CN112881239B - Method for determining tritium diffusion coefficient based on accumulated release share - Google Patents
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- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
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- G—PHYSICS
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Abstract
The invention provides a method for determining a tritium diffusion coefficient based on accumulated released share, wherein an experimental system comprises a gas carrying device, a heating furnace, a heating and catalytic oxidation device, a cooling device, a sampling device, a liquid scintillation meter and a tail gas recovery device; according to the method for determining the diffusion coefficient of tritium based on the accumulated release portion, the accumulated release portion of tritium of a spherical sample to be detected at different moments is measured at a plurality of temperatures within a certain temperature range, a specific numerical value of the diffusion coefficient of tritium in the sample to be detected at the temperature is obtained, a general expression of the diffusion coefficient of tritium in the spherical porous medium material sample within the corresponding temperature range is further obtained, and the diffusion coefficient of tritium in the spherical porous medium material sample within the heating temperature range is determined.
Description
Technical Field
The invention relates to the technical field of reactor engineering, in particular to a method for determining a tritium diffusion coefficient based on an accumulated release fraction.
Background
The ultra High Temperature Reactor (VHTR), which is one of six advanced fourth Generation nuclear energy systems defined by The fourth Generation nuclear energy system International Forum (GIF), has a great potential in The aspects of High Temperature heat supply and development of High Temperature processes such as High Temperature hydrogen production, seawater desalination and The like, in addition to being applied to commercial power Generation. The High Temperature Gas-cooled Reactor (HTGR) is a prototype of the ultra High Temperature Gas cooled Reactor, and its greatest feature is its intrinsic safety characteristics. Although the high-performance fuel elements fundamentally prevent the possible reactor core burnout accidents of the pressurized water reactor and retain most of the radioactive nuclides of the fuel elements, a small amount of tritium still exists in the primary loop helium due to the strong penetration of the tritium, the activation of Li impurities in carbon bricks, the activation of the primary loop helium impurities He-3 and the like. The 10MW high temperature gas-cooled reactor (HTR-10) in China belongs to the ball bed type high temperature gas-cooled reactor, and is the only ball bed type high temperature gas-cooled reactor which can operate in the world at present. A Pebble Bed Modular High-Temperature gas-cooled Reactor nuclear power plant Project (HTR-PM) designed and built on the basis of HTR-10 is a commercial demonstration power station of a first Pebble Bed High-Temperature gas-cooled Reactor worldwide and spans out an important step of commercialization of the High-Temperature gas-cooled Reactor. The research on the HTR-10 on the radioactive nuclide in the primary circuit has important significance for the evaluation of the radioactive containment capacity of the high-temperature gas cooled reactor and the evaluation of radiation safety.
The fuel elements of HTR-10 and HTR-PM are all ceramic type TRISO (structural-Isotropic) coated particle spherical fuel elements with a diameter of 60mm, divided into an inner spherical core with a diameter of 50mm, a spherical fuel zone of graphite matrix uniformly dispersed with TRISO coated particles, and an outer fuel-free graphite spherical shell with a thickness of 5 mm. The core of the TRISO-coated particles was 0.5mm UO2The small ball is coated with a loose pyrolytic carbon layer, an inner compact pyrolytic carbon layer, a silicon carbide layer and an outer compact pyrolytic carbon layer from inside to outside. The reactor active area is surrounded by graphite reflective layers and contains a large number of fuel elements (27000 fuel elements are contained in the HTR-10 balanced core, and 420000 fuel elements are contained in the HTR-PM single balanced core).
There are mainly four routes for tritium production in high temperature gas cooled reactors: ternary fission of fissionable nuclides in the fuel element; activating impurities of Li-6 and Li-7 in matrix graphite, a graphite reflecting layer and a carbon brick; activation of He-3 in the main loop coolant; activation of B-10 in absorption balls, control rods and carbon bricks. Because a large amount of graphite materials exist in the high-temperature gas cooled reactor, tritium generated in ternary fission and matrix graphite and structural graphite enters primary loop helium through transportation in the graphite. Tritium, as an isotope of hydrogen, is easily introduced into the biosphere and is difficult to remove once helium in a primary circuit leaks under normal operation conditions or accident conditions, and finally, a large public dose is caused. Thus, the measurement and analysis of tritium is a relatively interesting part of the assessment of environmental impact of nuclear facilities.
In the existing analysis of the source item of the high-temperature gas cooled reactor, the diffusion coefficient is the most important parameter in the research of the transport process of tritium in graphite, but the theoretical research and the experimental result of the diffusion coefficient of tritium in the graphite material of the high-temperature gas cooled reactor are relatively lacked. The measurement of the diffusion coefficient of tritium is mostly concentrated in various stainless materials, and is mostly obtained by simple mass correction of the diffusion coefficients of hydrogen and deuterium. The measurement methods and results far fail to satisfy the research on the transport behavior of tritium in reactor core fuel elements, graphite spheres, graphite reflecting layers and primary circuits in the high-temperature gas-cooled reactor.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for determining the diffusion coefficient of tritium based on the accumulated release portion, which comprises the steps of measuring the accumulated release portion of tritium of a spherical sample to be measured at different times within a certain temperature range, deriving the specific value of the diffusion coefficient of tritium in the sample to be measured under the temperature condition, and further obtaining a general expression of the diffusion coefficient of tritium in the spherical porous medium material within the corresponding temperature range, namely determining the diffusion coefficient of tritium in the heating temperature range in the porous medium material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method of determining a tritium diffusion coefficient based on a cumulative fraction released, the method comprising:
s1, heating the sample of the spherical porous medium material to diffuse and release HT and T in the sample2And CH3T is oxidized into HTO and T correspondingly2O and CO2HTO, T2O is retained in the distilled water sample liquid;
s2, during a certain time period 0-tjIn which t isj>0, starting from the experimental measurementsSetting the initial point as 0 moment, dividing the initial point into a plurality of time periods to correspondingly measure the activity of tritium in HTO and T2O in the distilled water sample liquid, and adding the tritium values cumulatively released in the time periods to obtain the cut-off time point TjCumulative tritium activity value A (t) released from sample to be testedj) And the initial total content A of tritium in the spherical porous medium material sample0The ratio of the two is the time point tjUpper corresponding fraction of cumulative tritium release F (t)j)；
Wherein R is the radius [ m ] of the spherical porous medium material sample]D is the diffusion coefficient [ m ]2/s]Pi is a circumferential constant, A0Is the initial total content [ Bq ] of tritium activity in a spherical porous medium material sample]，tjMeasuring the corresponding time [ s ] for a certain activity in the experiment]，A(tj) Is tjTritium activity value [ Bq ] cumulatively released from sample to be detected at corresponding moment]，F(tj) Is tjThe cumulative release share of tritium in the spherical porous medium material sample is obtained at the moment;
s3, a series of time points t measured experimentally at a certain temperaturejAnd the corresponding fraction of cumulative tritium release F (t)j) I.e. a set (t)j,F(tj) Data, using the cumulative fraction of tritium released F (t)j) Fitting a numerical value of an optimal diffusion coefficient D of tritium in the spherical porous medium material sample at the temperature by using the formula;
s4, changing the heating temperature of the spherical porous medium material and repeating the processes from S1 to S3 to obtain a series of temperature values and corresponding measured values of the diffusion coefficient of tritium in the spherical porous medium material at the temperature, namely a group of (T, D) data, and then obtaining the key parameters of the general expression of the diffusion coefficient in the corresponding experimental temperature range by utilizing Arrhenius formula fitting: diffusion frequency factor D0[m2/s]And diffusion excitation energy Q [ J/mol [ ]]Namely, a general expression of the diffusion coefficient of tritium in the spherical porous medium material in the corresponding temperature range is determined；
Wherein R isgIs an ideal gas constant with a value of 8.314[ J/(mol. K)]T is the temperature [ K ]]；
The diffusion coefficient expression determined by the spherical porous medium material sample is a general expression of the diffusion coefficient of tritium in the porous medium material within the heating temperature range.
In some embodiments, the heating temperature of the sample of spherical porous medium material is 300-.
In some embodiments, the HT and T diffused from the sample of porous media material is heated2And CH3T, oxidizing into HTO and T by adding a solid catalytic oxidation device2O and CO2、HTO。
Meanwhile, the present invention also provides an experimental system for implementing the method for determining a tritium diffusion coefficient based on a cumulative fraction released as set forth in claim 1, characterized in that the experimental system comprises:
a carrier gas device;
heating furnace;
a solid catalytic oxidation unit;
a sampling device;
and a liquid scintillation meter;
wherein the gas carrying device is communicated with the sampling device through a pipeline, the heating furnace is arranged on the pipeline, the liquid scintillation meter is matched with the sampling device and used for carrying out tritium activity measurement on a sample after sampling, and the catalytic oxidation device is arranged on the pipeline between the heating furnace and the sampling device.
In some embodiments, the cooling system is disposed on the conduit between the heating and catalytic oxidation device and the sampling device.
In some embodiments, the sampling device comprises a plurality of sampling bottles, distilled water is contained in the sampling bottles, adjacent sampling bottles are communicated through a pipeline, and a stop valve is arranged on the pipeline.
In some embodiments, the sampling device further comprises a temperature control device, wherein the temperature control device is matched with the sampling bottle to realize temperature control in the sampling bottle.
In some embodiments, the sampling assemblies are in multiple groups, and the multiple groups of sampling assemblies are arranged in parallel.
In some embodiments, the sampling vial is provided with a sparging device.
In some embodiments, the experimental system still includes tail gas recovery unit, tail gas recovery unit includes check valve, stop valve, pressure gauge and waste gas holding vessel, waste gas holding vessel is linked together through the gas outlet that is located the most terminal sampling bottle among pipeline and the sampling device, the pressure gauge is installed waste gas holding vessel air inlet department, check valve and stop valve are in proper order the series installation on the pipeline.
The invention has the beneficial effects that: according to the method and the experimental system for determining the diffusion coefficient of tritium in the spherical porous medium material, the accumulated release share of tritium of a spherical sample to be tested at different moments is measured at a plurality of temperatures within a certain temperature range, the numerical value of the diffusion coefficient of tritium in the spherical sample to be tested under the temperature condition is obtained, a general expression of the diffusion coefficient of tritium in the spherical porous medium material within the corresponding temperature range is further obtained, and the diffusion coefficient of tritium in the heating range in the porous medium material is determined.
Drawings
FIG. 1 is a schematic diagram of the structural principle of the experimental system in the present invention.
FIG. 2 is a schematic view of the measurement principle of the liquid scintillation meter of the present invention.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description.
The invention provides a method and an experimental system for determining a tritium diffusion coefficient based on accumulated release portions, aiming at the fact that in the existing high-temperature gas cooled reactor source item analysis, the diffusion coefficient is the most important parameter in the process of researching the transport of tritium in graphite, but theoretical research and experimental results of the diffusion coefficient of tritium in a porous medium material are relatively lacked at present, and the method and the experimental system measure the accumulated release portions of tritium of a spherical sample to be detected at different times within a certain temperature range, and obtain a specific numerical value of the diffusion coefficient of tritium in the spherical sample to be detected under the temperature condition, so as to obtain a general expression of the diffusion coefficient of tritium in the spherical porous medium material within a corresponding temperature range, namely determine the diffusion coefficient of tritium in the heating temperature range in the porous medium material.
First, the present invention provides a method for determining a tritium diffusion coefficient based on a cumulative release fraction, for convenience of description, the present embodiment is described by taking a graphite material in a porous medium material as an example, and other porous medium materials are also applicable to the following method and experimental system, without limitation. The method comprises the following steps:
s1, heating and irradiating graphite spheres or other spherical graphite materials at a certain temperature (in the embodiment, the temperature is 300 ℃ C. and 1400 ℃ C.), so as to diffuse and release HT and T in the sample2And CH3T is oxidized into HTO and T correspondingly2O and CO2HTO (preferably, in this embodiment, by using a solid catalytic oxidation device, so that the HT, T released by diffusion after heating the graphite nodule sample can be obtained2And CH3The chemical form of tritium in T is oxidized to tritium water (HTO or T)2O), the solid catalytic oxidant adopted in the device for conveniently collecting, heating and catalytic oxidation is CuO-ZnO-Al2O3Typical temperature 400-2O is retained in the distilled water sample solution.
S2, in a certain time period tj-tiInner (t)j>tiNot less than 0, and the initial point of the start of the experimental measurement is set to 0 time) of the HTO and T in the distilled water sample liquid2Activity of tritium in O, wherein the value of the activity is the time period tj-tiInternal cumulative tritium release value A (t)j-ti) The time period tj-tiInternal cumulative tritium release value A (t)j-ti) From time t to t before when t is 0iAdding tritium values cumulatively released in a plurality of time periods in the moment (the graphite nodule sample reaches a certain specific temperature T) to obtain a cut-off time point TjTritium activity value A (t) cumulatively released from graphite nodule sample to be detectedj) And the initial total content A of tritium in the graphite nodule sample0The ratio of the two is the time point tjUpper corresponding fraction of cumulative tritium release F (t)j)，
And through the formula, the method has the advantages that,
wherein R is the radius [ m ] of the graphite nodule sample]D is the diffusion coefficient [ m ]2/s]Pi is a circumferential constant, A0Is the initial total content [ Bq ] of tritium activity in a spherical porous medium material sample]，tjMeasuring the corresponding time [ s ] for a certain activity in the experiment]，A(tj) From the moment t-0 to a certain point in time t for collectionjInternal cumulative tritium Activity [ Bq]Is not the tj-tiTritium activity in time periods, e.g. 0-t1,t2-t1，t3-t2，…，tj-tiEtc., a certain t calculated in practicejTritium activity A (t) of cumulative tritium release at timej)＝A(t1-0)+A(t2-t1)+…+A(tj-ti) From time t to time t of 0jThe sum of the tritium activity accumulations in all the time before the moment, and then t can be obtained according to the formulajThe cumulative fraction F (t) released of tritium at the timej)。
S3, a series of time points t measured experimentally at a certain temperaturejAnd the corresponding fraction F (t) of tritium cumulative releasej) I.e. a set (t)j,F(tj) Data, using the cumulative fraction of tritium released F (t)j) Fitting a numerical value of an optimal diffusion coefficient D of tritium in the graphite nodule sample at the temperature by using the formula;
s4, changing the heating temperature of the graphite nodules and repeating the process to obtain the graphite nodulesThe measurement values of the diffusion coefficient of the series of temperature values T and tritium corresponding to the temperature in the graphite nodule sample D, namely a group of (T, D) data, are fitted by using an Arrhenius formula (as follows) to obtain the key parameters of the general expression of the diffusion coefficient in the corresponding experimental temperature range: diffusion frequency factor D0[m2/s]And diffusion excitation energy Q [ J/mol [ ]]Namely, a general expression of the diffusion coefficient of tritium in the graphite nodule in the corresponding temperature range is determined.
Wherein R isgIs an ideal gas constant with a value of 8.314[ J/(mol. K)]T is the temperature [ K ]]；
The diffusion coefficient of the porous medium material is determined by measuring the diffusion coefficient of the spherical porous medium material sample through a diffusion coefficient expression determined in the spherical porous medium material sample, namely a general expression of the diffusion coefficient of tritium in the porous medium material within the heating temperature range, namely the diffusion coefficient is the inherent property of the material and is irrelevant to the shape of the material.
Compared with the method adopting the tritium activity concentration on-line monitoring device, the method adopting the cumulative release share measuring method does not influence the measuring result of the tritium cumulative activity concentration if other inert gas nuclides, C-14 and the like exist, so that the method is more suitable for measuring the diffusion coefficient of tritium in the porous medium material sample containing various nuclides easy to release.
Referring to fig. 1, the present embodiment also provides an experimental system for implementing the method for determining the tritium diffusion coefficient based on the cumulative released fraction, which includes a carrier gas device 1, a heating furnace 2, a heating and catalytic oxidation device 3, a cooling device 4, a sampling device 5, a flash tank 19 and a tail gas recovery device 6. The carrier gas device 1 may provide helium gas as a carrier for diffusion release of tritium from the spherical porous media material. The gas outlet of the carrier gas device 1 is connected with one end of a heating furnace 2 through a pipeline 8, the heating furnace 2 heats helium entering the pipeline 8, and thenThe heating furnace 2 has the function of heating the porous medium material containing tritium to a required temperature and maintaining the temperature at a stable certain temperature for carrying out tritium release experiments, generally, the temperature range is 300-1400 ℃, and a thermometer 13 is arranged on the heating furnace 2 to monitor the working temperature. A stop valve 7, a pressure gauge 9, a mass flow meter 10, and a stop valve 12 are provided in this order in a pipe 8 between the gas carrying device 1 and the heating furnace 2. The other end of the heating furnace 2 is connected with one end of the heating and catalytic oxidation device 3 through a pipeline 8, a pair of stop valves 14 and 15 are arranged between the pipeline 8 positioned between the heating and catalytic oxidation device and the heating and catalytic oxidation device 3, and a thermometer 16 is arranged on the heating and catalytic oxidation device 3 for monitoring the working temperature of the heating and catalytic oxidation device. The other end of the heating and catalytic oxidation unit 3 is connected to one end of a cooling unit 4 via a pipe 8, the cooling unit 4 is used for cooling the heated helium gas to room temperature-25 ℃, and a stop valve 17 is provided on the pipe 8 between the heating and catalytic oxidation unit 3 and the cooling unit 4. The other end of the cooling device 4 is connected to a sampling device 5 for the HTO and T contained in the helium gas2Tritium in an O form is sampled by the sampling device 5, and the cooling device 4 has the function of preventing the temperature of helium carried with gas from being too high, so that the rapid evaporation of sampling liquid is avoided. The sampling device 5 includes a plurality of sampling bottles 51, in this embodiment, four sampling bottles 51, and in practice, the number of sampling bottles 51 is flexibly set according to the experimental requirements, and is not limited. The sampling bottles 51 are filled with distilled water, adjacent sampling bottles 51 are communicated through a pipeline 53, and a stop valve 54 is arranged on the pipeline 53. A sampling bottle 51 located at the end of the sampling device 5 is connected to the tail gas recovery device 6 by a pipe 53. Tail gas recovery unit 6 includes check valve 62, stop valve 63, pressure gauge 64 and waste gas holding vessel 61, and waste gas holding vessel 61 is linked together through the gas outlet that is located the most terminal sampling bottle 51 in pipeline and the sampling device 5, and pressure gauge 64 is installed in waste gas holding vessel 61 air inlet department, and check valve 62 and stop valve 63 are established ties in proper order and are installed on the pipeline.
Referring to fig. 2, the liquid scintillation meter 19 is a schematic structural diagram for measuring tritium activity in the sampling bottle 51. When the tritium activity detector is used, tritium activity in the sampling bottle is detected through an analytical instrument on the tritium activity detector.
In some embodiments, in order to enable the whole experiment system to perform detection at different temperatures, the sampling assemblies 5 are multiple groups, six groups are shown in this embodiment, the number of the sampling assemblies 5 in practice is flexibly set according to experiment requirements, and not limited, the multiple groups of the sampling assemblies 5 are mutually connected in parallel. The arrangement of a plurality of groups of sampling bottles connected in parallel ensures that the switching can be carried out without stopping when switching to the next group, for example, every 20 minutes, thereby realizing the uninterrupted accumulative sampling measurement of the released tritium and simultaneously recording enough experimental points (t) in a certain time rangej,F(tj) Fitting out a specific numerical value of the diffusion coefficient D at a certain temperature T. The expression of the diffusion coefficient in a certain temperature range conforms to the Arrhenius formula
The measurement process is repeated as a function of the temperature T, a specific value of the diffusion coefficient D corresponding to a plurality of temperatures T, i.e. a series of (T, D) data, is determined, D is determined according to the Arrhenius formula0And Q, and further solving a general expression of the diffusion coefficient of tritium in the porous medium material in a corresponding temperature range.
In some embodiments, in order to prevent the sample solution in the sample bottle 51 from rapidly evaporating, a temperature control device 52 is disposed around the sample bottle 51, and the temperature control device 52 is operated to control the temperature of the sample solution in the sample bottle 51, typically to 4-20 ℃.
In some embodiments, to ensure the HTO, T in the carrier gas in the sample bottle 512O and the distilled water of the sampling solution perform a sufficient isotope substitution reaction, a bubbling device is further arranged in the sampling bottle 51, and HTO and T in the carrier gas in the sampling bottle 51 are enabled to be carried out by the bubbling device2O is sufficiently retained in the sample solution.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (3)
1. A method for determining a tritium diffusion coefficient based on a cumulative fraction released, the method comprising:
s1, heating the sample of the spherical porous medium material to diffuse and release HT and T in the sample2And CH3T is oxidized into HTO and T correspondingly2O and CO2HTO, T2O is retained in the distilled water sample liquid;
s2, during a certain time period 0-tjIn which t isj>0, setting the initial point of the experimental measurement to be 0 time, dividing the initial point into a plurality of time periods to correspondingly measure the HTO and the T in the distilled water sample liquid2The activity of tritium in O is obtained by adding the tritium values cumulatively released in a plurality of time periods to obtain a cut-off time point tjCumulative tritium activity value A (t) released from sample to be testedj)[Bq]And the initial total content A of tritium in the spherical porous medium material sample0The ratio of the two is the time point tjUpper corresponding fraction of cumulative tritium release F (t)j)；
Wherein R is the radius [ m ] of the spherical porous medium material sample]D is the diffusion coefficient [ m ]2/s]Pi is a circumferential constant, A0Is the initial total content [ Bq ] of tritium activity in a spherical porous medium material sample]，tjMeasuring the corresponding time [ s ] for a certain activity in the experiment]，A(tj) Is tjTritium activity value [ Bq ] cumulatively released from sample to be detected at corresponding moment]，F(tj) Is tjThe cumulative release share of tritium in the spherical porous medium material sample is obtained at the moment;
s3, a series of time points t measured experimentally at a certain temperaturejAnd the corresponding fraction of cumulative tritium release F (t)j) I.e. a set (t)j,F(tj) Data, using the cumulative fraction of tritium released F (t)j) Is fitted with the formula ofThe optimal diffusion coefficient D value of tritium in the spherical porous medium material sample at the temperature;
s4, changing the heating temperature of the spherical porous medium material and repeating the processes from S1 to S3 to obtain a series of temperature values and corresponding measured values of the diffusion coefficient of tritium in the spherical porous medium material at the temperature, namely a group of (T, D) data, and then obtaining the key parameters of the general expression of the diffusion coefficient in the corresponding experimental temperature range by utilizing Arrhenius formula fitting: diffusion frequency factor D0[m2/s]And diffusion excitation energy Q [ J/mol [ ]]Determining a general expression of the diffusion coefficient of tritium in the spherical porous medium material within a corresponding temperature range;
wherein R isgIs an ideal gas constant with a value of 8.314[ J/(mol. K)]T is the temperature [ K ]]；
The diffusion coefficient expression determined by the spherical porous medium material sample is a general expression of the diffusion coefficient of tritium in the heating temperature range in the spherical porous medium material sample.
2. The method for determining the tritium diffusion coefficient based on the accumulated fraction released is characterized in that the heating temperature of the spherical porous medium material sample is 300-1400 ℃.
3. A method for determining tritium diffusion coefficient based on cumulative fraction released according to claim 1, characterized in that HT, T diffused from heating porous medium material sample2And CH3T, oxidizing into HTO and T by adding a solid catalytic oxidation device2O and CO2、HTO。
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