Rapid joint analysis method for Pu-239, Sr-90 and Cs-137 in waste liquid

A technology of pu-239 and cs-137, applied in the field of rapid combined analysis of Pu-239 and Cs-137 in waste liquid, and Sr-90, which can solve the problems of large amount of secondary waste liquid, cumbersome process and long analysis period.

Pending Publication Date: 2021-01-29
63653 FORCES PLA
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The current traditional method separates and quantifies the nuclides one by one through a separate analysis process. In the process, there are problems such as large total sample demand, cumbersome process, long analysis cycle, heavy workload, and large amount of secondary waste liquid, which is difficult to meet the military nuclear requirements. Requirements for rapid and accurate analysis and measurement of m

Method used

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  • Rapid joint analysis method for Pu-239, Sr-90 and Cs-137 in waste liquid
  • Rapid joint analysis method for Pu-239, Sr-90 and Cs-137 in waste liquid
  • Rapid joint analysis method for Pu-239, Sr-90 and Cs-137 in waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Take 1L of radioactive waste liquid produced in the laboratory in a beaker, after acidification, add 242 Pu 5pg diluent, stir well, as the test solution; add 2mL1.25mol / L Ca(NO 3 ) 2 , place the sample on a heating plate at 50°C for 20 min; add 0.75 mL of phenolphthalein indicator and 5 mL of 3.2 mol / L (NH 4 ) 2 HPO 4 solution; slowly add concentrated ammonia water to the solution, and stir continuously with a glass rod, and phenolphthalein determines the titration end point to generate Ca at this time. 3 (PO 4 ) 2 Precipitate; the precipitate naturally settled for 2 hours, and the supernatant was siphoned out; the remaining samples were transferred to a 250mL centrifuge tube, centrifuged at 3500rpm for 10min, the precipitate was separated, and the supernatant was poured out; the precipitate was washed with 10mL of water, and then centrifuged at 3500rpm for 10min. Separate the precipitate, pour off the supernatant, and combine all supernatants;

[0048] (2) U...

Embodiment 2

[0065] (1) Take 1L of radioactive waste liquid produced in the laboratory in a beaker, after acidification, add 242 Pu 10pg diluent, stir well, as the test solution; add 2mL1.25mol / L Ca(NO 3 ) 2 , place the sample on a heating plate at 60°C for 15 min; add 0.75 mL of phenolphthalein indicator and 5 mL of 3.2 mol / L (NH 4 ) 2 HPO 4 solution; slowly add concentrated ammonia water to the solution, and stir continuously with a glass rod, and phenolphthalein determines the titration end point to generate Ca at this time. 3 (PO 4 ) 2 Precipitate; the precipitate naturally settled for 3 hours, and the supernatant was siphoned out; the remaining samples were transferred to a 250mL centrifuge tube, centrifuged at 3500rpm for 10min, the precipitate was separated, and the supernatant was poured out; the precipitate was washed with 10mL of water, and then centrifuged at 3500rpm for 10min. Separate the precipitate, pour off the supernatant, and combine all supernatants;

[0066] (2) ...

Embodiment 3

[0082] In order to test and verify the separation process, take 1L of ultrapure water from 3 groups, after acidification, add 10pg of 242 Pu, 4 mg 133 Cs and 4mg 88 As the test solution in Example 1, Sr is analyzed according to the process of Example 1. The difference from Example 1 is that in step (3), directly use ICP-MS to measure the concentration of Sr in the desorption solution of the TEVA resin column. 242 The Pu content is used to calculate the recovery rate, and the experimental results are shown in Table 1.

[0083] Table 1 Pu, Sr and Cs recoveries (%)

[0084]

[0085] The recoveries of plutonium, strontium and cesium in the three samples were all relatively high.

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Abstract

The invention discloses a rapid joint analysis method for Pu-239, Sr-90 and Cs-137 in waste liquid. The rapid joint analysis method comprises the following steps of: precipitating plutonium and strontium by controlling a pH value of wastewater, and separating then from cesium; dissolving plutonium and strontium precipitates, meanwhile, adjusting a valence state of Pu to Pu(IV), separating 239Pu and 90Sr through using a TEVA resin and Sr resin double-column series connection method, and measuring 239Pu and 90Sr through using ICP-MS and a liquid scintillation counter respectively; and collectingall liquid in the plutonium and strontium precipitation process, directly enriching 137Cs through using KNiF-PAN resin, naturally airing the resin, and measuring 137Cs by using a gamma spectrometer.The rapid joint analysis method has the advantages of small sample size, simple process, short experiment period, high separation efficiency and the like, and a feasible and efficient technical meanscan be provided for rapid analysis of nuclide in nuclear emergency monitoring and nuclear safety supervision.

Description

technical field [0001] The invention relates to the technical field of radioactive element detection, in particular to a rapid combined analysis method for Pu-239, Sr-90 and Cs-137 in waste liquid. Background technique [0002] Due to nuclear tests, nuclear power plant accidents and spent fuel reprocessing activities will produce a large amount of radioactive waste, 239 Pu, 90 Sr and 137 Cs is the key nuclide among them, and its separation and quantitative analysis is an important research topic for waste liquid treatment and safety supervision. The current traditional method separates and quantifies the nuclides one by one through a separate analysis process. In the process, there are problems such as large total sample demand, cumbersome process, long analysis cycle, heavy workload, and large amount of secondary waste liquid, which is difficult to meet the military nuclear requirements. Requirements for rapid and accurate analysis and measurement of multiple radioisotop...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/74G01N30/06
CPCG01N30/02G01N30/72G01N30/74G01N30/06G01N2030/047G01N2030/062
Inventor 刘艳陈洁徐辉沈忠王煜臧建正张春
Owner 63653 FORCES PLA
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