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Separation method for separating neptunium from to-be-tested sample

A separation method and sample technology, which can be used in material separation, analysis materials, measuring devices, etc., can solve the problems of poor neptunium separation effect and inaccurate analysis, and achieve the effect of improving accuracy and yield.

Active Publication Date: 2020-09-04
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The embodiment of the present invention provides a separation method for separating neptunium from the sample to be tested, which solves the problems of poor neptunium separation effect and inaccurate analysis in the related art

Method used

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  • Separation method for separating neptunium from to-be-tested sample
  • Separation method for separating neptunium from to-be-tested sample
  • Separation method for separating neptunium from to-be-tested sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Embodiment 1 and Embodiment 2 take the sample to be tested as a rock sample as an example.

[0065] (1) Rock sample preparation:

[0066] Take standard granite rocks, and use ammonium bifluoride to dissolve the rocks (for example, according to the quality of the sample to be tested, take an appropriate amount of ammonium bifluoride, place the mixture in a digestion container, seal it, shake it slightly and mix it, and then place it in a heating device for predetermined time heating), Evaporate the solution to dryness; add 15.5mol / L nitric acid to dissolve (it can decompose organic impurities in the sample), continue to evaporate to dryness, and repeat once; add 8mol / L hydrochloric acid to dissolve, continue to evaporate to dryness, and finally add 8mol / L hydrochloric acid to dissolve and moisten .

[0067] Add separately to the completely dissolved rock solution 237 Np and natural U solution (as an indicator), add ferrous iron for reduction, the concentration of ferro...

Embodiment 2

[0089] The neptunium in the above rock samples was separated by a two-step column separation method combined with an extraction method.

[0090] Step (1) and step (2) are identical with embodiment 1; After step (2) finishes, calculate the yield of neptunium as shown in Table 1; The decontamination result of matrix element and uranium in rock is referred to Table 3;

[0091] Table 3 DMDODGA process decontamination results

[0092]

[0093] (3) Add an equal volume of 15.5mol / L nitric acid to the oxalic acid desorption solution, keep it warm in a water bath at 75-85°C for 20 minutes, add ferrous sulfamate and hydrazine hydrate to adjust the price, reduce for 30 minutes, and use 7.5mol / L nitric acid to adjust the solution Acidity; put the solution on a DOWEX-1×4 anion exchange column, use 20ml 7.5mol / L nitric acid to rinse the extraction column, and then use 15ml 0.3mol / L hydrochloric acid to desorb to obtain a desorption solution;

[0094] Calculate the yield of this step nep...

Embodiment 3

[0105] The separation method in the embodiment of the present invention is also applicable to the separation of plutonium.

[0106] The method for separating neptunium or plutonium in soil samples, river bottom sediments or mud samples, for example, includes the following steps:

[0107] (1) Use ammonium bifluoride to fully dissolve the sample (the river bottom sample needs to be dried, and remove organic matter in a muffle furnace), evaporate to dryness, add concentrated nitric acid to evaporate to dryness twice, add hydrochloric acid to evaporate to dryness once, and use 8mol / L hydrochloric acid Run out;

[0108] (2) Adjust the valence state of the elements in the solution to be tetravalent, use 8mol / L hydrochloric acid to adjust the acidity of the upper column solution; add the upper column solution to the chromatographic column containing DMDODGA resin, use 4ml4mol / L hydrochloric acid to rinse, 40ml 0.5mol / L hydrochloric acid rinse, and then use 6ml of saturated oxalic a...

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Abstract

The embodiment of the invention provides a separation method for separating neptunium from a to-be-tested sample. The method includes the following steps that ammonium bifluoride is used as a dissolving agent, and the to-be-tested sample is dissolved; dissolution of the to-be-tested sample makes contact with a first extracting agent, and an organic phase containing the neptunium is obtained; the organic phase makes contact with a complexing agent, and a water phase containing the neptunium is obtained; and the neptunium is extracted from the water phase through a second extracting agent. The first extracting agent is bisamide podand. The method for separating the neptunium is suitable for separating the neptunium from rock, soil and river bottom sediment samples. According to the method for separating the neptunium, a trace amount of neptunium can be enriched from a system containing a large quantity of interference elements or ions, the separation and purification effect of the neptunium is improved, and therefore the detection and analysis precision of the neptunium is improved.

Description

technical field [0001] The invention relates to the technical field of radionuclide recovery, in particular to a separation method for separating neptunium from samples to be tested. Background technique [0002] Isotopes of the transuranic element neptunium 237 Np has a long half-life (2.14×10 6 years), and strong radiotoxicity. Sources of neptunium in the environment include radioactive dust, nuclide leakage caused by nuclear power plant accidents, and element migration in deep geological disposal of high-level radioactive waste. Due to the strong radiotoxicity of neptunium, it is necessary to monitor neptunium in the environment. [0003] The content of neptunium in environmental samples (such as rock samples) is extremely low, and each gram of environmental samples contains only femtograms to picograms, and mass spectrometry is usually used for detection. However, it is very difficult to separate enough neptunium from rocks, and it needs to dissolve tens or even hund...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B60/02C22B3/14C22B3/26C22B3/32C22B3/34G01N30/06G01N30/08
CPCC22B3/14C22B60/0295C22B3/302C22B3/306C22B3/32G01N30/06G01N30/08G01N2030/062G01N2030/065Y02P10/20
Inventor 张曦余振华张生栋杨素亮杨志红姚曜晖
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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