CN103337265A - Chemical separation procedure for burnup analysis of spent fuel element - Google Patents
Chemical separation procedure for burnup analysis of spent fuel element Download PDFInfo
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- CN103337265A CN103337265A CN2013102499289A CN201310249928A CN103337265A CN 103337265 A CN103337265 A CN 103337265A CN 2013102499289 A CN2013102499289 A CN 2013102499289A CN 201310249928 A CN201310249928 A CN 201310249928A CN 103337265 A CN103337265 A CN 103337265A
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Abstract
The invention relates to a chemical separation procedure for burnup analysis of a spent fuel element. The chemical separation procedure comprises the following steps of: (I) dissolving a spent fuel element block, namely putting the spent fuel element block into concentrated nitric acid and concentrated hydrochloric acid mixed liquid with the volume ratio of 3:1 to make the spent fuel element block be completely dissolved, and cooling the dissolving liquid to room temperature; (II) diluting the dissolving liquid, namely mixing the dissolving liquid cooled in the step (I) and nitric acid, uniformly stirring the dissolving liquid and the nitric acid to obtain diluted dissolving liquid; and (III) separating uranium, plutonium, molybdenum and neodymium by a column chromatography method through the diluted dissolving liquid obtained in the step (II). The invention establishes a novel chemical separation procedure for measuring the burnup of the spent fuel element; according to the chemical separation procedure, some novel levextrel, ion exchange material and high performance liquid chromatography technologies are adopted, so that chemical separation of the uranium, the plutonium, the molybdenum and the neodymium is realized; the operation procedure is greatly simplified; the operation difficulty is reduced; and the radiation to researchers is reduced.
Description
Technical field
The invention belongs to spent fuel element burnup measurement technical field, be specifically related to the Chemical Decomposition flow process for the spent fuel element burnup analysis.
Background technology
The radiochemical analysis of spent fuel element burnup is internationally recognized method the most accurately.Nuclear submarine and novel nuclear reactor all need carry out the element test, have been generally the space burnup that obtains reactor core and have distributed, and understand single element in detail exactly axially and radially burnup distribution, and the destructive analysis of element is very necessary.Twentieth century 70 years, China has begun the research of burnup measurement method, the burnup measurement group has been developed analytical approach for this reason, 08,09 element burnup, 728 test element burnups have accurately been measured in succession, for the safe operation of China's nuclear submarine provides assurance, for China's seat of honour nuclear power station provides design parameter.Problems such as but flow processs many, that separate that there is sport technique segment in putting of the burnup assay method of setting up are loaded down with trivial details, the suffered dosage of researchist is big.Want people more than 30 to participate in as a burnup measurement, the radioactive intensity of operation reaches hundreds of Curie, and the used time reaches tens of days, and operation can't be satisfied the needs of current a large amount of sample analysis so for a long time.
Summary of the invention
At the defective that exists in the prior art, the purpose of this invention is to provide a kind of Chemical Decomposition flow process for the spent fuel element burnup analysis, this Chemical Decomposition flow process is simple to operation, and the suffered radiation dose of researchist is little.
For reaching above purpose, the technical solution used in the present invention is: be used for the Chemical Decomposition flow process of spent fuel element burnup analysis, may further comprise the steps:
(I) dissolving spent fuel element piece: the spent fuel element piece is put into the red fuming nitric acid (RFNA) that volume ratio is 3:1-concentrated hydrochloric acid mixed liquor, make dissolving fully, lysate is cooled to room temperature;
(II) dilution lysate: the cooled lysate that step (I) is obtained mixes with nitric acid, stirs, the lysate after obtaining diluting;
Lysate after the dilution that (III) use step (II) obtains adopts post partition method SEPARATION OF URANIUM, plutonium, molybdenum and neodymium element.
Further, in the step (I), the proportioning of spent fuel element piece and red fuming nitric acid (RFNA)-concentrated hydrochloric acid mixed liquor is 1g:120~150mL, and the spent fuel element piece is 0.08~0.09MPa, 85~90 ℃ of following heating for dissolving 50~60 minutes at pressure.
Further, in the step (II), it is 0.4mol/L nitric acid that nitric acid adopts concentration, and the cooled lysate that obtains of step (I) and the volume ratio of 0.4mol/L nitric acid are 1:200~1:300.
Further, in the step (III), may further comprise the steps during SEPARATION OF URANIUM: the lysate of getting after the dilution that 1mL step (II) obtains is made sample liquid, changes in the centrifuge tube, adds medium HNO
3, Fe (NH
2SO
3)
2And N
2H
6(NO
3)
2, regulate in the sample liquid and contain 4mol/L HNO
3, 0.05mol/lFe (NH
2SO
3)
2With 0.05mol/L N
2H
6(NO
3)
2, stir 3~5min, place 25min; Make the sample liquid regulated behind the medium flow through the TBP extracting chromatographic column with the flow velocity of 0.5mL/min, use 4mol/LHNO then
3Deionized water wash-out uranium is used in drip washing at last, collects the eluent of uranium-bearing.
Under the preferable case, in the method for SEPARATION OF URANIUM, adopt the TBP extracting chromatographic column of φ 3mm * 200mm, use 4mol/L HNO during drip washing
320 column volumes of drip washing are with the deionized water wash-out uranium of 6 column volumes.
Further, in the step (III), may further comprise the steps during separated plutonium: the lysate of getting after the dilution that 1mL step (II) obtains is made sample liquid, changes in the centrifuge tube, adds medium HNO
3And Fe (NH
2SO
3)
2, regulate sample liquid and contain 1mol/L HNO
3, 0.1mol/l Fe (NH
2SO
3)
2, stir 3~5min, place 25min; Add medium HNO again
3And NaNO
2, regulate and contain 7.1mol/L HNO
3With 0.5mol/L NaNO
2, stir 3~5min, place 25min; Make the sample liquid regulated behind the medium flow through anion column with the flow velocity of 0.3mL/min, use 7.1mol/L HNO
30.35mol/LHNO is used in washing again
30.35mol/L HNO is used in drip washing then
3-0.1mol/L DMHAN(N, the N-dimethyl hydroxylamine) mixed liquor wash-out plutonium, collect the eluent that contains plutonium.
Further again, anion column adopts the pyridine type anion column of φ 3mm * 35mm.
Under the preferable case, in the method for separated plutonium, during drip washing with the 7.1mol/LHNO of 20 column volumes
3The 0.35mol/L HNO of 3 column volumes is used in drip washing again
3The 0.35mol/L HNO of 12 column volumes is used in drip washing at last
3-0.1mol/L DMHAN(N, the N-dimethyl hydroxylamine) mixed liquor wash-out plutonium.
Further, in the step (III), may further comprise the steps during Separation of Molybdenum: the lysate of getting after the dilution that 1mL step (II) obtains is made sample liquid, changes in the centrifuge tube, adds medium HNO
3, regulate sample liquid and contain 0.8mol/L HNO
3, stir 1~2min; Make the sample liquid regulated behind the medium flow through the molybdenum resin column with the flow velocity of 1mL/min, use 0.8mol/L HNO
30.1mol/L NH is used in washing then
4OH wash-out molybdenum is collected the eluent that contains molybdenum.
Further again, the molybdenum resin that adopts in the molybdenum resin column is that the prepolymer by α-An Xixiangwo and styrene-divinylbenzene is polymerized, and can adopt following method preparation:
1) preparation dispersant solution: under agitation polyvinyl alcohol (PVA) and benzoyl peroxide are joined in the deionized water, be warmed up to 45-50 ℃, both are dissolved fully, concentration is 1.5-2wt%;
2) preparation contains the organic phase of α-An Xixiangwo: α-An Xixiangwo is joined in the organic solvent, the proportioning of α-An Xixiangwo and organic solvent is 1g:10-20mL, stirring makes the α-An Xixiangwo dissolving, add an amount of tackifier (as polystyrene or polyethylene glycol stearate diester) then, ultrasonic dispersion 30-40 minute;
3) preparation styrene-divinylbenzene prepolymer: styrene, divinylbenzene and initiating agent are mixed, stir, be warming up to 65-70 ℃, make reactant generation prepolymerization reaction 30-40 minute, obtain styrene-divinylbenzene prepolymer, concrete with reference to existing maturation process;
4) synthetic resin: styrene-divinylbenzene prepolymer that step 3) is obtained joins in the dispersant solution that step 1) obtains, and stirs to make it be dispersed into the pearl body, slowly be warming up to 65-70 ℃ after; Add step 2 in the gained potpourri) organic phase that contains α-An Xixiangwo that obtains, styrene in the system-divinylbenzene prepolymer, dispersant solution and the volume ratio of organic phase that contains α-An Xixiangwo are for (2-1): (2-1): 1, continue to be warming up to 80-85 ℃, reaction is 10-15 hour under this temperature, stop heating, naturally cooling; When temperature is down to 40-50 ℃, reaction mixture is filtered, wash sediment with water, dry naturally, namely get the synthetic resin that contains α-An Xixiangwo.
Under the preferable case, in the method for Separation of Molybdenum, the specification of molybdenum resin column is φ 3mm * 35mm, during washing with the 0.8mol/L HNO of 5 column volumes
3Washing, during wash-out with the 0.1mol/L NH of 3~5 column volumes
4OH wash-out molybdenum.
Further, may further comprise the steps when separating neodymium in the step (III): the lysate of getting after the dilution that 1mL step (II) obtains is made sample liquid, flows through cation exchange column with the flow velocity of 0.5mL/min, with 1.5mol/L HCl washing, uses 4mol/L HNO again
3The wash-out rare earth is collected the eluent that contains multiple rare earth element; To contain the eluent evaporate to dryness of multiple rare earth element, use nitric acid dissolve again, contain 0.01mol/L HNO in the regulator solution
3, flow through performance liquid chromatographic column with the flow velocity of 1.5mL/min, with the drip washing of 0.07mol/L alpha-hydroxybutyric dehydrogenase, collect the fraction that contains neodymium; Make the fraction that contains neodymium flow through (2 one ethylhexyl) phosphoric acid (HDEHP) extracting chromatographic column with the flow velocity of 0.5mL/min, use 0.02mol/L HNO
34mol/L HNO is used in drip washing
3The wash-out neodymium obtains containing the eluent of neodymium.
Under the preferable case, separate in the method for neodymium, when separating with cation exchange column, adopt the strong-acid type cation exchange column, specification is φ 3mm * 200mm, with the 1.5mol/LHCl washing of 20 column volumes, uses the 4mol/L HNO of 10~15 column volumes again during washing
3The wash-out rare earth; When containing the eluent of multiple rare earth element with the performance liquid chromatographic column processing, carry out under post pressure 2~2.5MPa, the specification of performance liquid chromatographic column is φ 4.6mm * 250mm; When separating with the HDEHP extracting chromatographic column, the specification of HDEHP extracting chromatographic column is φ 3mm * 80mm, uses 10mL 0.02mol/L HNO during drip washing
3Drip washing, during wash-out with 8~10 column volumes 4mol/L HNO
3The wash-out neodymium.
The present invention has set up one group of new Chemical Decomposition flow process in the spent fuel element burnup measurement, this Chemical Decomposition flow process has adopted some new extration resins, ion exchange material and high-efficient liquid phase chromatogram technology, realize the Chemical Decomposition of uranium, plutonium, molybdenum, neodymium, simplified operating process greatly, reduce operation easier, reduced the suffered radiation dose of researchist simultaneously.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment
The Chemical Decomposition flow process that the present invention is used for the spent fuel element burnup analysis can may further comprise the steps:
Step (I): dissolving spent fuel element piece.
5.2g spent fuel element piece is put into the three-necked bottle that fills the red fuming nitric acid (RFNA) that 140~150mL volume ratio is 3:1-concentrated hydrochloric acid mixed liquor, and 95 ℃ of water-bath heating are reduced pressure down and were dissolved 60 minutes, and pressure is 0.08MPa, and lysate is cooled to room temperature.
After the member block dissolving, lysate is applied on the glass sheet, does not observe particle with electron microscope, show that member block dissolves fully.
Step (II): dilution lysate.
Get the cooled lysate of 0.5mL to conical flask, mix with 100mL 0.4mol/L nitric acid, fully stir and obtain diluting lysate.Can in the dilution lysate, add suitable radiotracer, be used for follow-up tracer analysis.
Step (III), the dilution lysate that uses step (II) to obtain adopts post partition method SEPARATION OF URANIUM, plutonium, molybdenum and neodymium.In this step, different radioelement adopts different separating column and process conditions to separate, and concrete operation method is as follows:
A) uranium separates: the dilution lysate of getting 1mL step (II) changes in the centrifuge tube, adds medium red fuming nitric acid (RFNA), Fe (NH
2SO
3)
2And N
2H
6(NO
3)
2, regulate in the dilution lysate and contain 4mol/LHNO
3, 0.05mol/l Fe (NH
2SO
3)
2With 0.05mol/L N
2H
6(NO
3)
2Medium, glass bar stirs 3~5min, places 25min; Make the lysate after the placement flow through the TBP extracting chromatographic column of φ 3mm * 200mm with the flow velocity of 0.5mL/min, use the 4mol/L HNO of 20 column volumes then
3The deionized water wash-out uranium of 6 column volumes is used in drip washing at last, collects the eluent of uranium-bearing.
B) plutonium separates: the dilution lysate of getting 1mL step (II) changes in the centrifuge tube, adds medium red fuming nitric acid (RFNA) and Fe (NH
2SO
3)
2, regulate the dilution lysate and contain 1mol/L HNO
3, 0.1mol/lFe (NH
2SO
3)
2, glass bar stirs 3~5min, places 25min; Add dense HNO again
3And NaNO
2, regulate the dilution lysate and contain 7.1mol/L HNO
3With 0.5mol/L NaNO
2, glass bar stirs 3~5min, places 25min; Make the lysate after the placement flow through the pyridine type anion column of φ 3mm * 35mm with the flow velocity of 0.3mL/min, with the 7.1mol/L HNO of 20 column volumes
3Drip washing is with the 0.35mol/L HNO of 3 column volumes
3Drip washing is with the 0.35mol/LHNO of 12 column volumes
3-0.1mol/L DMHAN(N, the N-dimethyl hydroxylamine) mixed liquor wash-out plutonium, collect the eluent that contains plutonium.
C) molybdenum separates: the dilution lysate of getting 1mL step (II) changes in the centrifuge tube, adds the medium red fuming nitric acid (RFNA), regulates the dilution lysate and contains 0.8mol/L HNO
3, glass bar stirs 1~2min; Make the lysate after the adjusting flow through the molybdenum resin column (resin that molybdenum resin wherein can adopt the prepolymer of α-An Xixiangwo and styrene-divinylbenzene to be polymerized) of φ 3mm * 35mm with the flow velocity of 1mL/min, with the 0.8mol/L HNO of 5 column volumes
3Washing is with the 0.1mol/LNH of 3 column volumes
4OH wash-out molybdenum is collected the eluent that contains molybdenum.
D) neodymium separates: the dilution lysate of getting 1mL step (II) changes in the centrifuge tube, flows through the cation exchange column of φ 3mm * 200mm with the flow velocity of 0.5mL/min, washs with the 1.5mol/L HCl of 20 column volumes, uses 4mol/L HNO again
3The wash-out rare earth is collected eluent; With the eluent evaporate to dryness, with the red fuming nitric acid (RFNA) dissolving, contain 0.01mol/L HNO in the regulator solution again
3Flow through the performance liquid chromatographic column (it is 2.1MPa that post is pressed) of φ 4.6mm * 250mm with the flow velocity of 1.5mL/min, with 0.07mol/L alpha-hydroxybutyric dehydrogenase (pH is 3.8) drip washing, collection contains the fraction of neodymium, make the fraction that contains neodymium flow through the HDEHP extracting chromatographic column of φ 3mm * 80mm with the flow velocity of 0.5mL/min, with 10mL 0.02mol/L HNO
34mol/L HNO is used in drip washing
3Wash-out obtains containing the eluent of neodymium.
After separation finishes, adopt mass spectrum, liquid sudden strain of a muscle and gamma energy spectrometer to analyze the content of element in each eluent, as calculated as can be known, the chemical recovery rate of uranium, plutonium, molybdenum, neodymium is respectively 95%, 91%, 98% and 80%, and purity all can reach the requirement of mass spectrophotometry.
The whole process operation can be finished in 8 hours, had shortened analysis time greatly.
Above-described embodiment just illustrates of the present invention, and the present invention also can implement with other ad hoc fashion or other particular form, and does not depart from main idea of the present invention or essential characteristic.Therefore, the embodiment of description all should be considered as illustrative from any aspect but not be determinate.Scope of the present invention should be by additional claim explanation, and the intention of any and claim and the variation of scope equivalence also should be within the scope of the present invention.
Claims (10)
1. be used for the Chemical Decomposition flow process of spent fuel element burnup analysis, may further comprise the steps:
(I) dissolving spent fuel element piece: the spent fuel element piece is put into the red fuming nitric acid (RFNA) that volume ratio is 3:1-concentrated hydrochloric acid mixed liquor, make dissolving fully, lysate is cooled to room temperature;
(II) dilution lysate: the cooled lysate that step (I) is obtained mixes with nitric acid, stirs, the lysate after obtaining diluting;
Lysate after the dilution that (III) use step (II) obtains adopts post partition method SEPARATION OF URANIUM, plutonium, molybdenum and neodymium element.
2. the Chemical Decomposition flow process for the spent fuel element burnup analysis according to claim 1, it is characterized in that, in the step (I), the proportioning of spent fuel element piece and red fuming nitric acid (RFNA)-concentrated hydrochloric acid mixed liquor is 1g:120~150mL, and the spent fuel element piece is 0.08~0.09MPa, 85~90 ℃ of following heating for dissolving 50~60 minutes at pressure.
3. the Chemical Decomposition flow process for the spent fuel element burnup analysis according to claim 1, it is characterized in that, in the step (II), it is 0.4mol/L nitric acid that nitric acid adopts concentration, and the cooled lysate that obtains of step (I) and the volume ratio of 0.4mol/L nitric acid are 1:200~1:300.
4. according to the arbitrary described Chemical Decomposition flow process for the spent fuel element burnup analysis of claim 1-3, it is characterized in that, in the step (III), may further comprise the steps during SEPARATION OF URANIUM:
The lysate of getting after the dilution that 1mL step (II) obtains is made sample liquid, changes in the centrifuge tube, adds medium HNO
3, Fe (NH
2SO
3)
2And N
2H
6(NO
3)
2, regulate in the sample liquid and contain 4mol/L HNO
3, 0.05mol/l Fe (NH
2SO
3)
2With 0.05 mol/L N
2H
6(NO
3)
2, stir 3~5min, place 25min;
Make the sample liquid regulated behind the medium flow through the TBP extracting chromatographic column with the flow velocity of 0.5mL/min, use 4 mol/L HNO then
3Deionized water wash-out uranium is used in drip washing at last, collects the eluent of uranium-bearing.
5. according to the arbitrary described Chemical Decomposition flow process for the spent fuel element burnup analysis of claim 1-3, it is characterized in that, in the step (III), may further comprise the steps during separated plutonium:
The lysate of getting after the dilution that 1mL step (II) obtains is made sample liquid, changes in the centrifuge tube, adds medium HNO
3And Fe (NH
2SO
3)
2, regulate sample liquid and contain 1mol/L HNO
3, 0.1mol/l Fe (NH
2SO
3)
2, stir 3~5min, place 25min; Add HNO again
3And NaNO
2, regulate and contain 7.1mol/L HNO
3With 0.5mol/L NaNO
2, stir 3~5min, place 25min;
Make the sample liquid regulated behind the medium flow through anion column with the flow velocity of 0.3 mL/min, with 7.1 mol/L HNO
30.35 mol/L HNO is used in washing again
30.35 mol/L HNO is used in drip washing then
3-0.1mol/L N, N-dimethyl hydroxylamine mixed liquor wash-out plutonium is collected the eluent that contains plutonium.
6. the Chemical Decomposition flow process for the spent fuel element burnup analysis according to claim 5 is characterized in that, described anion column is the pyridine type anion column.
7. according to the arbitrary described Chemical Decomposition flow process for the spent fuel element burnup analysis of claim 1-3, it is characterized in that, may further comprise the steps during Separation of Molybdenum in the step (III):
The lysate of getting after the dilution that 1mL step (II) obtains is made sample liquid, changes in the centrifuge tube, adds medium HNO
3, regulate sample liquid and contain 0.8 mol/L HNO
3, stir 1~2min;
Make the sample liquid regulated behind the medium flow through the molybdenum resin column with the flow velocity of 1mL/min, with 0.8 mol/L HNO
30.1mol/L NH is used in washing then
4-OH wash-out molybdenum is collected the eluent that contains molybdenum.
8. the Chemical Decomposition flow process for the spent fuel element burnup analysis according to claim 7 is characterized in that, the molybdenum resin that adopts in the described molybdenum resin column is that the prepolymer by α-An Xixiangwo and styrene-divinylbenzene is polymerized.
9. according to the arbitrary described Chemical Decomposition flow process for the spent fuel element burnup analysis of claim 1-3, it is characterized in that, may further comprise the steps when separating neodymium in the step (III):
The lysate of getting after the dilution that 1mL step (II) obtains is made sample liquid, flows through cation exchange column with the flow velocity of 0.5mL/min, with 1.5mol/L HCl washing, uses 4mol/L HNO again
3The wash-out rare earth is collected the eluent that contains multiple rare earth element;
To contain the eluent evaporate to dryness of multiple rare earth element, use nitric acid dissolve again, contain 0.01mol/L HNO in the regulator solution
3, flow through performance liquid chromatographic column with the flow velocity of 1.5mL/min, with the drip washing of 0.07mol/L a-hydroxy-iso-butyric acid, collect the fraction that contains neodymium;
Make the fraction that contains neodymium flow through the di-(2-ethylhexyl)phosphoric acid extracting chromatographic column with the flow velocity of 0.5mL/min, use 0.02mol/L HNO
34mol/L HNO is used in drip washing
3The wash-out neodymium obtains containing the eluent of neodymium.
10. the Chemical Decomposition flow process for the spent fuel element burnup analysis according to claim 9 is characterized in that, described cation exchange column is the strong-acid type cation exchange column.
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CN103342769A (en) * | 2013-06-25 | 2013-10-09 | 中国原子能科学研究院 | Preparation method of molybdenum separation resin |
CN104361917A (en) * | 2014-11-06 | 2015-02-18 | 中国原子能科学研究院 | Automatic radiochemical separation system used for measuring fuel consumption of spent fuel element |
CN110831681A (en) * | 2017-06-29 | 2020-02-21 | 原子能和替代能源委员会 | Carboxamide for separating uranium (VI) and plutonium (IV) without reducing plutonium (IV) |
CN113409972A (en) * | 2021-06-23 | 2021-09-17 | 中国核动力研究设计院 | Nuclear fuel burnup measuring process |
CN113795894A (en) * | 2020-10-14 | 2021-12-14 | 中广核研究院有限公司 | Spent fuel dry post-treatment method based on plasma |
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