CN109581464A - In a kind of high activity liquid waste155Eu measures analysis method - Google Patents
In a kind of high activity liquid waste155Eu measures analysis method Download PDFInfo
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- CN109581464A CN109581464A CN201811611122.9A CN201811611122A CN109581464A CN 109581464 A CN109581464 A CN 109581464A CN 201811611122 A CN201811611122 A CN 201811611122A CN 109581464 A CN109581464 A CN 109581464A
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- 230000000694 effects Effects 0.000 title claims abstract description 49
- 238000004458 analytical method Methods 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 title description 2
- 239000010808 liquid waste Substances 0.000 claims abstract description 39
- 239000012071 phase Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005259 measurement Methods 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 15
- 150000003983 crown ethers Chemical class 0.000 claims abstract description 11
- 239000004698 Polyethylene Substances 0.000 claims abstract description 8
- -1 polyethylene Polymers 0.000 claims abstract description 8
- 229920000573 polyethylene Polymers 0.000 claims abstract description 8
- 239000012074 organic phase Substances 0.000 claims abstract description 7
- 230000000717 retained effect Effects 0.000 claims abstract description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000005642 Oleic acid Substances 0.000 claims abstract description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 6
- 238000012360 testing method Methods 0.000 claims abstract description 6
- 230000009514 concussion Effects 0.000 claims abstract description 5
- 238000001730 gamma-ray spectroscopy Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 235000015170 shellfish Nutrition 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000005461 Bremsstrahlung Effects 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/17—Circuit arrangements not adapted to a particular type of detector
- G01T1/178—Circuit arrangements not adapted to a particular type of detector for measuring specific activity in the presence of other radioactive substances, e.g. natural, in the air or in liquids such as rain water
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Molecular Biology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
In a kind of high activity liquid waste155Eu measures analysis method, comprising the following steps: S1: pipetting certain volume V high activity liquid waste in extraction test tube A, 4.5mol/L nitric acid solution, volume V is added0；S2: the hat of 0.3mol/L crown ether -0.05mol/L glasss-n-octyl alcohol V is added into extracting tube A0ML carries out concussion extraction according to 1:1, is centrifuged split-phase, discards organic phase, water phase is retained in extracting tube A；S3: the hat of 0.3mol/L crown ether -0.05mol/L glasss-n-octyl alcohol V is added into extracting tube A0mL；S4: water phase V in extracting tube A is pipetted1ML is to volumetric flask B, V2In, scale is diluted to 0.4mol/L nitric acid；S5: pipetting 0.4mol/L nitric acid 10.0mL in 25mL polyethylene bottle, measure on low energy high-purity oleic acid, records in t time of measuring, records 155Eu, the background count No of 105keV；S6: sample certain volume V in the volumetric flask B of S4 is pipetted3In 25mL polyethylene bottle, 0.4mol/L nitric acid 9.8mL is added, and measures sample under sample-out count the same terms, records 155Eu, the measurement count N of 105keV；S7: 155Eu activity concentration is calculated as follows in sample
Description
Technical field
Elimination of nuclear facilities Treatment process field, and in particular in a kind of high activity liquid waste155Eu measures analysis method.
Background technique
The high activity liquid waste that spentnuclear fuel reprocessing plant generates long inactivity under acid system is temporary, and there are security risks, needs
Processing disposition is carried out to high activity liquid waste.Currently, being both at home and abroad high activity liquid waste glass to the effective means of high level liquid waste processing disposition
Solidify engineering technology.The chemical constituent of high activity liquid waste, radionuclide type and level, acidity etc. can all influence glass solidified body
Research and technique design, need thus carry out high activity liquid waste analysis, understand the source item information of existing high activity liquid waste.
For in high activity liquid waste155The analysis of Eu measures, and the last century 90's is measured using high-purity oleic acid,
But due to155The half-life period of Eu is shorter, with the increase of temporary storage time,155Eu with137The activity concentration ratio of Cs increases,137The Compton peak that Cs is generated influences155The measurement of Eu, simultaneously90The bremsstrahlung effect of Y can be at high-purity oleic acid low energy end
(< 300keV) forms continuous spectral peak, also will affect in high activity liquid waste155Eu measurement.
A kind of new analysis method is found thus, is made in high activity liquid waste137Cs、90Y does not influence in high activity liquid waste155Eu's
Measurement.
Summary of the invention
It is an object of the invention to: 155Eu measurement analysis method in a kind of high activity liquid waste is provided, the invention purpose is developed and exists
When progress height puts middle 155Eu measurement, 137Cs, 90Y in high activity liquid waste do not influence its measurement.
Technical scheme is as follows: 155Eu measures analysis method in a kind of high activity liquid waste, comprising the following steps:
S1: certain volume V high activity liquid waste is pipetted in extraction test tube A, 4.5mol/L nitric acid solution, volume V is added0；
S2: the hat of 0.3mol/L crown ether -0.05mol/L glasss-n-octyl alcohol V is added into extracting tube A0ML is carried out according to 1:1
Concussion extraction, is centrifuged split-phase, discards organic phase, water phase is retained in extracting tube A；
S3: the hat of 0.3mol/L crown ether -0.05mol/L glasss-n-octyl alcohol V is added into extracting tube A0mL；
S4: water phase V in extracting tube A is pipetted1ML is to volumetric flask B, V2In, scale is diluted to 0.4mol/L nitric acid；
S5: pipetting 0.4mol/L nitric acid 10.0mL in 25mL polyethylene bottle, measure on low energy high-purity oleic acid, note
It records in t time of measuring, record155The background count No of Eu, 105keV；
S6: sample certain volume V in the volumetric flask B of S4 is pipetted3In 25mL polyethylene bottle, 0.4mol/L nitric acid is added
Sample is measured under 9.8mL, with sample-out count the same terms, is recorded155The measurement count N of Eu, 105keV；
S7: in sample155Eu activity concentration is calculated as follows
In the S1, test tube A is shaken up.
In the S2, concussion 3~5min of extraction is centrifuged 2~3min.
In the S3, repeats to extract once, be centrifuged split-phase, discard organic phase, water phase is retained in extracting tube A.
In the S3, if in sample90Sr、137Cs with155Eu increases this extraction times compared to too high.
It in the S4, shakes up, is sealed no less than 15 days with sealed membrane.
In the S7, in formula:
C --- in high setting-out product155Eu activity concentration, shellfish grams per milliliter Bq/mL；
N --- in the t time155The sample measurement count of Eu (105keV)；
No --- in the t time155The sample-out count of Eu (105keV) counts；
T --- γ spectrometry time, second s；
η——155Eu (105keV) γ spectrum efficiency；
Y——155γ emission probability of the Eu at 105keV energy, 21.12%；
Sample volume when V3 --- sample measures, milliliter mL；
V2 --- volumetric flask B volume, milliliter mL；
V1 --- water phase pipettes volume, milliliter mL；
Water phase total volume in Vo --- step 1, milliliter mL；
V --- high activity liquid waste sample volume, milliliter mL.
Remarkable result of the invention is:
Hat-the n-octyl alcohol of 0.3mol/L crown ether -0.05mol/L glasss does not extract in high activity liquid waste155Eu does not influence raffinate water
Xiang Zhong155The measurement of Eu；
In the hat of 0.3mol/L crown ether -0.05mol/L glasss-Extraction with n-Octanol high activity liquid waste90Sr、137Cs does it not
It disturbs in high activity liquid waste155The measurement of Eu, while the radioactive intensity of high activity liquid waste is reduced, reduce being shone for back-end analysis personnel
Dosage is conducive to the radiation protection of personnel；
Hat-the n-octyl alcohol of 0.3mol/L crown ether -0.05mol/L glasss is to iron, aluminium, magnesium, nickel, neodymium, the europium etc. in high activity liquid waste
It does not extract, raffinate water phase can be used for other elements analysis, reduce manpower and material resources.
Using in crown ether-cup crown- Extraction with n-Octanol high activity liquid waste90Sr、137Cs is efficiently solved in high activity liquid waste155Eu
When measurement137Cs、90Y interference, also reduces the radioactive intensity of high activity liquid waste, reduces the radioactive dose of back-end analysis personnel,
Be conducive to the radiation protection of personnel；Raffinate water phase can also be used in the analysis of iron, aluminium, magnesium, nickel, rare earth, reduce manpower and material resources
Specific embodiment
In a kind of high activity liquid waste155Eu measures analysis method, comprising the following steps:
S1: certain volume V high activity liquid waste is pipetted in extraction test tube A, 4.5mol/L nitric acid solution, volume V is added0,
It shakes up；
S2: the hat of 0.3mol/L crown ether -0.05mol/L glasss-n-octyl alcohol V0mL is added into extracting tube A, is carried out according to 1:1
Concussion 3~5min of extraction, is centrifuged 2~3min split-phase, discards organic phase, water phase is retained in extracting tube A；
S3: adding the hat of 0.3mol/L crown ether -0.05mol/L glasss-n-octyl alcohol V0mL into extracting tube A, repeats to extract
Once, it is centrifuged split-phase, discards organic phase, water phase is retained in extracting tube A.If (90Sr in sample,137Cs with155Eu is compared to too
Height can increase this extraction times)
S4: water phase V1mL is pipetted in extracting tube A to volumetric flask B, V2In, it is diluted to scale with 0.4mol/L nitric acid, is shaken up,
It is sealed no less than 15 days with sealed membrane.
S5: pipetting 0.4mol/L nitric acid 10.0mL in 25mL polyethylene bottle, measure on low energy high-purity oleic acid, note
It records in t time of measuring, record155The background count No of Eu, 105keV；
S6: sample certain volume V in the volumetric flask B of removing step 43In 25mL polyethylene bottle, 0.4mol/L nitre is added
Sample is measured under sour 9.8mL, with sample-out count the same terms, records the measurement count N of 155Eu (105keV).
S7: 155Eu activity concentration is calculated as follows in sample
In formula:
C --- in high setting-out product155Eu activity concentration, shellfish grams per milliliter (Bq/mL)；
N --- in the t time155The sample measurement count of Eu (105keV)；
No --- in the t time155The sample-out count of Eu (105keV) counts；
T --- γ spectrometry time, second s；
η——155Eu (105keV) γ spectrum efficiency；
Y——155γ emission probability of the Eu at 105keV energy, 21.12%；
Sample volume when V3 --- sample measures, milliliter mL；
V2 --- volumetric flask B volume, milliliter mL；
V1 --- water phase pipettes volume, milliliter mL；
Water phase total volume in Vo --- step 1, milliliter mL；
V --- high activity liquid waste sample volume, milliliter mL.
Claims (7)
1. 155Eu measures analysis method in a kind of high activity liquid waste, it is characterised in that: the following steps are included:
S1: certain volume V high activity liquid waste is pipetted in extraction test tube A, 4.5mol/L nitric acid solution, volume V is added0；
S2: the hat of 0.3mol/L crown ether -0.05mol/L glasss-n-octyl alcohol V is added into extracting tube A0ML is shaken according to 1:1
Extraction is centrifuged split-phase, discards organic phase, water phase is retained in extracting tube A；
S3: the hat of 0.3mol/L crown ether -0.05mol/L glasss-n-octyl alcohol V is added into extracting tube A0mL；
S4: water phase V in extracting tube A is pipetted1ML is to volumetric flask B, V2In, scale is diluted to 0.4mol/L nitric acid；
S5: pipetting 0.4mol/L nitric acid 10.0mL in 25mL polyethylene bottle, measure on low energy high-purity oleic acid, records t
In time of measuring, record155The background count No of Eu, 105keV；
S6: sample certain volume V in the volumetric flask B of S4 is pipetted3In 25mL polyethylene bottle, 0.4mol/L nitric acid 9.8mL is added,
Sample is measured under sample-out count the same terms, is recorded155The measurement count N of Eu, 105keV；
S7: in sample155Eu activity concentration is calculated as follows
2. in a kind of high activity liquid waste according to claim 1155Eu measures analysis method, it is characterised in that: in the S1,
Test tube A is shaken up.
3. in a kind of high activity liquid waste according to claim 1155Eu measures analysis method, it is characterised in that: in the S2,
Concussion 3~5min of extraction, is centrifuged 2~3min.
4. in a kind of high activity liquid waste according to claim 1155Eu measures analysis method, it is characterised in that: in the S3,
It repeats to extract once, is centrifuged split-phase, discards organic phase, water phase is retained in extracting tube A.
5. in a kind of high activity liquid waste according to claim 4155Eu measures analysis method, it is characterised in that: in the S3,
If in sample90Sr、137Cs with155Eu increases this extraction times compared to too high.
6. in a kind of high activity liquid waste according to claim 1155Eu measures analysis method, it is characterised in that: in the S4,
It shakes up, is sealed no less than 15 days with sealed membrane.
7. in a kind of high activity liquid waste according to claim 1155Eu measures analysis method, it is characterised in that: in the S7,
In formula:
C --- in high setting-out product155Eu activity concentration, shellfish grams per milliliter Bq/mL；
N --- in the t time155The sample measurement count of Eu (105keV)；
No --- in the t time155The sample-out count of Eu (105keV) counts；
T --- γ spectrometry time, second s；
η——155Eu (105keV) γ spectrum efficiency；
Y——155γ emission probability of the Eu at 105keV energy, 21.12%；
Sample volume when V3 --- sample measures, milliliter mL；
V2 --- volumetric flask B volume, milliliter mL；
V1 --- water phase pipettes volume, milliliter mL；
Water phase total volume in Vo --- step 1, milliliter mL；
V --- high activity liquid waste sample volume, milliliter mL.
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Cited By (1)
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| CN114689617A (en) * | 2020-12-25 | 2022-07-01 | 中核四0四有限公司 | Method for measuring gamma energy emissivity of fission product in neptunium dioxide sample |
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Application publication date: 20190405 |