficient, but a large amount of silver must be added as a catalyst. In order to ensure the quality of plutonium products, the analysis of silver content in purified plutonium dioxide is an important parameter to evaluate the purification efficiency of the process. [0003] At present, in the field of nuclear...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/48
Inventor 朱海巧罗中艳邵少雄吴继宗刘权卫
Owner CHINA INSTITUTE OF ATOMIC ENERGY