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Plutonium content analysis method

An analysis method and content technology, applied in the field of radiochemistry, can solve the problems of time-consuming source preparation, unfavorable for timely acquisition of plutonium content data in a post-processing plant, and difficulty in reaching the lower detection limit of an α measuring instrument due to low Pu concentration ratio, and achieves simple operation. , The effect of short measurement time and shortened analysis time

Inactive Publication Date: 2016-01-13
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Commonly used plutonium content analysis methods include TTA (thienoyltrifluoroacetone) extraction-α counting method, TIOA (triisooctylamine) extraction-α counting method and lanthanum fluoride carrier-α counting method, in which lanthanum fluoride The analysis procedure of the carrier tape method is more complicated, including steps such as reduction, precipitation, centrifugal separation, precipitation washing, and source preparation, and then the source is prepared by precipitation; the TIOA extraction method directly uses the organic phase to prepare the source, and a special graphite drying table is required. To prevent the organic phase from overflowing; the TTA extraction method is to take a few microliters of the Pu-containing 8mol / L nitric acid solution obtained by back-extraction and evaporate it to make the source. This method makes the concentration of Pu low and difficult to reach the α measuring instrument. lower detection limit
At the same time, the above three methods are time-consuming to prepare sources, which is not conducive to the timely acquisition of plutonium content data in reprocessing plants.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0041] A method for analyzing plutonium content provided by the application, the method comprises the following steps:

[0042] (1) Sampling and addition of isotope diluent

[0043] Weigh the post-treatment PUREX process 1CU material liquid as the sample solution to be analyzed 0.1mL, add 242 Pu tracer, 242 The amount of Pu tracer in the sample solution 239 The content of Pu is close to that.

[0044] (2) Valence regulation of Pu

[0045] Add the ferrous sulfamate solution of 7mol / L nitric acid solution and 0.5mol / L in above-mentioned sample solution to be analyzed, make the nitric acid acidity be 0.5mol / L in the sample solution to be analyzed, ferrous sulfamate concentration is 0.1mol / L L, and kept for 40min, the ferrous sulfamic acid solution reduced the valence state of Pu to Pu(Ⅲ); then added 0.8mol / L sodium nitrite solution to the sample solution to be analyzed, kept for 40min, and Pu(Ⅲ) Oxidation to Pu(Ⅳ);

[0046] (3) TTA-xylene solution extraction

[0047] Extra...

Embodiment 2

[0065] Different from Example 1, the volume of the sample solution to be analyzed is 0.3mL in the step (1); the concentration of the nitric acid solution added in the step (2) is 8mol / L, and the acidity of nitric acid in the sample solution to be adjusted is 1mol / L L, ferrous sulfamic acid concentration is 0.2mol / L, and the concentration of sodium nitrite solution is 0.9mol / L; In step (3), the concentration of TTA-xylene solution is 0.5mol / L, TTA-xylene solution and The volume ratio of Pu (Ⅳ) solution is 2:1; In step (4), the concentration of washing nitric acid is 1mol / L, and the concentration of stripping nitric acid is 8mol / L; Among the step (5), nitric acid concentration is 8mol / L, Each 25mL of pretreatment reagent, flow velocity is 20mL / min; The volume of stripping aqueous phase solution taken in step (6) is 12mL, and flow velocity is 18mL / min, and the concentration of washing nitric acid is 8mol / L, and flow velocity is 18mL / min; In step (8), the low-background α-energy s...

Embodiment 3

[0067] Different from Example 1, the volume of the sample solution to be analyzed is 0.5mL in the step (1); the concentration of the nitric acid solution added in the step (2) is 9mol / L, and the acidity of nitric acid in the sample solution to be adjusted is 1.5mol / L, the concentration of ferrous sulfamic acid is 0.2mol / L, and the concentration of sodium nitrite solution is 1.0mol / L; In step (3), the concentration of TTA-xylene solution is 0.6mol / L; In step (4) , the concentration of washing nitric acid is 1.5mol / L, and the concentration of stripping nitric acid is 9mol / L; In the step (5), the concentration of nitric acid is 9mol / L; The volume of the stripping aqueous phase solution taken in the step (6) is 15mL, The flow rate is 20mL / min, the concentration of washing nitric acid is 9mol / L, and the flow rate is 20mL / min.

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Abstract

The invention belongs to the technical field of radiochemistry, and discloses a plutonium content analysis method. According to the method, plutonium in a sample solution is extracted by utilizing a TTA-xylene solution firstly, then fission elements are further separated by utilizing anionic solid phase extraction pieces and plutonium is purified and condensed, and the purification and separation effect of plutonium is enhanced so that the plutonium content analysis method has advantages of being easy to operate and accurate in plutonium content analysis result.

Description

technical field [0001] The invention belongs to the technical field of radiation chemistry, and in particular relates to an analysis method for plutonium content. Background technique [0002] In the spent fuel reprocessing process, the α counting method is commonly used to analyze the Pu content in the feed liquid. Before analyzing the Pu content, it is necessary to separate Pu from the post-treatment feed liquid, concentrate and prepare a pretreatment process such as a radioactive source suitable for the measurement of the α measuring instrument. The impact of content analysis results is particularly important. Commonly used plutonium content analysis methods include TTA (thienoyltrifluoroacetone) extraction-α counting method, TIOA (triisooctylamine) extraction-α counting method and lanthanum fluoride carrier-α counting method, in which lanthanum fluoride The analysis procedure of the carrier tape method is more complicated, including steps such as reduction, precipitati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01T1/167
Inventor 孙宏清毛国淑杨素亮丁有钱黄昆梁小虎
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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