CN106932423A - A kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample - Google Patents
A kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample Download PDFInfo
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Abstract
The invention belongs to spentnuclear fuel post-processing technology field, and in particular to a kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample.Comprise the following steps：It is prepared by nitrate acid and hydrofluoric acid；Plutonium standard substance is sampled and the sampling of uranium standard substance；Standard substance powder dissolves；It is prepared by uranium and plutonium standard reserving solution；It is prepared by uranium, neptunium, plutonium series standard；Measurement series standard.A kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample that the present invention is provided, the need for waste minimization and spent fuel reprocessing process control analysis can be met.
Description
Technical field
The invention belongs to spentnuclear fuel post-processing technology field, and in particular to a kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample.
Background technology
External power reactor spentnuclear fuel post processing starting is relatively early, and reprocessing analysis technology has obtained tremendous development and raising, and classical radiochemical analysis is increasingly replaced by modern instrumental method；Be applied to the pre- diffraction X-fluorescence technology of graphite crystal in reprocessing plant industrial analysis by the Areva factories of France.But because the analytical technology of external uranium, neptunium, plutonium is blocked, the analysis method for directly measure uranium, neptunium, plutonium has not been reported.
The country common are extract and separate α counting methods, AAS, extract and separate alpha energy spectrum method etc. for slightly enriched uranium, neptunium, the analysis method of plutonium, but the above method belongs to destructive method of analysis, have the shortcomings that cumbersome, sample analysis time is long, personnel's exposure dosage is big.China Atomic Energy Science Research Institute develops graphite crystal diffracting X-rays fluorescence analyser, the research in terms of having carried out single uranium, plutonium with the instrument.The above method can not simultaneously determine uranium, neptunium, plutonium in process sample.
The content of the invention
It is an object of the invention to provide a kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample, the need for meeting waste minimization and spent fuel reprocessing process control analysis.
To reach above-mentioned purpose, the technical solution used in the present invention is：
A kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample, comprises the following steps：
(1) prepared by nitrate acid and hydrofluoric acid：In pipetting the pure nitric acid of analysis to the volumetric flask demarcated with pipette, then with pipette pipette analytically pure hydrofluoric acid to the volumetric flask, be prepared into concentration of nitric acid for 8mol/L~12mol/L, hydrofluoric acid concentration is the nitration mixture of 0.05mol/L~0.10mol/L；
(2) plutonium standard substance sampling：Plutonium dioxide standard substance is accurately weighed using a ten thousandth balance to put into high pressure counteracting tank, nitrate acid and hydrofluoric acid nitration mixture 4mL obtained by step (1)~5mL is added into high-pressure digestion tank, close the lid, high-pressure digestion tank is put into supporting stainless steel cylinder, stainless steel cylinder puts to the electric furnace with graphite cake heating；Uranium standard substance is sampled：Triuranium octoxide standard substance is accurately weighed using a ten thousandth balance to put into high pressure counteracting tank, nitrate acid and hydrofluoric acid nitration mixture 4mL obtained by step (1)~5mL is added into high-pressure digestion tank, close the lid, high-pressure digestion tank is put into supporting stainless steel cylinder, stainless steel cylinder puts to the electric furnace with graphite cake heating；
(3) standard substance powder dissolving：The stainless steel cylinder that step (2) holds sample is heated into 4h~8h at 160~180 DEG C, high-pressure digestion cover is opened, confirms that the uranium in high-pressure digestion tank and the solid powder of plutonium are completely dissolved；
(4) prepared by uranium and plutonium standard reserving solution：During two samples of step (3) are moved into two volumetric flasks with glue head dropper, with the nitric acid constant volume of 1mol/L~4mol/L, that is, the uranium and plutonium standard reserving solution of water phase are obtained；
(5) prepared by uranium, neptunium, plutonium series standard：Uranium, plutonium standard reserving solution and the neptunium standard liquid of accurate removing step (4) are distinguished in 6 10ml volumetric flasks, with the salpeter solution constant volume of 1mol/L~4mol/L, you can obtain serial uranium, neptunium, plutonium mixed standard solution；
(6) series standard is measured：The series standard solution 1.0mL~1.2mL of removing step (5) determines 600s~1000s in bottle is measured with the pre- diffracting X-rays fluorescence analyser of graphite crystal respectively, and the measuring condition of instrument is:Voltage -50kV, electric current 4mA, preserve measurement spectrogram.
Plutonium dioxide standard substance is GBW 04201 in the step (2).
Triuranium octoxide standard substance is GBW 04201 in the step (2).
Step (2) the mesohigh counteracting tank material is polytetrafluoroethylene (PTFE).
Neptunium standard liquid is United Kingdom National physics laboratory in the step (5), and activity is 148.2kBq.g-1, expanded uncertainty is ± 1.6kBq.g-1Solution.
After described step (6), following steps are also carried out：(7) drawing curve：Using the spectrogram of step (6) using deduction background, peak height method drawing curve；(8) add-back yield checking again：Optional step (7) working curve determines unknown aqueous process sample 6 times, and water phase uranium, neptunium, plutonium standard liquid are separately added into the unknown process sample, uranium, neptunium, the content addition of plutonium standard is prepared respectively and is 10.00 × 10-6g、10.00×10-6g、10.00×10-6Three 1mL aqueous samples of g, the uranium of the addition of measure, neptunium, the average of the measurement result of the standard of plutonium are respectively 9.99 × 10-6g、10.28×10-6g、10.02×10-6G, then add-back yield is respectively 99.9%, 102.8%, 100.2% again.
Having the beneficial effect that acquired by the present invention：
Determined while slightly enriched uranium, neptunium, plutonium content in the achievable radioactive liquid sample of the present invention, and 5 × 10-3When in the range of g/L~1.00g/L, the relative standard deviation of measurement result is better than 5%, and add-back yield is 95%~110% again, can meet the requirement of control analysis.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.
The analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample of the present invention comprises the following steps：
(1) prepared by nitrate acid and hydrofluoric acid：In the pure nitric acid of a certain amount of analysis to the volumetric flask demarcated being pipetted with pipette, in pipetting a certain amount of analytically pure hydrofluoric acid to the volumetric flask with pipette again, it is the nitration mixture of 0.05mol/L~0.10mol/L for 8mol/L~12mol/L- hydrofluoric acid concentrations to be prepared into concentration of nitric acid.
(2) plutonium standard substance sampling：A certain amount of plutonium dioxide standard substance (GBW 04201) is accurately weighed using a ten thousandth balance to put into the high-pressure digestion tank of polytetrafluoroethylene (PTFE) material, nitrate acid and hydrofluoric acid nitration mixture 4mL obtained by step (1)~5mL is added into high-pressure digestion tank, close the lid, high-pressure digestion tank is put into supporting stainless steel cylinder, stainless steel cylinder puts to the electric furnace with graphite cake heating.
Uranium standard substance is sampled：A certain amount of triuranium octoxide standard substance (GBW 04201) is accurately weighed using a ten thousandth balance to put into the high-pressure digestion tank of polytetrafluoroethylene (PTFE) material, nitrate acid and hydrofluoric acid nitration mixture 4mL obtained by step (1)~5mL is added into high-pressure digestion tank, close the lid, high-pressure digestion tank is put into supporting stainless steel cylinder, stainless steel cylinder puts to the electric furnace with graphite cake heating.
(3) standard substance powder dissolving：The stainless steel cylinder for holding sample of step (2) is heated into 4h~8h at 160~180 DEG C, counteracting tank lid is opened, confirms that the uranium in high-pressure digestion tank and the solid powder of plutonium are completely dissolved.
(4) prepared by uranium and plutonium standard reserving solution：During two samples of step (3) are moved into two volumetric flasks with glue head dropper, with the nitric acid constant volume of 1mol/L~4mol/L, that is, the uranium and plutonium standard reserving solution of water phase are obtained.
(5) prepared by uranium, neptunium, plutonium series standard：(United Kingdom National physics laboratory, activity is 148.2kBq.g accurately to pipette uranium, plutonium standard reserving solution and the neptunium standard liquid of a certain amount of step (4) respectively-1, expanded uncertainty is ± 1.6kBq.g-1) in 6 10ml volumetric flasks, with the salpeter solution constant volume of 1mol/L~4mol/L, you can obtain serial uranium, neptunium, plutonium mixed standard solution.
(6) series standard is measured：In bottle is measured, the measuring condition for determining 600s~1000s instruments with the pre- diffracting X-rays fluorescence analyser of graphite crystal is the series standard 1.0mL~1.2mL of removing step (5) respectively:Voltage is -50kV, and electric current is 4mA, preserves measurement spectrogram.
(7) drawing curve：Using the spectrogram of step (6) using deduction background, peak height method drawing curve.
(8) add-back yield checking again：Optional step (7) working curve determines unknown aqueous process sample 6 times, and water phase uranium, neptunium, plutonium standard liquid are separately added into the unknown process sample, uranium, neptunium, the content addition of plutonium standard is prepared respectively and is 10.00 × 10-6g、10.00×10-6g、10.00×10-6Three 1mL aqueous samples of g, the uranium of the addition of measure, neptunium, the average of the measurement result of the standard of plutonium are respectively 9.99 × 10-6g、10.28×10-6g、10.02×10-6G, then add-back yield is respectively 99.9%, 102.8%, 100.2% again.
Claims (6)
1. a kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample, it is characterised in that：Bag
Include following steps：
(1) prepared by nitrate acid and hydrofluoric acid：In the pure nitric acid of analysis to the volumetric flask demarcated being pipetted with pipette, then
In pipetting analytically pure hydrofluoric acid to the volumetric flask with pipette, be prepared into concentration of nitric acid for 8mol/L~
12mol/L, hydrofluoric acid concentration is the nitration mixture of 0.05mol/L~0.10mol/L；
(2) plutonium standard substance sampling：Using a ten thousandth balance accurately weigh plutonium dioxide standard substance put to
In high-pressure digestion tank, the nitrate acid and hydrofluoric acid nitration mixture 4mL obtained by step (1)~5mL is added into high-pressure digestion
Tank, is closed the lid, and high-pressure digestion tank is put into supporting stainless steel cylinder, and stainless steel cylinder is put to graphite cake
Heated on electric furnace；Uranium standard substance is sampled：Triuranium octoxide reference material is accurately weighed using a ten thousandth balance
Matter is put into high pressure counteracting tank, the nitrate acid and hydrofluoric acid nitration mixture 4mL obtained by step (1)~5mL is added high
Pressure counteracting tank, is closed the lid, and high-pressure digestion tank is put into supporting stainless steel cylinder, and stainless steel cylinder is put to band stone
Heated on the electric furnace of black plate；
(3) standard substance powder dissolving：Step (2) is held into the stainless steel cylinder of sample at 160~180 DEG C
Lower heating 4h~8h, opens high-pressure digestion cover, confirms the solid powder of the uranium and plutonium in high-pressure digestion tank
It is completely dissolved；
(4) prepared by uranium and plutonium standard reserving solution：Two samples of step (3) are moved to two with glue head dropper
In individual volumetric flask, with the nitric acid constant volume of 1mol/L~4mol/L, that is, the uranium and plutonium standard reserving solution of water phase are obtained；
(5) prepared by uranium, neptunium, plutonium series standard：The uranium of accurate removing step (4), the storage of plutonium standard respectively
Standby liquid and neptunium standard liquid in 6 10ml volumetric flasks, with the salpeter solution constant volume of 1mol/L~4mol/L,
Can obtain serial uranium, neptunium, plutonium mixed standard solution；
(6) series standard is measured：Respectively removing step (5) series standard solution 1.0mL~1.2mL in
In measurement bottle, 600s~1000s, the measurement of instrument are determined with the pre- diffracting X-rays fluorescence analyser of graphite crystal
Condition is:Voltage -50kV, electric current 4mA, preserve measurement spectrogram.
2. the analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample according to claim 1,
It is characterized in that：Plutonium dioxide standard substance is GBW 04201 in the step (2).
3. the analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample according to claim 1,
It is characterized in that：Triuranium octoxide standard substance is GBW 04201 in the step (2).
4. the analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample according to claim 1,
It is characterized in that：Step (2) the mesohigh counteracting tank material is polytetrafluoroethylene (PTFE).
5. the analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample according to claim 1,
It is characterized in that：Neptunium standard liquid is United Kingdom National physics laboratory in the step (5), and activity is
148.2kBq.g-1, expanded uncertainty is ± 1.6kBq.g-1Solution.
6. the analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample according to claim 1,
It is characterized in that：After described step (6), following steps are also carried out：(7) drawing curve：
Using the spectrogram of step (6) using deduction background, peak height method drawing curve；(8) add-back yield is tested again
Card：Optional step (7) working curve determines unknown aqueous process sample 6 times, by water phase uranium, neptunium, plutonium mark
Quasi- solution is separately added into the unknown process sample, prepare respectively uranium, neptunium, plutonium standard content addition it is equal
It is 10.00 × 10-6g、10.00×10-6g、10.00×10-6Three 1mL aqueous samples of g, the addition of measure
Uranium, neptunium, the average of the measurement result of the standard of plutonium are respectively 9.99 × 10-6g、10.28×10-6g、10.02×10-6G,
Then add-back yield is respectively 99.9%, 102.8%, 100.2% again.
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| CN107843640A (en) * | 2017-11-01 | 2018-03-27 | 广西壮族自治区食品药品检验所 | The assessment method of 20 kinds of constituent content uncertainties in honeysuckle |
| CN108152850A (en) * | 2017-12-18 | 2018-06-12 | 中核四0四有限公司 | Multinuclear element rapid analysis method in a kind of radioactive pollution soil |
| CN108303306A (en) * | 2017-12-21 | 2018-07-20 | 中核四0四有限公司 | Spentnuclear fuel post-processes high-content uranium, neptunium, the direct method for measuring of plutonium in feed liquid |
| CN110455843A (en) * | 2019-09-16 | 2019-11-15 | 核工业二三O研究所 | A kind of method that strontium internal standard-XRF solwution method measures uranium element in natural uranium product |
| CN110530906A (en) * | 2019-08-14 | 2019-12-03 | 中国原子能科学研究院 | The measuring method of plutonium concentration in a kind of spent fuel solution |
| CN112697777A (en) * | 2021-01-20 | 2021-04-23 | 中国核动力研究设计院 | Method for determining content of lithium, sodium, magnesium and calcium in uranium compound |
| CN112763449A (en) * | 2020-12-14 | 2021-05-07 | 中国原子能科学研究院 | Method for simultaneously determining neptunium and plutonium concentrations in nitric acid-containing solution |
| CN112924518A (en) * | 2019-12-05 | 2021-06-08 | 中核四0四有限公司 | Method for analyzing neptunium content in neptunium dioxide sample |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107449789A (en) * | 2017-07-31 | 2017-12-08 | 四川新先达测控技术有限公司 | Sample concentration detection means and system |
| CN107843640A (en) * | 2017-11-01 | 2018-03-27 | 广西壮族自治区食品药品检验所 | The assessment method of 20 kinds of constituent content uncertainties in honeysuckle |
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| CN110455843A (en) * | 2019-09-16 | 2019-11-15 | 核工业二三O研究所 | A kind of method that strontium internal standard-XRF solwution method measures uranium element in natural uranium product |
| CN110455843B (en) * | 2019-09-16 | 2022-04-05 | 核工业二三O研究所 | Method for determining uranium element in natural uranium product by strontium internal standard-XRF solution method |
| CN112924518A (en) * | 2019-12-05 | 2021-06-08 | 中核四0四有限公司 | Method for analyzing neptunium content in neptunium dioxide sample |
| CN112924518B (en) * | 2019-12-05 | 2023-02-21 | 中核四0四有限公司 | Method for analyzing neptunium content in neptunium dioxide sample |
| CN112763449A (en) * | 2020-12-14 | 2021-05-07 | 中国原子能科学研究院 | Method for simultaneously determining neptunium and plutonium concentrations in nitric acid-containing solution |
| CN112697777A (en) * | 2021-01-20 | 2021-04-23 | 中国核动力研究设计院 | Method for determining content of lithium, sodium, magnesium and calcium in uranium compound |
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