CN117741092A - Analysis method for nitrogen content in neptunium dioxide sample - Google Patents
Analysis method for nitrogen content in neptunium dioxide sample Download PDFInfo
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- CN117741092A CN117741092A CN202311546952.9A CN202311546952A CN117741092A CN 117741092 A CN117741092 A CN 117741092A CN 202311546952 A CN202311546952 A CN 202311546952A CN 117741092 A CN117741092 A CN 117741092A
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- nitrogen
- nitrogen content
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000004458 analytical method Methods 0.000 title claims abstract description 41
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 33
- QKUTVYUEUPNRBO-UHFFFAOYSA-N [O--].[O--].[Np+4] Chemical compound [O--].[O--].[Np+4] QKUTVYUEUPNRBO-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910000478 neptunium(IV) oxide Inorganic materials 0.000 title claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000005259 measurement Methods 0.000 claims abstract description 22
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 21
- 239000010959 steel Substances 0.000 claims abstract description 21
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000012937 correction Methods 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000012360 testing method Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000004164 analytical calibration Methods 0.000 claims description 3
- 238000007872 degassing Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000003758 nuclear fuel Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 239000002585 base Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 239000011824 nuclear material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention relates to the technical field of nuclear fuel analysis, in particular to a method for analyzing the nitrogen content in a neptunium dioxide sample. The method comprises the following steps: (1) Preparing an instrument, namely preheating the instrument by using an oxygen-nitrogen analyzer; (2) an empty load instrument; (3) The instrument correction is carried out by adopting a standard steel sample with the absolute nitrogen content similar to that of the neptunium dioxide sample to be detected; (4) The result measurement, namely placing a neptunium dioxide sample to be measured into a nickel bag, removing air, and measuring; and (5) data processing. The analysis method provided by the invention adopts a pulse heating melting-thermal conductivity method to measure, each sample is analyzed for only 5 minutes, no acid or alkali is used in the sample analysis process, the cost of reagent consumable materials is saved, the analysis dosage of the sample is small, the time of human body irradiation of an analyst is reduced, and the rapid and accurate analysis of the nitrogen content in the neptunium dioxide powder sample is realized.
Description
Technical Field
The invention relates to the technical field of nuclear fuel analysis, in particular to a method for analyzing the nitrogen content in a neptunium dioxide sample.
Background
According to the requirements of 'technical conditions for post-processing neptunium dioxide powder', the nitrogen content is used as one of the judging indexes of whether the neptunium dioxide product is qualified or not, and is determined by an accurate and reliable analysis method. At present, a laboratory adopts a distillation-Neschler reagent spectrophotometry method to measure the nitrogen content in a neptunium dioxide sample, and the method has the following defects: (1) The glass distillation device is used, the conditions of crushing and wearing can be generated in the installation and use processes, and the reagent consumable cost is high; (2) The analysis time is long, each sample takes about 45 minutes to analyze, and the human body of an analysis person is irradiated by radiation for a long time; (3) The concentrated acid and the concentrated alkali are used in the sample analysis and detection, so that the glove box is severely corroded; (4) The consumption of nuclear material is large, and the sampling amount of the sample is 50 mg-100 mg. Accordingly, the present invention has been made to provide a novel method for analyzing the nitrogen content of neptunium dioxide samples to solve the above-mentioned problems.
Disclosure of Invention
The invention aims to provide an analysis method for the nitrogen content in a neptunium dioxide sample, which does not need a glass distillation device, is short in sample analysis time consumption, does not use acid or alkali in the sample analysis process, reduces the corrosion phenomenon of a glove box, can reduce experiment cost, and reduces the irradiation time of the human body of an analyst.
The invention provides an analysis method of nitrogen content in neptunium dioxide samples, which comprises the following steps:
(1) Instrument preparation
Using an oxygen-nitrogen analyzer to perform, regulating the pressure of nitrogen and helium, and preheating the instrument;
(2) Empty load instrument
Carrying out no-load analysis test on the oxygen-nitrogen analyzer to determine that the analyzer is normal;
(3) Instrument calibration
Weighing a standard steel sample with the absolute nitrogen content similar to that of a neptunium dioxide sample to be detected, putting the standard steel sample into an instrument sample injection chamber, inputting the mass of the standard steel sample on an analysis interface of an oxygen-nitrogen analyzer software, carrying out analysis test, repeating for a plurality of times, correcting a standard value of the standard steel sample through a plurality of measurement results, and carrying out standard steel sample measurement for at least 2 times after correction, so that a measured value is within a standard value required error range, and finishing instrument correction;
(4) Results measurement
Placing a neptunium dioxide sample to be detected into a nickel bag, exhausting air in the nickel bag, then putting the nickel bag wrapped with the sample into a sample injector, and clicking to start measurement;
(5) Data processing
The results are automatically given in ppm or after the instrument measurement is completed, and the results remain integers.
Preferably, in the step (1), the nitrogen pressure is regulated to be 0.4 Mpa-0.6 Mpa, and the helium pressure is regulated to be 0.2 Mpa-0.4 Mpa.
Preferably, in the step (1), the instrument is ventilated and preheated for 30-60 min.
Preferably, after the instrument in the step (1) is preheated, the degassing power of the oxygen and nitrogen analyzer is set to be 4KW, and the analysis power is set to be 3.5KW.
Preferably, the specific process of the step (2) is as follows: the method comprises the steps of manually inputting 20 mg-100 mg of sample mass on an analysis interface of an oxygen-nitrogen analyzer, placing a new graphite crucible on a graphite crucible base, carrying out no-load analysis test, repeating for 2-4 times until the measurement result of a nitrogen channel is 0.00ppm, and determining that the instrument is normal.
Preferably, in the step (3), 500mg or 1000mg of solid particle standard steel sample with the absolute nitrogen content similar to that of the neptunium dioxide sample to be measured is weighed and put into an instrument sample injection chamber.
Preferably, the test is repeated 2 to 5 times when the standard steel sample is adopted for correction in the step (3).
Preferably, the neptunium dioxide sample to be detected is in the form of powder, and the particle size is not more than 200 μm.
In summary, compared with the prior art, the technical scheme provided by the invention has the following advantages:
according to the invention, the nitrogen content in the neptunium dioxide powder sample is measured by using a nitrogen oxidation analyzer by adopting a pulse heating melting-thermal conductivity method, the analysis time of each sample is only 5 minutes, compared with a distillation-Neschler reagent spectrophotometry method, the sample analysis time is greatly shortened, no acid or alkali is used in the analysis process, the cost of reagent consumables is saved, and the corrosion phenomenon of a glove box is reduced; the sampling amount is reduced from 50mg to 100mg to 30mg to 50mg, so that the experimental cost is reduced, the analysis amount of the sample and the irradiation time of a human body are reduced, and the rapid and accurate analysis of the nitrogen content in the neptunium dioxide powder sample is realized.
The analysis method provided by the invention is suitable for analyzing the nitrogen content in the neptunium dioxide powder sample, the precision is better than 5.0%, and the measurement is accurate and reliable.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular forms also include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
The analysis method of the nitrogen content in the neptunium dioxide sample comprises the following specific processes:
(1) Instrument preparation
The method is carried out by using a nitrogen-oxygen analyzer (model is ON 900), the pressure of nitrogen is regulated to be 0.4 Mpa-0.6 Mpa, the pressure of helium is regulated to be 0.2 Mpa-0.4 Mpa, ventilation and preheating of the instrument are carried out for 30 min-60 min, the degassing power of the oxygen-nitrogen analyzer is set to be 4KW, and the analysis power is set to be 3.5KW.
(2) Empty load instrument
The method comprises the steps of manually inputting 20 mg-100 mg of sample mass on a software analysis interface of an oxygen-nitrogen analyzer, placing a new graphite crucible on a graphite crucible base, carrying out no-load analysis test, repeating for 2-4 times until the measurement result of a nitrogen channel is 0.00ppm, and determining that the instrument is normal.
(3) Instrument calibration
Weighing 500mg or 1000mg of solid particle standard steel sample with the absolute nitrogen content similar to that of neptunium dioxide powder sample with the particle size not more than 200 mu m, putting the solid particle standard steel sample into an instrument sample injection chamber, inputting the mass of the standard steel sample on an oxygen nitrogen analyzer software analysis interface, putting a new graphite crucible on a graphite crucible base, carrying out analysis test, repeating the analysis test for 2-5 times, correcting the standard value of the solid particle standard steel sample through a plurality of measurement results, and carrying out solid particle standard steel sample measurement for not less than 2 times after the correction, so that the measured value is within the standard value requirement error range, completing the instrument correction, otherwise, continuing the correction according to the steps until the measured value of the solid particle standard steel sample is within the requirement error range.
(4) Results measurement
Weighing 30-50 mg of neptunium dioxide powder in a nickel bag, exhausting air in the nickel bag as much as possible by using tools such as lead sealing pliers, tweezers and the like, so that the volume of the nickel bag is minimized as much as possible, a sample is not sprayed out of the nickel bag, the nickel bag wrapped with the sample is put into a sample injector, a new graphite crucible is placed on a graphite crucible base, and measurement is started by clicking.
(5) Data processing
The results are automatically given in ppm or after the instrument measurement is completed, and the results remain integers.
(6) Precision of
Under the repetitive condition, the relative standard deviation of the nitrogen content in the neptunium dioxide powder sample is superior to 5.0% for six times.
The analysis method provided by the invention is suitable for analyzing the nitrogen content in the neptunium dioxide powder sample, has the precision better than 5.0%, and has the advantages of accurate and reliable measurement, less sampling amount, short measurement time and strong practicability.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (8)
1. A method for analyzing the nitrogen content of a neptunium dioxide sample, comprising the steps of:
(1) Instrument preparation
Using an oxygen-nitrogen analyzer to perform, regulating the pressure of nitrogen and helium, and preheating the instrument;
(2) Empty load instrument
Carrying out no-load analysis test on the oxygen-nitrogen analyzer to determine that the analyzer is normal;
(3) Instrument calibration
Weighing a standard steel sample with the absolute nitrogen content similar to that of a neptunium dioxide sample to be detected, putting the standard steel sample into an instrument sample injection chamber, inputting the mass of the standard steel sample on an analysis interface of an oxygen-nitrogen analyzer software, carrying out analysis test, repeating for a plurality of times, correcting a standard value of the standard steel sample through a plurality of measurement results, and carrying out standard steel sample measurement for at least 2 times after correction, so that a measured value is within a standard value required error range, and finishing instrument correction;
(4) Results measurement
Placing a neptunium dioxide sample to be detected into a nickel bag, exhausting air in the nickel bag, then putting the nickel bag wrapped with the sample into a sample injector, and clicking to start measurement;
(5) Data processing
The results are automatically given in ppm or after the instrument measurement is completed, and the results remain integers.
2. The method according to claim 1, wherein the nitrogen pressure is adjusted to 0.4Mpa to 0.6Mpa and the helium pressure is adjusted to 0.2Mpa to 0.4Mpa in the step (1).
3. The method according to claim 2, wherein the instrument is aerated and preheated in step (1) for 30 to 60 minutes.
4. The method according to claim 3, wherein the oxygen nitrogen analyzer is set to have a degassing power of 4KW and an analyzing power of 3.5KW after the instrument is preheated in the step (1).
5. The method according to claim 1, wherein the specific process of step (2) is as follows: the method comprises the steps of manually inputting 20 mg-100 mg of sample mass on an analysis interface of an oxygen-nitrogen analyzer, placing a new graphite crucible on a graphite crucible base, carrying out no-load analysis test, repeating for 2-4 times until the measurement result of a nitrogen channel is 0.00ppm, and determining that the instrument is normal.
6. An analysis method according to claim 1, wherein in step (3), 500mg or 1000mg of solid particulate standard steel sample having an absolute nitrogen content similar to that of the neptunium dioxide sample to be measured is weighed and introduced into the instrument sample chamber.
7. The method according to claim 1, wherein the test is repeated 2 to 5 times when the calibration is performed using the standard steel sample in the step (3).
8. An analysis method according to claim 1, characterized in that the neptunium dioxide sample to be tested is in powder form, with a particle size not greater than 200 μm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311546952.9A CN117741092A (en) | 2023-11-20 | 2023-11-20 | Analysis method for nitrogen content in neptunium dioxide sample |
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| CN202311546952.9A CN117741092A (en) | 2023-11-20 | 2023-11-20 | Analysis method for nitrogen content in neptunium dioxide sample |
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