CN111474234A - Method for analyzing content of trace plutonium in large amount of uranium in nuclear fuel post-processing flow - Google Patents
Method for analyzing content of trace plutonium in large amount of uranium in nuclear fuel post-processing flow Download PDFInfo
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Abstract
The invention belongs to the technical field of analytical chemistry, and relates to an analysis method for content of trace plutonium in a large amount of uranium in a nuclear fuel post-processing flow, which sequentially comprises the following steps of (1) taking a certain volume of sample, adding concentrated nitric acid to adjust the concentration of the nitric acid to 1-2 mol/L, (2) adding a sodium nitrite solution into the sample, uniformly mixing and placing for a period of time, (3) adding an extracting agent into the sample for extraction, centrifugally separating, removing a water phase and retaining an organic phase, (4) washing the organic phase for 2-5 times by using a washing solution, removing the water phase after each washing, retaining the organic phase, (5) diluting the organic phase by using isopropanol, and analyzing the diluted organic phase by using ICP-MS (inductively coupled plasma Mass Spectrometry) provided with an organic sample introduction system.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and relates to a method for analyzing the content of trace plutonium in a large amount of uranium in a nuclear fuel post-processing flow.
Background
The control of plutonium in uranium products is very strict by nuclear fuel reprocessing in reprocessing uranium products with uranium concentrations of tens of grams per litre and uranium-plutonium ratios exceeding 1 × 109Large amount of uranium to trace amount239Pu analysis is disturbed very much, need the plutonium concentration of accurate survey sample solution, just need pass through strict uranium plutonium separation preliminary treatment process, make uranium plutonium can separate. Therefore, a good uranium-plutonium separation pretreatment process is the key to the accuracy of the analysis data. And the nuclear fuel post-treatment needs many samples to be analyzed, wherein some intermediate samples and all levels of samples have small sample sampling amount due to process and equipment limitation, and the volume requirement of the analyzed samples cannot be met.
At present, there are two main methods for analyzing plutonium in uranium products: the radioactivity method and the ion exchange-mass spectrometry method are adopted.
The radioactivity method comprises the steps of separating plutonium from a large amount of uranium by using a TTA extracting agent, preparing an appropriate amount of the extracting agent on a specially-made stainless steel small disc to form α radioactive sources, and measuring the activity of the plutonium-239 in the radioactive sources by using α energy spectrum, wherein the method needs a sample volume of 5-50ml, the sample sampling amount is large, the pretreatment process of uranium-plutonium separation needs evaporation, extraction concentration and other measures, the operation steps are complex, and the measurement result of the plutonium activity is low due to self absorption of α caused by salt-containing components of the radioactive sources, so that the analysis error is large, the sensitivity is low (the analysis error is more than 10%, and the analysis lower limit is 1 × 10)-9g/L) (see [1 ]]Anion chromatographic separation- α counting method for determining trace amount of Pu [ J ] in high-level radioactive waste liquid]Atomic energy science and technology 1997,31(5): 435; [2]Liu's right, separation and determination of neptunium plutonium in large amount of uranium, design and application of ion exchange system with pressure-emptying column [ D]Beijing, national institute of atomic energy science, 2005).
The ion exchange-mass spectrometry method is that after the acid and the valence of a sample are adjusted, tetravalent plutonium is adsorbed by an ion exchange column to realize uranium-plutonium separation, then the plutonium is desorbed from the ion exchange column by dilute nitric acid, and finally the concentration of the plutonium is analyzed by mass spectrometry. The pretreatment process of uranium-plutonium separation comprises the processes of adsorption, leaching, elution and the like, the process is complex, and the pretreatment of a single sample needs 2-4 hours; the sample consumption is large, and 5-50ml is needed; samples with low plutonium concentrations will have some plutonium lost during the adsorption, elution and elution processes of ion exchange, resulting in lower analytical results (see: li, li jin ying, nigao et al. separation of traces of plutonium in uranium matrix [ J ]. nuclear chemistry and radiochemistry, 2007,29(3): 135-.
Therefore, the method has the defects of large analysis error, large sampling amount, complex separation process, long operation time and the like when the nuclear fuel post-processing process sample is analyzed.
TTA is called 2-thenoyltrifluoroacetone, is widely used for extracting and separating plutonium in a nitric acid medium, and has an extraction distribution coefficient of Pu (IV) of more than 1 × 10 in a 1-2 mol/L nitric acid system4By using the characteristic of extracting the TTA in a 1 mol/L nitric acid system, the TTA can be used for extracting the plutonium, and more than 99 percent of the plutonium can be separated from the uranium.
Inductively coupled plasma mass spectrometry (ICP-MS) is an instrument that can be used to determine ultra trace element and isotope ratios, with the advantages of: has very low detection limit (reaching ng/ml or lower), small matrix effect, simple spectral line and capability of simultaneously measuring a plurality of elements. The ICP-MS provided with the organic sample injection system can analyze trace elements of an organic phase sample.
Disclosure of Invention
The invention aims to provide a method for analyzing the content of trace plutonium in a large amount of uranium in a nuclear fuel post-processing flow, which can be used for analyzing the content of trace plutonium in the large amount of uranium in the nuclear fuel post-processing flow simply, conveniently, quickly and accurately with small required sample amount and small interference.
To achieve this object, in a basic embodiment, the invention provides a method for analyzing the content of trace plutonium in a large quantity of uranium in a nuclear fuel reprocessing line, said method comprising the following steps in sequence:
(1) taking a certain volume of sample, adding concentrated nitric acid to adjust the concentration of nitric acid to 1-2 mol/L (the sample sampling amount is generally 1-5 ml; adding concentrated nitric acid to adjust the acid to 1-2 mol/L is because the extraction distribution ratio of an extractant TTA-xylene solution to plutonium is the highest in a solution with the concentration of 1-2 mol/L nitric acid);
(2) adding sodium nitrite solution into the sample, mixing uniformly and standing for a period of time (TTA-xylene only extracts tetravalent plutonium, and the oxidation of sodium nitrite can be used to keep plutonium at tetravalent);
(3) after the extractant is added into the sample for extraction, the sample is centrifugally separated, the water phase is removed, and the organic phase is remained (the extraction water phase is removed, because uranium only exists in the water phase, and the removal of the water phase can realize uranium-plutonium separation);
(4) washing the organic phase for 2-5 times by using washing liquid, removing the water phase after each washing, and retaining the organic phase (the washing liquid is used for washing and extracting the organic phase, so that uranium carried in the organic phase can be reduced, and the interference of uranium on plutonium is reduced);
(5) the organic phase was diluted with isopropanol and the diluted organic phase was analyzed by ICP-MS equipped with an organic sampling system.
In a preferred embodiment, the invention provides a method for analyzing the trace plutonium content of a large amount of uranium in a nuclear fuel reprocessing line, wherein in step (1), 1 to 5ml of a sample is taken, concentrated nitric acid is added to the sample at a concentration of 8 to 12 mol/L, the uranium concentration in the sample is 50 to 90 g/L, and the plutonium concentration is 1.5 × 10-6-5×10-8g/L。
In a preferred embodiment, the invention provides a method for analyzing the content of trace plutonium in a large amount of uranium in a nuclear fuel reprocessing flow, wherein in step (2), 0.03 to 0.07ml of a 0.5 to 1.5 mol/L mol sodium nitrite solution is added to a sample, and the mixture is left to stand for 2 to 10 minutes after being mixed.
In a preferred embodiment, the invention provides a method for analyzing the content of trace plutonium in a large amount of uranium in a nuclear fuel reprocessing line, wherein in step (3), the extractant is a 0.4 to 0.6 mol/L TTA-xylene solution, added in a volume of 0.4 to 0.6 ml.
In a preferred embodiment, the invention provides a method for analyzing the trace plutonium content in a large amount of uranium in a nuclear fuel reprocessing flow, wherein in step (3), the extraction time is 7-15 minutes, and the centrifugation is carried out for 1-3 minutes at a rotation speed of 2000-4000 revolutions/minute (extraction time is 7-15 minutes, in order to ensure that TTA-xylene can sufficiently extract Pu (IV)).
In a preferred embodiment, the invention provides a method for analyzing the content of trace plutonium in a large amount of uranium in a nuclear fuel reprocessing flow, wherein in step (4), the washing liquid is 0.8 to 1.2 mol/L of nitric acid, and each washing time is 4 to 6 min.
In a preferred embodiment, the invention provides a method for analyzing the trace plutonium content of a large amount of uranium in a nuclear fuel reprocessing line, wherein in step (5), the dilution factor is 10 to 50.
In a preferred embodiment, the invention provides a method for analyzing the trace plutonium content in a large amount of uranium in a nuclear fuel reprocessing line, wherein in step (5), an operating curve of ICP-MS analysis is plotted for preparing an aqueous plutonium standard solution of isopropanol.
In a preferred embodiment, the invention provides a method for analyzing the content of trace plutonium in a large amount of uranium in a nuclear fuel post-processing flow, wherein in the step (5), oxygen is introduced into the organic sample introduction system (the introduction of the oxygen can make the organic phase burn sufficiently, so that the flame of ICP-MS is stable and not easy to extinguish on one hand, and on the other hand, the organic phase burns sufficiently, so that carbon atoms are changed into carbon dioxide, the carbon deposition at the outlet of the instrument is avoided and the blockage is avoided, and the sensitivity of ICP-MS is improved).
The method for analyzing the content of the trace plutonium in the large amount of uranium in the nuclear fuel post-processing flow has the advantages that the method for analyzing the content of the trace plutonium in the large amount of uranium in the nuclear fuel post-processing flow can be used for analyzing the content of the trace plutonium in the large amount of uranium in the nuclear fuel post-processing flow simply, conveniently, quickly and accurately, and is small in required sample amount and small in interference.
The analysis method can meet the requirement of analyzing the concentration of trace plutonium in a sample containing a large amount of uranium in the post-treatment process flow, and the lower limit of the plutonium analysis by the method can reach 1 × 10-10g/L, the analysis error is 5%, the analysis precision is far higher than that of a radioactive analysis method, the required sample volume is small and is only 0.5-5ml, 8-16 samples can be simultaneously operated in one batch of uranium-plutonium separation process, the time required by the whole uranium-plutonium separation pretreatment process is not more than 1 hour, and an analyst can simultaneously complete pretreatment and separation of a plurality of samples at one time according to the analysis requirement (in a thermal experiment, the analyst has the working time of 8 hours)And the number of samples to be pretreated is up to 40), so that compared with a radioactive analysis method and an ion exchange method, the pretreatment separation time is greatly shortened, the sample consumption is greatly reduced, the plutonium loss is small, and the analysis error is reduced.
According to the analysis method, a TTA extractant is selected to realize uranium-plutonium separation, and then the inductive coupling plasma mass spectrometry of the organic phase sampling system is used for analyzing the plutonium, so that the uranium-plutonium separation pretreatment time is greatly shortened, the analysis sensitivity is improved, and the sample consumption is reduced. The method successfully determines the concentration of trace plutonium in a sample containing a large amount of uranium in a batch of post-treatment process thermal experiments.
Detailed Description
The following examples further illustrate embodiments of the present invention.
Example 1:
(1) 5ml of a model sample (uranium concentration 50 g/L, plutonium concentration 5.12 × 10)-8g/L), adding 1.2ml of 10 mol/L nitric acid to make the acidity of the solution reach 2 mol/L;
(2) adding 0.05ml of 1 mol/L sodium nitrite solution, uniformly mixing, standing for 2 minutes, and oxidizing plutonium to quadrivalence;
(3) adding 0.5 mol/L TTA-xylene solution 0.5ml of an extractant to extract Pu (IV) for 10min, centrifugally separating for 2min at the rotating speed of 3000 r/min, and discarding the water phase to realize uranium-plutonium separation;
(4) the organic phase was washed three times with 1 mol/L nitric acid for 5 minutes each to elute a small amount of uranium entrained in the organic phase;
(5) diluting 0.1ml of organic phase with isopropanol to 2.5ml, analyzing plutonium concentration with ICP-MS equipped with organic sample injection system (drawing working curve of ICP-MS analysis of aqueous phase plutonium standard solution prepared with isopropanol, introducing oxygen into organic sample injection system), and analyzing plutonium concentration to 5.26 × 10-8g/L, relative standard deviation 2.73%.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (9)
1. A method for analyzing the content of trace plutonium in a large amount of uranium in a nuclear fuel reprocessing process is characterized by sequentially comprising the following steps:
(1) taking a certain volume of sample, and adding concentrated nitric acid to adjust the concentration of the nitric acid to 1-2 mol/L;
(2) adding sodium nitrite solution into the sample, uniformly mixing and standing for a period of time;
(3) adding an extracting agent into a 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 aqueous phase after each washing, and retaining the organic phase;
(5) the organic phase was diluted with isopropanol and the diluted organic phase was analyzed by ICP-MS equipped with an organic sampling system.
2. The method according to claim 1, wherein in the step (1), 1 to 5ml of the sample is taken, and concentrated nitric acid is added to the sample in an amount of 8 to 12 mol/L, the sample has a uranium concentration of 50 to 90 g/L, and a plutonium concentration of 1.5 × 10-6-5×10-8g/L。
3. The analytical method according to claim 1, wherein in the step (2), 0.03 to 0.07ml of 0.5 to 1.5 mol/L mol sodium nitrite solution is added to the sample, and the mixture is left to stand for 2 to 10 minutes.
4. The analytical method according to claim 1, wherein in the step (3), the extractant is a 0.4 to 0.6 mol/L TTA-xylene solution, and the volume of the extractant added is 0.4 to 0.6 ml.
5. The analytical method of claim 1, wherein: in the step (3), the extraction time is 7-15 minutes, and the centrifugal separation is carried out for 1-3 minutes at the rotating speed of 2000-4000 revolutions per minute.
6. The analytical method according to claim 1, wherein in the step (4), the washing solution is 0.8 to 1.2 mol/L of nitric acid, and each washing time is 4 to 6 min.
7. The analytical method of claim 1, wherein: in the step (5), the dilution multiple is 10-50 times.
8. The analytical method of claim 1, wherein: and (5) drawing a working curve for ICP-MS analysis of the aqueous plutonium standard solution prepared into the isopropanol.
9. The analytical method of claim 1, wherein: and (5) introducing oxygen into the organic sample introduction system.
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Cited By (6)
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| CN113311465A (en) * | 2021-04-08 | 2021-08-27 | 中国辐射防护研究院 | Combined analysis method for content of Pu isotope and Np-237 in sample |
| CN113311466A (en) * | 2021-04-08 | 2021-08-27 | 中国辐射防护研究院 | Method for analyzing plutonium content in plant sample |
| CN113311469A (en) * | 2021-04-12 | 2021-08-27 | 中国辐射防护研究院 | Method for analyzing uranium isotope content in reduction system |
| CN113409972A (en) * | 2021-06-23 | 2021-09-17 | 中国核动力研究设计院 | Nuclear fuel burnup measuring process |
| CN114136883A (en) * | 2021-11-22 | 2022-03-04 | 杭州谱育科技发展有限公司 | Detection system and method for multivalent plutonium element in nuclear fuel reprocessing |
| CN118050767A (en) * | 2024-01-10 | 2024-05-17 | 中国核电工程有限公司 | Sample analysis system and method for nuclear fuel post-treatment plant |
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| CN118050767A (en) * | 2024-01-10 | 2024-05-17 | 中国核电工程有限公司 | Sample analysis system and method for nuclear fuel post-treatment plant |
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