CN116735695A - Method for measuring quality of high-temperature molten salt - Google Patents
Method for measuring quality of high-temperature molten salt Download PDFInfo
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- CN116735695A CN116735695A CN202310691550.1A CN202310691550A CN116735695A CN 116735695 A CN116735695 A CN 116735695A CN 202310691550 A CN202310691550 A CN 202310691550A CN 116735695 A CN116735695 A CN 116735695A
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- 150000003839 salts Chemical class 0.000 title claims abstract description 207
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims abstract description 8
- 239000000700 radioactive tracer Substances 0.000 claims abstract description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 16
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 14
- RPFLLVICGMTMIE-UHFFFAOYSA-L calcium;sodium;dichloride Chemical group [Na+].[Cl-].[Cl-].[Ca+2] RPFLLVICGMTMIE-UHFFFAOYSA-L 0.000 claims description 12
- 239000001103 potassium chloride Substances 0.000 claims description 12
- 235000011164 potassium chloride Nutrition 0.000 claims description 12
- 238000005070 sampling Methods 0.000 claims description 12
- 235000013619 trace mineral Nutrition 0.000 claims description 12
- 239000011573 trace mineral Substances 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010935 stainless steel Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 238000005336 cracking Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000012625 in-situ measurement Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 230000001788 irregular Effects 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 9
- OYEHPCDNVJXUIW-FTXFMUIASA-N 239Pu Chemical compound [239Pu] OYEHPCDNVJXUIW-FTXFMUIASA-N 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 229910052778 Plutonium Inorganic materials 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000003758 nuclear fuel Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C17/00—Monitoring; Testing ; Maintaining
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
- G01N2001/388—Other diluting or mixing processes mixing the sample with a tracer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- General Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- High Energy & Nuclear Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring the quality of high-temperature molten salt, which comprises the steps of continuously and cumulatively adding the same molten salt with a certain known quality into molten salt bottom salt as an element tracer, and monitoring the concentration of the element tracer added into the molten salt bottom salt each time through ICP-MS. And calculating the total mass of the bottom salt of the initial molten salt by calculating the ratio of the mass of the added element tracker to the measured concentration. The invention has the advantages that: firstly, an element tracking method is originally provided for measuring the total mass of high-temperature molten salt; the measuring method can measure the quality of the high-temperature molten salt in extremely severe environments, such as the molten salt quality in high-radiation environments; thirdly, the measuring method can be used for measuring the quality of the high-temperature molten salt with unknown density in the irregular container.
Description
Technical Field
The invention belongs to the field of high-temperature molten salt quality measurement, and particularly relates to a method for measuring the high-temperature molten salt quality of unknown density in an irregular container by an element tracking dilution method.
Background
Molten salt reactors are one of the most recently international reactors at present, in which molten salt is used as a liquid fuel in the molten salt reactor, both as a nuclear fuel in the reactor and as a coolant for the molten salt reactor. Actinide-containing molten salt fuels require a higher level of safety protection compared to traditional solid fuels. Because the plutonium-239 in the molten salt reactor can be used directly or concentrated to convert into a nuclear weapon raw material. Therefore, it is necessary to detect the quality of plutonium-239 in molten salt reactors. Since molten salt in a molten salt reactor acts as a carrier for fissionable materials, the mass measurement of plutonium-239 in a molten salt reactor can be divided into a measurement of the concentration of plutonium and a measurement of the total mass in the molten salt reactor.
Currently, there are many methods for measuring the concentration of plutonium in molten salt reactors, including Laser Induced Breakdown Spectroscopy (LIBS), electrochemical analysis methods, and inductively coupled plasma mass spectrometry (ICP-MS), among others. But the measurement of the total mass of molten salt in a molten salt reactor is difficult.
In general, the mass of the molten salt can be determined by liquid level measurement and molten salt density measurement or computational synthesis, but for high temperature molten salt reactors, liquid level measurement is not effected while the molten salt flows through tortuous piping and heat exchangers. Meanwhile, in a molten salt reactor, it is also difficult to assign a single density to the molten salt in the molten salt reactor due to the difference in temperature around the high-temperature molten salt and the variability caused by nuclear fuel fission. In summary, measurement of molten salt mass in molten salt reactors is of less concern and challenging.
Disclosure of Invention
The invention provides a method for measuring the quality of high-temperature molten salt in an irregular container, aiming at the difficulty in measuring the quality of the high-temperature molten salt in the existing high-temperature molten salt reactor. The invention can be used for effectively measuring the quality of the high-temperature molten salt with unknown density in the irregular container.
In order to achieve the above purpose, the invention provides a high-temperature molten salt quality measurement method, which comprises the following steps:
A. obtaining experimental data
Taking appointed molten salt as an element tracking agent, and selecting a part of molten salt bottom salt with mass to be detected as a bottom salt sample, wherein the appointed molten salt contains elements which are not contained in the molten salt bottom salt with mass to be detected;
weighing and mixing the appointed molten salt and the bottom salt sample according to a certain proportion;
adding the mixture into an alumina crucible, and heating to a molten state, which is called a molten salt system 1;
inserting a stainless steel full-threaded rod into the molten salt system 1 in the molten state, and rapidly sampling, wherein the collected molten salt sample is called as a molten salt sample 1;
cooling the molten salt system 1 to room temperature;
weighing the designated molten salt again, adding the molten salt into the molten salt system 1 cooled to room temperature, and mixing and heating to a molten state, namely a molten salt system 2;
inserting a stainless steel full-threaded rod into the molten salt system 2 in the molten state, and rapidly sampling, wherein the collected molten salt sample is called as a molten salt sample 2;
cooling the molten salt system 2 to room temperature;
repeatedly adding appointed molten salt into a cooled molten salt system n, heating the molten salt system n to a molten state, namely a molten salt system n+1, rapidly sampling by using a stainless steel full-threaded rod, marking the molten salt as a molten salt sample n+1, and cooling the molten salt system to room temperature, wherein n is an integer greater than or equal to 2;
detecting the concentration of trace elements from the collected molten salt sample 1 to the molten salt sample n+1, calculating the mass of the bottom salt sample when mixing is started according to the detected concentration of the trace elements and the mass of the trace elements actually added, comparing the calculated mass of the bottom salt sample with the mass of the bottom salt sample weighed at the moment, calculating a mass error, and obtaining the concentration of the corresponding trace elements when the mass error is a set value, wherein the concentration is marked as a reference value;
according to the obtained data of the molten salt samples 1 to n+1, obtaining the functional relation among the mass of the added element tracker, the detected concentration and the mass of the bottom salt;
B. in-situ measurement of high temperature molten salt mass
Adding specified molten salt with known mass into molten salt bottom salt with to-be-detected mass in a divided manner, fully stirring after adding the specified molten salt each time, and sampling and detecting the actual concentration of trace elements in the molten salt bottom salt; stopping adding the specified molten salt when the actual concentration is greater than or equal to the reference value, and recording the total mass of the specified molten salt added until the moment; and calculating to obtain the mass of the bottom salt of the molten salt to be detected according to the actual concentration of the trace element, the total mass of the specified molten salt and the functional relation.
Preferably, in step a, when the added molten salt element tracer reaches the concentration of the reference value, the steps of adding the element tracer, heating, sampling, and cooling are stopped to repeat.
Preferably, the specified molten salt comprises one of potassium chloride and cerium chloride, and the molten salt bottom salt is sodium chloride-calcium chloride.
Preferably, the molten salt purity: the potassium chloride is more than or equal to 99.0 percent, the cerium chloride is more than or equal to 99.9 percent, the sodium chloride is more than or equal to 99.99 percent, and the calcium chloride is more than or equal to 99.99 percent.
Preferably, the alumina crucible containing the specified molten salt and molten salt bottom salt is a Advalue Technology company 100-ml alumina crucible, model: AL-2100A 250-ml alumina crucible was additionally used to hold a 100-ml alumina crucible to prevent high temperature molten salt from flowing out after cracking.
Preferably, all the experimental procedures are carried out in a glove box filled with argon shielding gas, while H is in the glove box 2 Concentration of O and O 2 The concentration is less than 1ppm.
Preferably, the molten salt system heating process parameters are as follows: the temperature was 650℃and the heating rate was 100℃per hour.
Preferably, after the molten salt system is heated to 650 ℃, it is maintained at a set temperature of 650 ℃ for 3 hours, and the molten salt system in a molten state is stirred for 3 minutes using a tungsten rod to ensure uniformity of the molten salt system.
Preferably, the stainless steel full-threaded rod is 316SS rod.
Preferably, the molten salt sample is collected in an amount of 50mg each time, and separately collected and stored in a clean glass bottle for sealing and preservation, and when concentration detection is performed, the whole molten salt sample is dissolved in 2vol% nitric acid, and then ICP-MS element detection is performed.
The method for measuring the quality of the high-temperature molten salt is characterized in that the same molten salt with a certain known quality is continuously and cumulatively added into the molten salt bottom salt to serve as an element tracking agent, and concentration monitoring is carried out on the element tracking agent added into the molten salt bottom salt each time through ICP-MS. And calculating the total mass of the bottom salt of the initial molten salt by calculating the ratio of the mass of the added element tracker to the measured concentration. In the measuring process of the quality of the high-temperature molten salt, the invention is not influenced by the extreme environment of high-temperature radiation, and can also carry out more accurate quality measurement on the molten salt with unknown density and the molten salt mixture in an irregular container.
Drawings
FIG. 1 is a schematic diagram of a part of the flow chart in a method for measuring the quality of high-temperature molten salt;
FIG. 2 is a comparison of ICP-MS detection results of cerium element in sodium chloride-calcium chloride molten salt in example 1 with theoretical calculation results;
FIG. 3 is a comparison of the ICP-MS test results of elemental potassium in the sodium chloride-calcium chloride molten salt in example 2 with theoretical calculation results.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting thereof.
Example 1
And taking cerium chloride as a designated molten salt, taking element cerium as an element tracking agent, and taking sodium chloride-calcium chloride as molten salt bottom salt to measure the quality of the molten salt. Cerium chloride is added into 84.7g of sodium chloride-calcium chloride molten salt bottom salt for 11 times as an element tracking agent, the sodium chloride-calcium chloride molten salt bottom salt and the element tracking agent cerium chloride are uniformly mixed, the mixture is placed into a 100-ml aluminum oxide crucible, the mixture is heated in a muffle furnace, a stainless steel full-threaded rod is used for batch sampling, and all experimental processes are carried out in a glove box. Wherein, 2.14g cerium chloride is added in total, the molten salt system is heated to 650 ℃, and the heating rate is 100 ℃/h.
Table 1 shows the mass of cerium chloride added each time and the cumulative total mass of cerium chloride added and the percentage of cerium chloride in the molten salt system. It was calculated that when the concentration of cerium chloride was more than 1.1wt%, the error rate of measuring the mass of sodium chloride-calcium chloride molten salt using potassium chloride as an element tracker was 2.39%.
TABLE 1
Example 2
And taking potassium chloride as a designated molten salt, taking element potassium as an element tracking agent, and taking sodium chloride-calcium chloride as molten salt bottom salt to measure the quality of the molten salt. Adding potassium chloride into 38.5g of sodium chloride-calcium chloride molten salt bottom salt for 10 times as an element tracking agent, uniformly mixing the sodium chloride-calcium chloride molten salt bottom salt with the element tracking agent potassium chloride, placing the mixture into a 100-ml aluminum oxide crucible, heating the mixture in a muffle furnace, sampling the mixture in batches by using a stainless steel full-threaded rod, and carrying out all experimental processes in a glove box. Wherein, 1.06g of potassium chloride is added in total, the molten salt system is heated to 650 ℃, and the heating rate is 100 ℃/h.
Table 2 shows the mass of each addition of potassium chloride and the cumulative total of the mass of cerium chloride added and the percentage of cerium chloride in the molten salt system. It was calculated that when the concentration of potassium chloride was greater than 1.1wt%, the error rate of measuring the mass of sodium chloride-calcium chloride molten salt using potassium chloride as an element tracker was 1.82%.
TABLE 2
| Sample name | Adding CeCl 3 Quality (g) | Cumulative addition of CeCl 3 Quality (g) | CeCl 3 Concentration (wt%) |
| NCK-001 | +0.1028 | 0.1028 | 0.267％ |
| NCK-002 | +0.0990 | 0.2018 | 0.522％ |
| NCK-003 | +0.1088 | 0.3106 | 0.801％ |
| NCK-004 | +0.1012 | 0.4118 | 1.059％ |
| NCK-005 | +0.1063 | 0.5181 | 1.329％ |
| NCK-006 | +0.1077 | 0.6258 | 1.601％ |
| NCK-007 | +0.0854 | 0.7112 | 1.816％ |
| NCK-008 | +0.1123 | 0.8235 | 2.096％ |
| NCK-009 | +0.0930 | 0.9165 | 2.328％ |
| NCK-010 | +0.1455 | 1.0620 | 2.687％ |
Claims (10)
1. The method for measuring the quality of the high-temperature molten salt is characterized by comprising the following steps of:
A. obtaining experimental data
Taking appointed molten salt as an element tracking agent, and selecting a part of molten salt bottom salt with mass to be detected as a bottom salt sample, wherein the appointed molten salt contains elements which are not contained in the molten salt bottom salt with mass to be detected;
weighing and mixing the appointed molten salt and the bottom salt sample according to a certain proportion;
adding the mixture into an alumina crucible, and heating to a molten state, which is called a molten salt system 1;
inserting a stainless steel full-threaded rod into the molten salt system 1 in the molten state, and rapidly sampling, wherein the collected molten salt sample is called as a molten salt sample 1;
cooling the molten salt system 1 to room temperature;
weighing the designated molten salt again, adding the molten salt into the molten salt system 1 cooled to room temperature, and mixing and heating to a molten state, namely a molten salt system 2;
inserting a stainless steel full-threaded rod into the molten salt system 2 in the molten state, and rapidly sampling, wherein the collected molten salt sample is called as a molten salt sample 2;
cooling the molten salt system 2 to room temperature;
repeatedly adding appointed molten salt into a cooled molten salt system n, heating the molten salt system n to a molten state, namely a molten salt system n+1, rapidly sampling by using a stainless steel full-threaded rod, marking the molten salt as a molten salt sample n+1, and cooling the molten salt system to room temperature, wherein n is an integer greater than or equal to 2;
detecting the concentration of trace elements from the collected molten salt sample 1 to the molten salt sample n+1, calculating the mass of the bottom salt sample when mixing is started according to the detected concentration of the trace elements and the mass of the trace elements actually added, comparing the calculated mass of the bottom salt sample with the mass of the bottom salt sample weighed at the moment, calculating a mass error, and obtaining the concentration of the corresponding trace elements when the mass error is a set value, wherein the concentration is marked as a reference value;
according to the obtained data of the molten salt samples 1 to n+1, obtaining the functional relation among the mass of the added element tracker, the detected concentration and the mass of the bottom salt;
B. in-situ measurement of high temperature molten salt mass
Adding specified molten salt with known mass into molten salt bottom salt with to-be-detected mass in a divided manner, fully stirring after adding the specified molten salt each time, and sampling and detecting the actual concentration of trace elements in the molten salt bottom salt; stopping adding the specified molten salt when the actual concentration is greater than or equal to the reference value, and recording the total mass of the specified molten salt added until the moment; and calculating to obtain the mass of the bottom salt of the molten salt to be detected according to the actual concentration of the trace element, the total mass of the specified molten salt and the functional relation.
2. The method according to claim 1, wherein in step a, when the added molten salt element tracer reaches the concentration of the reference value, the steps of adding the element tracer, heating, sampling, and cooling are stopped to be repeated.
3. The method of claim 1 wherein the specified molten salt comprises one of potassium chloride and cerium chloride and the molten salt bottom salt is sodium chloride-calcium chloride.
4. A method according to claim 3, wherein the molten salt purity: the potassium chloride is more than or equal to 99.0 percent, the cerium chloride is more than or equal to 99.9 percent, the sodium chloride is more than or equal to 99.99 percent, and the calcium chloride is more than or equal to 99.99 percent.
5. The method of claim 1, wherein the alumina crucible containing the specified molten salt and the molten salt bottom salt is a Advalue Technology company 100-ml alumina crucible, model: AL-2100A 250-ml alumina crucible was additionally used to hold a 100-ml alumina crucible to prevent high temperature molten salt from flowing out after cracking.
6. The method according to claim 1, wherein all the experimental procedures are carried out in a glove box filled with an argon shielding gas, while H is contained in the glove box 2 Concentration of O and O 2 The concentration is less than 1ppm.
7. The method of claim 1 wherein the molten salt system heating process parameters are as follows: the temperature was 650℃and the heating rate was 100℃per hour.
8. The method of claim 7 wherein the molten salt system is maintained at a set temperature of 650 ℃ for 3 hours after heating to 650 ℃ and stirring the molten salt system in the molten state using a tungsten rod for 3 minutes to ensure homogeneity of the molten salt system.
9. The method of claim 1, wherein the stainless steel full threaded rod is 316SS rod.
10. The method according to claim 1, wherein the molten salt sample is collected in an amount of 50mg each time, and separately collected and stored in a clean glass bottle for sealing and preservation, and when the concentration detection is performed, the whole molten salt sample is dissolved in 2vol% nitric acid, and then the ICP-MS element detection is performed.
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| CN202310691550.1A CN116735695A (en) | 2023-06-12 | 2023-06-12 | Method for measuring quality of high-temperature molten salt |
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