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CN115979779B - Control method of multimode enrichment analysis device for xenon background - Google Patents

Control method of multimode enrichment analysis device for xenon background Download PDF

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Publication number
CN115979779B
CN115979779B CN202310033131.9A CN202310033131A CN115979779B CN 115979779 B CN115979779 B CN 115979779B CN 202310033131 A CN202310033131 A CN 202310033131A CN 115979779 B CN115979779 B CN 115979779B
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valve
separation column
stage
xenon
xenon separation
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CN115979779A (en
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王文鹏
金玉仁
毛传林
吴程
潘志东
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Zhejiang Hengda Instruments Co ltd
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Zhejiang Hengda Instruments Co ltd
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Abstract

The invention discloses a control method of a multimode enrichment analysis device for a xenon background, which is characterized in that the control method comprises the steps of setting working parameters of a plurality of program control valves, a gas taking enrichment device, a plurality of stages of xenon separation columns, a refrigerator and a xenon separation column activation regeneration device of the device through a control system. The invention realizes shallow low-temperature adsorption by controlling the adsorption temperature to be minus 28 ℃ to 18 ℃ through the refrigerator, realizes pressurized adsorption by increasing the tail pressure of each stage of xenon separation column to be 0.1MPa to 0.6MPa, improves the dynamic adsorption coefficient of each stage of xenon separation column from 0.43L/g to 1.2 to 3.4L/g at normal temperature and pressure, and realizes self-elevation of adsorption performance, thereby improving adsorption efficiency and reducing the loading amount of the adsorbent of each stage of xenon separation column under specified air inlet volume; the invention can also be suitable for large-volume sampling monitoring and high-frequency small-volume sampling monitoring, purifying and concentrating sensitive sampling monitoring, so that the invention not only can be used for forensics of nuclear events and early warning of nuclear accidents, but also can be used for sampling and monitoring nuclear emergency radioactive xenon immediately.

Description

Control method of multimode enrichment analysis device for xenon background
Technical Field
The invention relates to a control method of a monitoring device for radioactive xenon in air, in particular to a control method of a multimode enrichment analysis device for xenon background.
Background
The nuclear activities of nuclear facilities such as a reactor, a nuclear power station, a nuclear test and the like can generate radioactive xenon isotopes and possibly leak into the air, and monitoring of characteristic radioactive nuclides is a necessary measure for guaranteeing the nuclear activities of the nuclear facilities and the environmental safety of the nuclear facilities. Radioactivity in ambient air 133 Xe background is low, normally only about 0.2. 0.2mBq/m 3 About, the sensitivity of radioactive xenon sampling monitoring is high, which has been proved to be nuclear facility nuclear activity radiationEffective means of sexual leakage monitoring and nuclear event evidence collection.
However, the control method of the xenon enrichment device in air disclosed in the prior art has the following problems:
1. the enrichment method of forward adsorption and forward desorption of the enrichment device is controlled, so that the loading of the adsorbent is influenced, the volume of the membrane product gas entering the adsorption tower cannot be automatically matched with the dosage of the adsorbent, and the loss of the adsorbent is further caused, thereby increasing the maintenance frequency and the operation and maintenance cost of the enrichment device, and further influencing that the enrichment device cannot be used in environments of large-volume sampling enrichment and high-frequency rapid sampling enrichment.
2. By controlling the enrichment method of forward adsorption and forward desorption of the enrichment device, the total amount of gas entering the next stage of adsorption cannot be reduced, so that the two-stage and three-stage adsorption devices are larger in order to adapt to the desorption gas amount of the previous stage and the tail gas amount of forward adsorption, and the total volume and the production cost of the device are increased.
3. The sampling monitoring sensitivity of the radioactive xenon in the air is insufficient, and the daily monitoring of the radioactive xenon background in the air is difficult to develop, so that the early warning capability of the radioactive xenon leakage of nuclear accidents is insufficient.
4. The related equipment in the equipment cannot be controlled to work in a shallow low-temperature environment, so that the energy consumption of the equipment is increased.
Therefore, the above problems are not solved, and the present invention provides a control method of a multimode enrichment analysis device for xenon background.
Disclosure of Invention
The invention aims to solve the problems and provides a control method of a multimode enrichment analysis device for a xenon background.
In order to achieve the above purpose, the present invention provides a control method of a multimode enrichment analysis device for xenon background, which is characterized in that the control method comprises:
1) Setting working parameters of a plurality of program control valves, a gas taking enrichment device, a plurality of stages of xenon separation columns, a refrigerator and a xenon separation column activation regeneration device of the device through a control system;
2) The refrigerating equipment in the refrigerator is controlled through the control system, the temperature of the refrigerator is kept between minus 28 ℃ and 18 ℃, the gas taking enrichment device is controlled to take gas for enrichment, constant components and granular substances in the air are removed, high-concentration product gas is obtained, and the high-concentration product gas enters the primary buffer mechanism;
3) Controlling the first-stage xenon separation column A or the first-stage xenon separation column B to alternately work for first-stage purification and concentration, wherein one of the first-stage xenon separation column A or the first-stage xenon separation column B carries out first-stage forward pressure-increasing adsorption, and the other one carries out a first-stage low-pressure reverse desorption procedure; then controlling a program control valve connected with the primary buffer mechanism and the purification concentration unit to open a certain opening, so that product gas in the primary buffer mechanism is sent into a primary xenon separation column A or a primary xenon separation column B, controlling the discharge amount of a first mass flow controller to be lower than the air inflow of the valve, controlling the pressure in front of the primary xenon separation column A or the primary xenon separation column B to be higher than the pressure behind the column, discharging the adsorbed tail gas through the first mass flow controller to realize primary forward boost adsorption, and controlling the primary xenon separation column A or the primary xenon separation column B to perform a primary low-pressure reverse desorption process after the primary forward boost adsorption is finished;
4) When the primary low-pressure reverse desorption is completed, carrying out primary activation regeneration, vacuumizing a primary xenon separation column A or a primary xenon separation column B by controlling a vacuum pump, controlling an electric heating belt of a xenon separation column activation regeneration device to heat the primary xenon separation column A or the primary xenon separation column B to 250-350 ℃, maintaining the temperature for 40-180 min, stopping heating, then controlling an air door connected with a refrigerator to be opened, simultaneously controlling an induced draft fan to start, introducing low-temperature gas in the refrigerator into the xenon separation column activation regeneration device by the induced draft fan, and cooling the primary xenon separation column A or the primary xenon separation column B until the temperature is cooled to an adsorption temperature, thereby completing activation regeneration;
5) During secondary purification and concentration, first performing secondary forward boost adsorption, pushing primary desorption gas in a secondary buffer mechanism to enter a secondary xenon separation column through primary adsorption tail gas of the primary xenon separation column A or the primary xenon separation column B, performing secondary adsorption and purification for 10-40 min, setting the discharge pressure or flow of a first pressure regulator to be smaller than the pressure or flow of the secondary xenon separation column when air is taken in, thereby raising the adsorption tail pressure of the secondary xenon separation column, and performing secondary forward boost adsorption;
6) After the secondary forward boost adsorption is finished, controlling a vacuum pump to vacuumize the secondary xenon separation column, reducing the pressure in the secondary xenon separation column to 5-20 Pa, stopping vacuumizing, and then controlling an electric heating belt to heat the secondary xenon separation column to 120-220 ℃; then controlling a vacuum pump to vacuumize the three-stage buffer mechanism to the limit vacuum of 1-5 Pa; controlling the connection pipeline of the second-stage xenon separation column and the third-stage buffer mechanism to be communicated, controlling the maintenance temperature of the second-stage xenon separation column to be 10-60 min, and controlling the first-stage adsorption tail gas to be introduced into the second-stage xenon separation column to push the second-stage desorption gas in the second-stage xenon separation column into the third-stage buffer mechanism until the pressure sensor detects that the pressure in the third-stage buffer mechanism reaches a specified pressure value or is not raised any more, and completing the second-stage reverse low-pressure desorption;
7) After the secondary reverse low-pressure desorption is finished, controlling a vacuum pump to vacuumize the secondary xenon separation column, controlling an electric heating belt of an activation regeneration device of the secondary xenon separation column to heat the secondary xenon separation column to an activation temperature of 280-350 ℃, controlling the electric heating belt to stop heating after maintaining the temperature for 40-180 min, then controlling an air door connected with a refrigerator in the activation regeneration device of the secondary xenon separation column to be opened, simultaneously controlling an induced draft fan to start, introducing low-temperature gas in the refrigerator into the secondary xenon separation column to cool through the induced draft fan until a temperature sensor detects that the secondary xenon separation column is cooled to a set adsorption temperature, and completing activation regeneration;
8) Then controlling the first-stage adsorption tail gas to push the second-stage desorption gas stored in the third-stage buffer mechanism into the third-stage xenon separation column for three-stage purification and concentration, and controlling the discharge pressure or flow of the second pressure of the pressure regulator to be smaller than the pressure or flow of the air inlet of the third-stage xenon separation column, so as to raise the adsorption pressure of the third-stage xenon separation column, and discharging the tail gas subjected to pressure-raising adsorption by the third-stage xenon separation column through the second pressure regulator to finish three-stage forward pressure-raising adsorption;
9) After the three-stage forward boost adsorption is finished, controlling a vacuum pump to vacuumize the three-stage xenon separation column, reducing the pressure of the three-stage xenon separation column to 2-25 Pa, controlling an electric heating belt in an activation regeneration device of the three-stage xenon separation column to heat the three-stage xenon separation column to 120-220 ℃, and controlling the vacuum pump to vacuumize a source chamber to 2-5 Pa; then, connecting the three-stage xenon separation column and a source chamber to carry out high-temperature desorption and vacuum diffusion of the three-stage xenon separation column, and maintaining the temperature for 10-60 min; then controlling the three-stage buffer mechanism to be communicated with the three-stage xenon separation column, and pushing vacuum desorption gas and re-desorption gas in the three-stage xenon separation column to a source chamber to complete three-stage low-pressure reverse desorption source preparation;
10 After the three-stage low-pressure reverse desorption is completed, controlling a vacuum pump to vacuumize the three-stage xenon separation column, controlling an electric heating belt to heat the three-stage xenon separation column to 280-350 ℃, and stopping heating after maintaining the temperature for 40-180 min; then controlling an air door in an activation regeneration device of the three-stage xenon separation column to be opened, controlling a draught fan to be opened, introducing low-temperature gas in a refrigerator into the activation regeneration device by the draught fan, cooling the three-stage xenon separation column until a temperature sensor detects that the two-stage xenon separation column is cooled to a set adsorption temperature, and completing activation regeneration; after the source is manufactured, throughMeasuring the activity of the radioactive xenon in the source chamber in accordance with the measuring device; then the vacuum pump is controlled to vacuumize a plurality of archives, the source room, the thermal conductivity detector TCD and the archives are communicated after vacuumization, the sample gas in the sample source room is transferred to the archives for storage, and the total concentration of xenon is analyzed through the thermal conductivity detector TCD after pressure balance.
Further preferably, when the gas taking enrichment device takes gas enrichment, an air compressor of the gas taking enrichment device is controlled to convey air to a coarse filter through a pipeline, the air enters a cold dryer after passing through the coarse filter, the air enters a filter assembly after passing through the cold dryer, the air is conveyed to a multi-stage filtration module for multi-stage filtration, and then the air is conveyed into a polyimide hollow fiber membrane separator for removing constant components in the air, so that high-concentration product gas is obtained.
Further preferably, the control system controls the valve A or the valve B to be opened during the first-stage forward boost adsorption, so that the product gas in the first-stage buffer mechanism enters the first-stage xenon separation column A or the first-stage xenon separation column B; simultaneously controlling the valve F or the valve G and the first mass flow controller to be opened, and controlling the pressure of the adsorption tail gas through the first mass flow controller to enable the first-stage xenon separation column A or the first-stage xenon separation column B to carry out supercharging adsorption; the first-stage xenon separation column A and the first-stage xenon separation column B alternately perform uninterrupted continuous gas-taking adsorption on the product gas.
Further preferably, before the first-stage low-pressure reverse desorption, the vacuum pump is controlled to vacuumize the first-stage xenon separation column A or the first-stage xenon separation column B, the pressure in the column is reduced, when the pressure in the column reaches a set pressure value, the pressure sensor feeds back the pressure value in the column to the control system, and the control system controls the vacuum pump and the vacuumizing valve path of the first-stage xenon separation column A or the first-stage xenon separation column B to be closed; then controlling an electric heating belt to heat the first-stage xenon separation column A or the first-stage xenon separation column B to 120-220 ℃, and feeding back a temperature signal to a control system when a temperature sensor detects that the temperature reaches a set value; the control system controls the vacuum pump to vacuumize the secondary buffer mechanism, when the pressure sensor feeds back a signal of the secondary buffer mechanism at the limit negative pressure to the control system, the control system controls the vacuum pump to stop vacuuming, then controls a low-pressure reverse desorption pipeline of the primary xenon separation column A or the primary xenon separation column B to be communicated with the secondary buffer mechanism, maintains the temperature of the primary xenon separation column A or the primary xenon separation column B for 10-60 min for high-temperature vacuum desorption, and then pushes vacuum desorption gas and low-pressure desorption gas in the primary xenon separation column B or the primary xenon separation column A into the secondary buffer mechanism through an adsorption tail gas recycling pipeline of the primary xenon separation column A or the primary xenon separation column B until the pressure sensor detects that the pressure value of the secondary buffer mechanism reaches a specified pressure value or the pressure is not increased any more, and the secondary forward boost adsorption and the primary activation regeneration are prepared;
When the first-stage xenon separation column A or the first-stage xenon separation column B is vacuumized before reverse desorption, a control system controls a vacuum pump, a valve AC, a valve K, a valve E or a vacuum pump, a valve R, a valve L and a valve H to open a vacuumizing pipeline of the first-stage xenon separation column A or the first-stage xenon separation column B, and controls a valve D, a valve G and a valve J to close or controls a valve C, a valve F and a valve S to close when vacuumizing is completed, and then the vacuum pump and a program-controlled valve on the corresponding vacuumizing pipeline are closed;
when the first-stage xenon separation column A or the first-stage xenon separation column B is reversely desorbed, a control system controls a vacuum pump, a valve AC, a valve M and a valve N to open a vacuumizing pipeline forming a secondary buffer mechanism, so that the secondary buffer mechanism is vacuumized, wherein the control valve K, the valve L, the valve O, the valve P and the valve I are closed during vacuumizing, and the vacuum pump and the corresponding program-controlled valve are closed after vacuumizing; then the control system controls the valve B, the valve G, the mass flow controller II, the valve I, the valve C, the valve K, the valve M, the valve N or the valve A, the valve F, the mass flow controller II, the valve J, the valve D, the valve L, the valve M and the valve N to be opened, controls the valve E and the valve H to be closed, forms a reverse desorption pipeline of the first-stage xenon separation column A or the first-stage xenon separation column B, and pushes desorption gas in the first-stage xenon separation column A or the first-stage xenon separation column B into the second-stage buffer mechanism and then closes the corresponding program control valve;
When the first-stage xenon separation column A or the first-stage xenon separation column B is activated and regenerated, a control system is used for controlling a vacuum pump, a valve R, a valve K, a valve E or controlling the vacuum pump, a valve R, a valve L and a valve H to be opened, a control valve D, a valve G and a valve J to be closed or a control valve C, a valve F and a valve S to be closed, vacuumizing the first-stage xenon separation column A or the first-stage xenon separation column B, and controlling the vacuum pump and the corresponding program-controlled valve to be closed after vacuumizing is finished.
Further preferably, during the second-stage forward pressure-increasing adsorption, the control system controls the valve O, the valve N, the valve P, the valve Q and the first pressure regulator to be opened, the adsorption tail gas of the first-stage xenon separation column A or the first-stage xenon separation column B is used for pushing the first-stage desorption gas in the second-stage buffer mechanism into the second-stage xenon separation column, the discharge pressure or the flow of the first pressure regulator is controlled to be smaller than the pressure or the flow of gas when the first-stage forward pressure-increasing adsorption enters the second-stage xenon separation column, so that the second-stage forward pressure-increasing adsorption is performed, and the program-controlled valve at the corresponding position is controlled to be closed after the adsorption is completed;
when the second-stage low-pressure reverse desorption is performed, a control system is used for controlling a vacuum pump, a valve AC, a valve AD and a valve R to be opened so as to vacuumize the second-stage xenon separation column, and the vacuum pump and a program-controlled valve at a corresponding position are closed after vacuumization; then the control system controls the vacuum pump, the valve AD, the valve X and the valve V to open, vacuumizes the three-stage buffer mechanism to a limit negative pressure state, and then closes the vacuum pump and the program-controlled valve at the corresponding position;
When the adsorption tail gas of the first-stage xenon separation column A or the first-stage xenon separation column B pushes the low-pressure desorption gas in the second-stage xenon separation column into the third-stage buffer mechanism, the control system controls the valve O, the valve S, the valve R and the valve U to be opened, and the adsorption tail gas of the first-stage xenon separation column A or the first-stage xenon separation column B pushes the low-pressure desorption gas in the second-stage xenon separation column into the third-stage buffer mechanism until the pressure in the third-stage buffer mechanism reaches a specified pressure value or is not raised any more, and then program-controlled valves at corresponding positions are closed to complete the second-stage low-pressure reverse desorption;
when the secondary xenon separation column is activated, regenerated and vacuumized, the vacuum pump, the valve M and the valve S are controlled to be opened by the control system, then the secondary xenon separation column is vacuumized, and the vacuum pump and the corresponding program-controlled valve are controlled to be closed after the vacuumizing is completed.
Further preferably, when the three-stage forward pressure-increasing adsorption is performed, the valve T, the valve U and the valve V are controlled to be opened by a control system, and the second-stage desorption gas in the three-stage buffer mechanism is pushed into the three-stage xenon separation column for three-stage adsorption by the adsorption tail gas of the first-stage xenon separation column A or the first-stage xenon separation column B; when three-stage reverse desorption vacuumizing is performed, the control system controls the vacuum pump, the valve AC, the valve AD and the valve W to be opened, and the vacuum pump and the corresponding program control valve are closed after the vacuumizing is completed; when the three-stage xenon separation column is activated, regenerated and vacuumized, the control system controls the vacuum pump, the valve AC, the valve AD and the valve X to be opened, namely, the three-stage xenon separation column is vacuumized, and after the vacuumizing is completed, the control system controls the vacuum pump and the corresponding program-controlled valve to be closed.
Further preferably, when the source chamber is vacuumized, the control system controls the vacuum pump, the valve AC and the valve B6 to vacuumize the source chamber, and after vacuumization is completed, the vacuum pump and the program-controlled valve at the corresponding position are closed.
Further preferably, when the archive bottle is vacuumized, the control system controls the vacuum pump, the valve AC, the valve AE and the valve AB to be vacuumized after being opened, and controls the vacuum pump, the valve AC, the valve AE and the valve AB to be closed after the vacuumization is completed; when xenon in the source room is transferred to the file bottle, the transfer can be completed by controlling the opening of the valve AB and the valve B6 through the control system.
The invention also provides a control method for re-concentrating the sample gas in the archive bottle, which comprises the following steps: the first buffer group of the secondary buffer mechanism is vacuumized by controlling the vacuum pump, the valve AC and the valve M to be opened, the vacuum pump and the corresponding program-controlled valve are closed after the vacuumization is completed, then the valve AB and the valve AE are controlled to be opened, the valve AB is closed after xenon in the archives is transferred to the first buffer group, and then the archives are transferred to the archives for preservation after the secondary purification and the tertiary purification, so that the reconcentration of the sample gas is completed.
The invention also provides a control method for high-frequency rapid sampling monitoring, which comprises the following steps: the working time of one working period of the multi-mode enrichment analysis device is set, the gas taking enrichment device is controlled to take gas for pre-enrichment and then is conveyed to the first-stage xenon separation column A or the first-stage xenon separation column B, and the control system controls the first-stage xenon separation column A and the first-stage xenon separation column B to alternately carry out gas adsorption and separation column desorption regeneration of the pure nitrogen membrane product rich in xenon; when the first-stage xenon separation column A is adsorbed, the control system controls the first-stage xenon separation column B to carry out desorption for 20-40 min, activation for 40-60 min and cooling for 20-40 min; when the first-stage xenon separation column B is adsorbed, the control system controls the first-stage xenon separation column A to carry out desorption for 20-40 min, activation for 40-60 min and cooling for 20-40 min; the control system controls the valve B, the first-stage xenon separation column B, the valve G, the second mass flow controller, the valve I, the valve C, the valve K, the valve M, the valve R, the valve Q and the pressure regulator I to be opened for carrying out the first-stage xenon separation column B to adsorb the first-stage xenon separation column A for desorbing the second-stage adsorption for 20 to 40 minutes, or controls the valve A, the valve F, the second mass flow controller, the valve J, the valve D, the valve L, the valve M, the valve R, the valve Q and the pressure regulator I to be opened for carrying out the first-stage xenon separation column A to adsorb the first-stage xenon separation column B for desorbing the second-stage adsorption for 20 to 40 minutes; then controlling the valve O, the valve S, the valve R, the valve X and the pressure regulator II to be opened, introducing carrier gas into the three-stage xenon separation column, and carrying out secondary desorption and three-stage adsorption for 10-40 min; after the secondary desorption is completed, the induced draft fan is controlled to introduce cold air of the refrigerator seeds to cool the three-stage xenon separation column To adsorption temperature; then the control system controls the vacuum pump, the valve R and the valve B6 to be opened to vacuumize the source chamber, and the vacuum pump is closed after vacuumization; then the control system controls the three-stage xenon separation column to carry out vacuum desorption for 10-40 min, then controls the valve U and the valve W to open, and the headspace three-stage xenon separation column is closed after the source preparation is completed; then controlling the three-stage xenon separation column to be activated in vacuum for 40-60 min, and then cooling for 40-60 min to the adsorption temperature, and carrying out three-stage adsorption of the next sample; the simultaneous control system controls twoThe coincidence measuring device is used for receiving three-level desorption gas in a round manner, and measuring the activity of radioactive xenon after the source preparation is completed; 20-30 min before the next sample gas is received in the source chamber, the control system controls the measurement of the radioactivity of the sample gas before the end of the measurement and transfers the measurement to an archive bottle for storage, the total concentration of xenon is analyzed by a thermal conductivity detector TCD, the effective sampling volume is calculated according to the stable xenon background in the air, the 133Xe activity concentration or the minimum detectable activity concentration MDC in the air is calculated by combining the actual measured radioactivity 133Xe net activity; after the number of the samples is 40-80, the control system controls the adsorption columns at each level to perform vacuum activation for 2-3 h, and cooling for 20-40 min to complete regeneration.
The invention realizes shallow low-temperature adsorption by controlling the adsorption temperature to be minus 28 ℃ to 18 ℃ through the refrigerator, realizes pressurized adsorption by increasing the tail pressure of each stage of xenon separation column to be 0.1MPa to 0.6MPa, improves the dynamic adsorption coefficient of each stage of xenon separation column from 0.43L/g to 1.2 to 3.4L/g at normal temperature and pressure, and realizes self-elevation of adsorption performance, thereby improving adsorption efficiency and reducing the loading amount of the adsorbent of each stage of xenon separation column under specified air inlet volume;
the control method of the invention realizes shallow low-temperature supercharging adsorption high-temperature vacuum desorption reverse desorption, can greatly increase the redundant loading of the adsorbent, realizes the self-adaptation of the adsorbent dosage to the air inflow, only needs to use the corresponding amount of adsorbent from bottom to top for adsorption and desorption of the entering large amount of raw gas, improves the service life of the adsorbent, and further enables the equipment to be suitable for large-volume sampling monitoring and high-frequency small-volume sampling monitoring, purification, concentration and sensitive sampling monitoring, thereby being not only used for evidence taking and early warning of nuclear accidents, but also switching into nuclear emergency radioactive xenon sampling monitoring immediately;
the invention controls the adsorption tail gas of the first-stage xenon separation column A or the first-stage xenon separation column B to be used as carrier gas, and does not need to provide carrier gas for helium and nitrogen cylinders, so that common activated carbon adsorbent can be used as filler of the xenon separation column for gradual concentration, no carrier gas is required to be externally connected, and a specific adsorbent is selected, thereby saving the cost.
Drawings
FIG. 1 is a schematic illustration of the process flow of the present invention;
fig. 2 is a schematic diagram of the control flow of the present invention.
Legend description: 1. a gas-taking enrichment device; 11. an air compressor, 12, a sampling head; 13. a cold dryer; 14. a filter; 15. polyimide hollow fiber membrane separator; 2. a purification concentration unit; 3. a refrigerator; 4. a first-stage buffer mechanism; 5. a first-stage xenon separation column A; 6. a first-stage xenon separation column B; 7. a mass flow controller I; 8. a vacuum pump; 10. an induced draft fan; 21. a secondary buffer mechanism; 211. a first buffer group; 212. a second buffer group; 22. a second stage xenon separation column; 23. a first pressure regulator; 24. a three-stage buffer mechanism; 25. a three-stage xenon separation column; 26. a second pressure regulator; 27. a source chamber; 271.a coincidence measurement device; 28. an archive bottle; 29. a thermal conductivity detector TCD; 9. a thermal insulation sleeve; 91. and (3) a damper.
Detailed Description
The following will further describe a control method of a multimode enrichment analysis device for xenon background according to the present invention with reference to fig. 1-2 of the accompanying drawings.
In the following embodiments, a first-stage xenon separation column A, a first-stage xenon separation column B, a second-stage xenon separation column and a third-stage xenon separation column are connected with a temperature sensor and a pressure sensor; the first-stage buffer mechanism, the second-stage buffer mechanism, the third-stage buffer mechanism, the source chamber, the first mass flow controller, the second mass flow controller, the first pressure regulator, the second pressure regulator and the pipeline are also connected with pressure sensors.
Example 1
The control system controls the temperature of the refrigerator 3 to be reduced to minus 28-18 ℃;
then the control system controls the air compressor 11 to start, the extracted air enters the air compressor 11 after filtering impurities with large particle size by the sampling head 12, the air compressor 11 transmits the gas to the coarse filter for filtering, then the air flow temperature is cooled by the cold dryer 13, impurities with particle size larger than 0.01 mu m are removed by the fine filter and the super fine filter, finally the constant components in the air are removed by the polyimide hollow fiber membrane separators 15 connected in series, and the highly concentrated xenon-enriched pure nitrogen membrane product gas is obtained and then enters the primary buffer mechanism 4 to finish gas extraction enrichment;
the method comprises the steps that a valve A is opened through a control system, pure nitrogen rich in xenon in a first-stage buffer mechanism 4 is sent into a first-stage xenon separation column A5, then the discharge amount of a first mass flow controller 7 is controlled, the pressure of adsorption tail gas is controlled to be 0.1-0.6 MPa, the pressure value is transmitted through a pressure sensor transmission value control system, the first-stage xenon separation column is subjected to forward pressure-increasing adsorption, when the adsorption of the first-stage xenon separation column A5 is finished, the control system is closed, the valve B is opened, namely the first-stage xenon separation column B6 is converted into the first-stage xenon separation column through the valve B, the control system is opened during the adsorption of the first-stage xenon separation column B6, the control system is used for controlling the valve G and the first mass flow controller 7, the pressure of adsorption tail gas is controlled to be 0.1-0.6 MPa, and the two xenon separation columns alternately enter the pure xenon-rich nitrogen film product gas for continuous gas absorption;
First-stage low-pressure reverse desorption: when the adsorption of the first-stage xenon separation column A5 is finished, desorption is carried out, firstly, a vacuum pump 8, a valve AC, a valve K and a valve E are controlled to open a communication vacuumizing pipeline to pump air for the first-stage xenon separation column A5, after a pressure sensor in the first-stage xenon separation column A5 senses that the pressure of a matched column is reduced to 15kPa, a control system closes the vacuum pump 8 and a corresponding program control valve, so that the vacuumizing pipeline is closed, then an electric heating belt is controlled to heat the first-stage xenon separation column A5 until a temperature sensor in the first-stage xenon separation column A5 senses that the temperature reaches 120-220 ℃ and maintains for 10-60 min for high-temperature vacuum desorption, then, the vacuum pump 8, the valve AC, the vacuumizing pipeline, the valve M and the valve N are controlled to start the pressure of a second-stage pumping buffer mechanism 21 to be 2Pa, and then the vacuumizing pipeline is closed; then, the valve B, the valve G, the valve I, the valve C, the valve K, the valve M and the valve N are controlled to be opened, and the low-pressure desorption gas in the first-stage xenon separation column A5 is pushed into the second-stage buffer mechanism 21 through the adsorption tail gas of the first-stage xenon separation column B6, and then the corresponding program-controlled valve is closed; then opening a valve B, a valve G, a valve O and a valve N to introduce the adsorption tail gas in the first-stage xenon separation column B6 into the second-stage buffer mechanism 21 until the pressure of the second-stage buffer mechanism 21 reaches a specified pressure value or the pressure of the second-stage buffer mechanism 21 is not increased any more, and then starting to communicate with the second-stage xenon separation column 22 to carry out second-stage adsorption;
Primary activation and regeneration: when the desorption of the first-stage xenon separation column A5 is finished, introducing the desorbed low temperature Jie Xiqi into a second-stage buffer mechanism 21, and regenerating the next-stage xenon separation column A5, firstly controlling a vacuum pump 8 to vacuumize the first-stage xenon separation column A5 through a valve AC, a valve K and a valve E by a control system, then controlling an electric heating belt to heat the first-stage xenon separation column A5 until the temperature sensed by a pressure sensor in the first-stage xenon separation column A5 reaches 250-350 ℃, maintaining the temperature for 120-180 min, stopping heating, then starting a draught fan 10, simultaneously opening an air door 97 connected with a refrigerator by a program control valve, introducing low-temperature gas in the refrigerator 3 into the first-stage xenon separation column A5 for cooling by the draught fan 10, and closing the draught fan 10 and the air door 97 until the temperature sensed by the temperature sensor is reduced to the adsorption temperature, thereby completing the activation regeneration;
second-stage forward boost adsorption: the adsorption tail gas of the first-stage xenon separation column B6 is introduced into the second-stage buffer mechanism 21, then the low-pressure desorption gas in the second-stage buffer mechanism 21 is pushed into the second-stage xenon separation column 22, the exhaust pressure of a first pressure regulator 23 is set, the adsorption tail pressure of the second-stage xenon separation column 22 is increased, and the second-stage forward boost adsorption is performed;
Second-stage low-pressure reverse desorption: after the secondary adsorption is finished, the control system controls the vacuum pump 8, the valve AC, the valve AD and the valve R to start and open a vacuumizing pipeline to suck air for the secondary xenon separation column 22, reduces the pressure sensed by the pressure sensor in the secondary xenon separation column 22 to be reduced to 5-20 Pa, closes the vacuumizing pipeline for the secondary xenon separation column 22, and then controls the electric heating belt to heat the secondary xenon separation column 22 to 120-220 ℃ and maintain the temperature; then controlling a vacuum pump 8, a valve AD, a valve X and a valve V to open to vacuumize the three-stage buffer mechanism 5 to reach a negative pressure limit state, heating the three-stage buffer mechanism for 10 to 60 minutes, then opening a valve R and a valve U, then opening a valve O, a first buffer group 211, a valve S, a second-stage xenon separation column 22, a valve R, a valve X and a valve V, pushing low-pressure desorption gas in the second-stage xenon separation column 22 into the three-stage buffer mechanism 24 through adsorption tail gas of the first-stage xenon separation column A5 or the first-stage xenon separation column B6 until a pressure sensor in the three-stage buffer mechanism 24 senses that the pressure reaches a designated pressure value or the pressure of the three-stage buffer mechanism 24 is not increased any more, and then closing a corresponding program-controlled valve to complete the second-stage low-pressure reverse desorption;
secondary activation regeneration: after the secondary low-pressure reverse desorption is completed, controlling a vacuum pump 8, a valve AC, a valve M and a valve S to open so as to vacuumize a secondary xenon separation column 22, controlling an electric heating belt to heat the secondary xenon separation column 22 until a temperature sensor senses that the temperature reaches 280-350 ℃, maintaining for 120-180 min, stopping heating, then starting a draught fan 10 and an air door 91, introducing low-temperature gas in a refrigerator 3 by the draught fan 10, cooling the secondary xenon separation column 22 until the temperature sensor senses that the temperature reaches an adsorption temperature, closing the draught fan 10 and the air door 91, stopping cooling, and completing activation regeneration of the secondary xenon separation column 22;
Three-stage forward boost adsorption: the control valve T, the valve U and the valve V are opened to lead the adsorption tail gas of the first-stage xenon separation column A5 or the first-stage xenon separation column B6 into the three-stage buffer mechanism 24, then the low-pressure desorption gas in the three-stage buffer mechanism 24 is pushed into the three-stage xenon separation column 25 through the valve V, the adsorption pressure of the three-stage xenon separation column 25 is increased through setting the discharge amount of the second pressure regulator 26, and the adsorption tail gas is discharged through the second pressure regulator 26 in the adsorption pipeline of the three-stage xenon separation column 25;
three-stage low-pressure reverse desorption: after the three-stage xenon separation column 25 is adsorbed, a vacuum pump 8, a valve AC, a valve AD and a valve W are controlled to be opened to vacuumize the three-stage xenon separation column 25, the pressure of the three-stage xenon separation column 25 is reduced to 2-25 Pa, after the vacuumizing is finished, the vacuum pump 8 and a program control valve at a corresponding position are closed, and an electric heating belt is controlled to heat a temperature sensor in the three-stage xenon separation column 25 to sense the temperature to 120-220 ℃; then controlling a vacuum pump 8, a valve AC and a valve B6 to open, vacuumizing the source chamber 27 of the online measurement and analysis unit to a limit vacuum of 2-5 Pa, stopping vacuumizing, opening a valve Y to communicate the three-stage xenon separation column 25 and the source chamber 27, performing high-temperature desorption vacuum diffusion of the three-stage xenon separation column 25, opening a valve U and a valve W after maintaining the temperature for 20-40 min, transferring re-desorption gas and vacuum adsorption gas in the three-stage xenon separation column 25 into the source chamber 27, and completing three-stage low-pressure reverse desorption source preparation;
And (3) tertiary activation and regeneration: after three-stage reverse desorption is completed, the vacuum pump 8, the valve AC, the valve AD and the valve X are controlled to vacuumize the three-stage xenon separation column 25, then the three-stage xenon separation column is closed, the three-stage xenon separation column is heated to 250-350 ℃ through an electric heating belt, heating is stopped after the temperature is maintained for 180min, then the induced draft fan 10 is started, the induced draft fan 10 introduces the gas in the refrigerator 3, and the three-stage xenon separation column 25 is cooled to the adsorption temperature to complete activation regeneration;
measurement and analysis: after the source is manufactured, throughThe coincidence measurement device 271 measures the activity of the radioactive xenon in the source chamber 27; then controlling a vacuum pump 8, a valve AC and a valve AB to vacuumize an archive bottle 28 in the xenon storage unit, opening the valve AB and a valve B6 after vacuumization is finished, communicating a source chamber 27, a thermal conductivity detector TCD29 and the archive bottle 28, and transferring xenon in the source chamber 27 into the archive bottle 28 for storage; and opening the thermal conductivity detector TCD29 until the thermal conductivity detector TCD is stable, and reading an indication value to complete the online analysis of the total concentration of xenon in the sample gas.
Example 2
In the embodiment, the process of re-concentrating the sample gas by adopting the device is adopted, so that the repeated detection of xenon among different devices can be realized, and the accuracy and the reliability of the detection are ensured; the repeated determination and detection effects of the measured sample gas of the device can also be realized; thereby realizing the accuracy and reliability of the early warning capability of nuclear leakage accidents;
Specific control ofThe method comprises the following steps: the enriched and purified sample gas of the device or other devices is utilized, the vacuum pump 8, the valve AC and the valve M are controlled to be opened to vacuumize the first buffer group 211, and the valve AB of the appointed archive bottle 28 is opened after the vacuumization is finished, so that the sample gas is transferred to the first buffer group 211 through a pipeline; then the sample gas in the first buffer group 211 is pushed into the second xenon separation column 22 for adsorption through the adsorption tail gas in the first xenon separation column A5 or the first xenon separation column B6, the adsorbed tail gas is discharged through the first pressure regulator 23, a second-stage low-pressure reverse desorption procedure is carried out after the second-stage adsorption is completed, the second-stage low-pressure reverse desorption procedure is carried out through the adsorption tail gas recycling pipeline of the first xenon separation column A5 or the first xenon separation column B6 after the second-stage low-pressure reverse desorption procedure is completed, the second-stage desorption sample gas pushed into the third-stage buffer mechanism 24 by the first-stage adsorption tail gas is sent into the third-stage xenon separation column 25 for secondary purification adsorption, the third-stage low-pressure reverse desorption is carried out after the adsorption is completed, the sample gas is concentrated again, and the second-stage low-pressure reverse desorption procedure is carried out after the concentration is completedThe coincidence measurement device measures the activity of the radioactive xenon in the sample source chamber 27; then the vacuum pump 8 is controlled to vacuumize a designated archive bottle 28 in the xenon storage unit, after vacuumization is finished, the source chamber 27, the thermal conductivity detector TCD29 and the archive bottle 28 are communicated, sample gas in the source chamber 27 is transferred into the archive bottle 28 for storage, and after pressure balance, the total concentration of the re-concentrated xenon is analyzed through the thermal conductivity detector TCD 29.
Example 3
Conventional sampling and monitoring of xenon in air:
the method described in the above example 1 was used to continuously sample and monitor the single-recovery gas of the first-stage xenon separation column A5 and the first-stage xenon separation column B6 for 4 hours, 1 sample/24 hours, continuously gas-taking and pre-enriching the gas with the polyimide hollow fiber membrane separator 15, alternately performing adsorption/desorption regeneration on the first-stage xenon separation column A5 and the first-stage xenon separation column B6, and performing 40min desorption, 160min activation and 40min cooling on the first-stage xenon separation column B6 when the first-stage xenon separation column A5 is adsorbed; when the first-stage xenon separation column B69 is used for adsorption, the first-stage xenon separation column A5 is subjected to 40min desorption, 160min activation and 40min cooling; after the secondary buffer mechanism 21 receives the primary desorption gas, the secondary xenon separation column 22 is used for 40min adsorption, 40min desorption, 120min activation and 40min cooling;
after the first 5 times of a certain sample and the second-stage desorption gas is received by the third-stage buffer mechanism 24, the adsorption is carried out for 40 minutes by using the third-stage xenon separation column 25; after the third-stage buffer mechanism 24 receives the second-stage desorption gas, the third-stage xenon separation column 25 is used for 40min adsorption, 60min desorption, 100min activation and 40min cooling;
20 minutes before the source chamber 27 receives the sample gas, the control system controls the measurement of the radioactivity of the sample before the end, transfers the sample gas to the archive flask 28 for storage, uses the thermal conductivity detector TCD29 to analyze the total concentration of xenon on line, calculates the effective sampling volume according to the stable xenon background in the air, calculates the 133Xe activity concentration or the minimum detectable activity concentration MDC in the air by combining the actual measured radioactivity 133Xe net activity.
Example 4
High-frequency rapid sampling monitoring: the high-frequency rapid sampling monitoring is used for nuclear emergency monitoring;
through the operation steps of gas extraction and enrichment in the embodiment 1, the polyimide hollow fiber membrane separator 15 is used for gas extraction and pre-enrichment by using the membrane separation working parameter with the maximum xenon yield in 2 hours, the single-cycle adsorption time of the first-stage xenon separation column A5 or the first-stage xenon separation column B6 is 2 hours, and the first-stage desorption, the second-stage adsorption, the second-stage desorption, the third-stage adsorption, the third-stage desorption source preparation and the measurement analysis are carried out after each cycle of the first-stage adsorption;
the first-stage xenon separation column A5 and the first-stage xenon separation column B6 alternately perform gas adsorption and separation column desorption regeneration of the pure nitrogen membrane product rich in xenon; when the first-stage xenon separation column A5 is used for adsorption, the first-stage xenon separation column B6 is subjected to 40min desorption, 40min activation and 40min cooling; when the first-stage xenon separation column B6 is used for adsorption, the first-stage xenon separation column A5 is subjected to desorption for 40min, activation for 40min and cooling for 40min; after the control valve B, the first-stage xenon separation column B6, the valve, the second mass flow controller 71, the valve I, the first-stage xenon separation column A5, the valve C, the valve K, the valve M, the first buffer group 211, the valve R, the second-stage xenon separation column 22, the valve Q and the pressure regulator I23 are opened, the second-stage buffer mechanism 21 is used for receiving the first vacuum desorption gas and low-pressure desorption gas, and the first-stage xenon separation column B6 is used for adsorbing the first-stage xenon separation column A5 and desorbing the second-stage adsorption for 40min, or the control valve A, the first-stage xenon separation column A5, the valve F, the second mass flow controller 71, the valve J, the first-stage xenon separation column B6, the valve D, the valve L, the valve M, the first buffer group 211, the valve R, the second-stage xenon separation column 22, the valve Q and the pressure regulator I23 are opened, and the first-stage xenon separation column A5 is used for adsorbing the first-stage xenon separation column B6 and desorbing the second-stage adsorption for 40min;
Then the valve O, the first buffer group 211, the valve S, the second-stage xenon separation column 22, the valve R, the valve X, the third-stage xenon separation column 25 and the pressure controller II are controlled to open the carrier gas, and the second-stage desorption and third-stage adsorption are carried out for 30min; after the secondary desorption is completed, the control system controls the three-stage xenon separation column 25 to be cooled to the adsorption temperature;
then controlling a vacuum pump 8, a valve AC, a vacuumizing pipeline, a thermal conductivity detector TCD29, a valve B6 and a source chamber 27 gas circuit to suck the source chamber 27 to high vacuum, then controlling a heating three-stage heat preservation sleeve to a desorption temperature, performing three-stage vacuum desorption for 30min, setting the pressure of a pressure controller II to 98kPa, then opening a valve U and a valve W, and completing source preparation by a head space three-stage xenon separation column 25; then controlling an electric heating belt to heat the three-stage xenon separation column 25 to 350 ℃, stopping heating after vacuum activation for 30min, controlling the induced draft fan 10 to open and cool the three-stage xenon separation column 2530min, closing after reaching the adsorption temperature, and carrying out three-stage adsorption of the next sample;
then use twoThe coincidence measurement device 271 receives three-stage desorption gas in turn, and after the source preparation is completed, the radioactive xenon activity is measured; 20 minutes before the next sample gas is received in the source chamber 27, the control system controls the measurement of the radioactivity of the sample gas before the end, and transfers it to the archive flask 28 for storage, and uses the thermal conductivity detector TCD29 to analyze the total concentration of xenon, calculate the effective sampling volume from the stable xenon background in air, calculate the 133Xe activity concentration or minimum detectable activity concentration MDC in air in combination with the measured radioactivity 133Xe net activity.
The scope of protection of the present invention is not limited to the above embodiments and variations thereof. Conventional modifications and substitutions by those skilled in the art based on the content of the present embodiment fall within the protection scope of the present invention.

Claims (10)

1. The control method of the multimode enrichment analysis device for the xenon background is characterized by comprising the following steps of:
setting working parameters of a plurality of program control valves, a gas taking enrichment device, a plurality of stages of xenon separation columns, a refrigerator and a xenon separation column activation regeneration device of the device through a control system;
the refrigerating equipment in the refrigerator is controlled through the control system, the temperature of the refrigerator is kept between minus 28 ℃ and 18 ℃, the gas taking enrichment device is controlled to take gas for enrichment, constant components and granular substances in the air are removed, high-concentration product gas is obtained, and the high-concentration product gas enters the primary buffer mechanism;
controlling the first-stage xenon separation column A or the first-stage xenon separation column B to alternately work for first-stage purification and concentration, wherein one of the first-stage xenon separation column A or the first-stage xenon separation column B carries out first-stage forward pressure-increasing adsorption, and the other one carries out a first-stage low-pressure reverse desorption procedure; then controlling a program control valve connected with the primary buffer mechanism and the purification concentration unit to open a certain opening, so that product gas in the primary buffer mechanism is sent into a primary xenon separation column A or a primary xenon separation column B, controlling the discharge amount of a first mass flow controller to be lower than the air inflow of the valve, controlling the pressure in front of the primary xenon separation column A or the primary xenon separation column B to be higher than the pressure behind the column, discharging the adsorbed tail gas through the first mass flow controller to realize primary forward boost adsorption, and controlling the primary xenon separation column A or the primary xenon separation column B to perform a primary low-pressure reverse desorption process after the primary forward boost adsorption is finished;
When the primary low-pressure reverse desorption is completed, carrying out primary activation regeneration, vacuumizing a primary xenon separation column A or a primary xenon separation column B by controlling a vacuum pump, controlling an electric heating belt of a xenon separation column activation regeneration device to heat the primary xenon separation column A or the primary xenon separation column B to 250-350 ℃, maintaining the temperature for 40-180 min, stopping heating, then controlling an air door connected with a refrigerator to be opened, simultaneously controlling an induced draft fan to start, introducing low-temperature gas in the refrigerator into the xenon separation column activation regeneration device by the induced draft fan, and cooling the primary xenon separation column A or the primary xenon separation column B until the temperature is cooled to an adsorption temperature, thereby completing activation regeneration;
during secondary purification and concentration, first performing secondary forward boost adsorption, pushing primary desorption gas in a secondary buffer mechanism to enter a secondary xenon separation column through primary adsorption tail gas of the primary xenon separation column A or the primary xenon separation column B, performing secondary adsorption and purification for 10-40 min, setting the discharge pressure or flow of a first pressure regulator to be smaller than the pressure or flow of the secondary xenon separation column when air is taken in, thereby raising the adsorption tail pressure of the secondary xenon separation column, and performing secondary forward boost adsorption;
after the secondary forward boost adsorption is finished, controlling a vacuum pump to vacuumize the secondary xenon separation column, reducing the pressure in the secondary xenon separation column to 5-20 Pa, stopping vacuumizing, and then controlling an electric heating belt to heat the secondary xenon separation column to 120-220 ℃; then controlling a vacuum pump to vacuumize the three-stage buffer mechanism to the limit vacuum of 1-5 Pa; controlling the connection pipeline of the second-stage xenon separation column and the third-stage buffer mechanism to be communicated, controlling the maintenance temperature of the second-stage xenon separation column to be 10-60 min, and controlling the first-stage adsorption tail gas to be introduced into the second-stage xenon separation column to push the second-stage desorption gas in the second-stage xenon separation column into the third-stage buffer mechanism until the pressure sensor detects that the pressure in the third-stage buffer mechanism reaches a specified pressure value or is not raised any more, and completing the second-stage reverse low-pressure desorption;
After the secondary reverse low-pressure desorption is finished, controlling a vacuum pump to vacuumize the secondary xenon separation column, controlling an electric heating belt of an activation regeneration device of the secondary xenon separation column to heat the secondary xenon separation column to an activation temperature of 280-350 ℃, controlling the electric heating belt to stop heating after maintaining the temperature for 40-180 min, then controlling an air door connected with a refrigerator in the activation regeneration device of the secondary xenon separation column to be opened, simultaneously controlling an induced draft fan to start, introducing low-temperature gas in the refrigerator into the secondary xenon separation column to cool through the induced draft fan until a temperature sensor detects that the secondary xenon separation column is cooled to a set adsorption temperature, and completing activation regeneration;
then controlling the first-stage adsorption tail gas to push the second-stage desorption gas stored in the third-stage buffer mechanism into the third-stage xenon separation column for three-stage purification and concentration, and controlling the discharge pressure or flow of the second pressure of the pressure regulator to be smaller than the pressure or flow of the air inlet of the third-stage xenon separation column, so as to raise the adsorption pressure of the third-stage xenon separation column, and discharging the tail gas subjected to pressure-raising adsorption by the third-stage xenon separation column through the second pressure regulator to finish three-stage forward pressure-raising adsorption;
after the three-stage forward boost adsorption is finished, controlling a vacuum pump to vacuumize the three-stage xenon separation column, reducing the pressure of the three-stage xenon separation column to 2-25 Pa, controlling an electric heating belt in an activation regeneration device of the three-stage xenon separation column to heat the three-stage xenon separation column to 120-220 ℃, and controlling the vacuum pump to vacuumize a source chamber to 2-5 Pa; then, connecting the three-stage xenon separation column and a source chamber to carry out high-temperature desorption and vacuum diffusion of the three-stage xenon separation column, and maintaining the temperature for 10-60 min; then controlling the three-stage buffer mechanism to be communicated with the three-stage xenon separation column, and pushing vacuum desorption gas and re-desorption gas in the three-stage xenon separation column to a source chamber to complete three-stage low-pressure reverse desorption source preparation;
After the three-stage low-pressure reverse desorption is completed, controlling a vacuum pump to vacuumize the three-stage xenon separation column, controlling an electric heating belt to heat the three-stage xenon separation column to 280-350 ℃, maintaining the temperature for 40-180 min, and stopping heating; then controlling an air door in an activation regeneration device of the three-stage xenon separation column to be opened, controlling a draught fan to be opened, introducing low-temperature gas in a refrigerator into the activation regeneration device by the draught fan, cooling the three-stage xenon separation column until a temperature sensor detects that the two-stage xenon separation column is cooled to a set adsorption temperature, and completing activation regeneration; after the source is manufactured, throughMeasuring the activity of the radioactive xenon in the source chamber in accordance with the measuring device; then the vacuum pump is controlled to vacuumize a plurality of archives, the source room, the thermal conductivity detector TCD and the archives are communicated after vacuumization, the sample gas in the sample source room is transferred to the archives for storage, and the total concentration of xenon is analyzed through the thermal conductivity detector TCD after pressure balance.
2. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: when the gas taking enrichment device takes gas enrichment, an air compressor of the gas taking enrichment device is controlled to convey air to a coarse filter through a pipeline, the air enters a cold dryer after passing through the coarse filter, the air is conveyed to a filter assembly through the cold dryer to be subjected to multistage filtration, and then the air is conveyed into a polyimide hollow fiber membrane separator to remove constant components in the air, so that high-concentration product gas is obtained.
3. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: when the first-stage forward boost adsorption is performed, the control system controls the valve A or the valve B to be opened, so that the product gas in the first-stage buffer mechanism enters the first-stage xenon separation column A or the first-stage xenon separation column B; simultaneously controlling the valve F or the valve G and the first mass flow controller to be opened, and controlling the pressure of the adsorption tail gas through the first mass flow controller to enable the first-stage xenon separation column A or the first-stage xenon separation column B to carry out supercharging adsorption; the first-stage xenon separation column A and the first-stage xenon separation column B alternately perform uninterrupted continuous gas-taking adsorption on the product gas.
4. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: before the first-stage low-pressure reverse desorption, a vacuum pump is controlled to vacuumize a first-stage xenon separation column A or a first-stage xenon separation column B, the pressure in the column is reduced, when the pressure in the column reaches a set pressure value, the pressure value in the column is fed back to a control system by a pressure sensor, and the control system controls a vacuum pump and a vacuumizing valve path of the first-stage xenon separation column A or the first-stage xenon separation column B to be closed; then controlling an electric heating belt to heat the first-stage xenon separation column A or the first-stage xenon separation column B to 120-220 ℃, and feeding back a temperature signal to a control system when a temperature sensor detects that the temperature reaches a set value; the control system controls the vacuum pump to vacuumize the secondary buffer mechanism, when the pressure sensor feeds back a signal of the secondary buffer mechanism at the limit negative pressure to the control system, the control system controls the vacuum pump to stop vacuuming, then controls a low-pressure reverse desorption pipeline of the primary xenon separation column A or the primary xenon separation column B to be communicated with the secondary buffer mechanism, maintains the temperature of the primary xenon separation column A or the primary xenon separation column B for 10-60 min for high-temperature vacuum desorption, and then pushes vacuum desorption gas and low-pressure desorption gas in the primary xenon separation column B or the primary xenon separation column A into the secondary buffer mechanism through an adsorption tail gas recycling pipeline of the primary xenon separation column A or the primary xenon separation column B until the pressure sensor detects that the pressure value of the secondary buffer mechanism reaches a specified pressure value or the pressure is not increased any more, and the secondary forward boost adsorption and the primary activation regeneration are prepared;
When the first-stage xenon separation column A or the first-stage xenon separation column B is vacuumized before reverse desorption, a control system controls a vacuum pump, a valve AC, a valve K, a valve E or a vacuum pump, a valve R, a valve L and a valve H to open a vacuumizing pipeline of the first-stage xenon separation column A or the first-stage xenon separation column B, and controls a valve D, a valve G and a valve J to close or controls a valve C, a valve F and a valve S to close when vacuumizing is completed, and then the vacuum pump and a program-controlled valve on the corresponding vacuumizing pipeline are closed;
when the first-stage xenon separation column A or the first-stage xenon separation column B is reversely desorbed, a control system controls a vacuum pump, a valve AC, a valve M and a valve N to open a vacuumizing pipeline forming a secondary buffer mechanism, so that the secondary buffer mechanism is vacuumized, wherein the control valve K, the valve L, the valve O, the valve P and the valve I are closed during vacuumizing, and the vacuum pump and the corresponding program-controlled valve are closed after vacuumizing; then the control system controls the valve B, the valve G, the mass flow controller II, the valve I, the valve C, the valve K, the valve M, the valve N or the valve A, the valve F, the mass flow controller II, the valve J, the valve D, the valve L, the valve M and the valve N to be opened, controls the valve E and the valve H to be closed, forms a reverse desorption pipeline of the first-stage xenon separation column A or the first-stage xenon separation column B, and pushes desorption gas in the first-stage xenon separation column A or the first-stage xenon separation column B into the second-stage buffer mechanism and then closes the corresponding program control valve;
When the first-stage xenon separation column A or the first-stage xenon separation column B is activated and regenerated, a control system is used for controlling a vacuum pump, a valve R, a valve K, a valve E or controlling the vacuum pump, a valve R, a valve L and a valve H to be opened, a control valve D, a valve G and a valve J to be closed or a control valve C, a valve F and a valve S to be closed, vacuumizing the first-stage xenon separation column A or the first-stage xenon separation column B, and controlling the vacuum pump and the corresponding program-controlled valve to be closed after vacuumizing is finished.
5. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: the method comprises the steps that during secondary forward boost adsorption, a control system controls a valve O, a valve N, a valve P, a valve Q and a first pressure regulator to be opened, adsorption tail gas in a secondary buffer mechanism is pushed into a secondary xenon separation column through adsorption tail gas of a primary xenon separation column A or a primary xenon separation column B, the discharge pressure or flow of the first pressure regulator is controlled to be smaller than the pressure or flow of gas when the first pressure regulator enters the secondary xenon separation column, so that secondary forward boost adsorption is performed, and a program-controlled valve at a corresponding position is controlled to be closed after adsorption is completed;
when the second-stage low-pressure reverse desorption is performed, a control system is used for controlling a vacuum pump, a valve AC, a valve AD and a valve R to be opened so as to vacuumize the second-stage xenon separation column, and the vacuum pump and a program-controlled valve at a corresponding position are closed after vacuumization; then the control system controls the vacuum pump, the valve AD, the valve X and the valve V to open, vacuumizes the three-stage buffer mechanism to a limit negative pressure state, and then closes the vacuum pump and the program-controlled valve at the corresponding position;
When the adsorption tail gas of the first-stage xenon separation column A or the first-stage xenon separation column B pushes the low-pressure desorption gas in the second-stage xenon separation column into the third-stage buffer mechanism, the control system controls the valve O, the valve S, the valve R and the valve U to be opened, and the adsorption tail gas of the first-stage xenon separation column A or the first-stage xenon separation column B pushes the low-pressure desorption gas in the second-stage xenon separation column into the third-stage buffer mechanism until the pressure in the third-stage buffer mechanism reaches a specified pressure value or is not raised any more, and then program-controlled valves at corresponding positions are closed to complete the second-stage low-pressure reverse desorption;
when the secondary xenon separation column is activated, regenerated and vacuumized, the vacuum pump, the valve M and the valve S are controlled to be opened by the control system, then the secondary xenon separation column is vacuumized, and the vacuum pump and the corresponding program-controlled valve are controlled to be closed after the vacuumizing is completed.
6. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: during the three-stage forward boost adsorption, a control system controls a valve T, a valve U and a valve V to be opened, and the adsorption tail gas of a first-stage xenon separation column A or a first-stage xenon separation column B pushes the second-stage desorption gas in a three-stage buffer mechanism into a three-stage xenon separation column for three-stage adsorption; when three-stage reverse desorption vacuumizing is performed, the control system controls the vacuum pump, the valve AC, the valve AD and the valve W to be opened, and the vacuum pump and the corresponding program control valve are closed after the vacuumizing is completed; when the three-stage xenon separation column is activated, regenerated and vacuumized, the control system controls the vacuum pump, the valve AC, the valve AD and the valve X to be opened, namely, the three-stage xenon separation column is vacuumized, and after the vacuumizing is completed, the control system controls the vacuum pump and the corresponding program-controlled valve to be closed.
7. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: when the source chamber is vacuumized, the control system controls the vacuum pump, the valve AC and the valve Z to vacuumize the source chamber, and the vacuum pump and the program control valve at the corresponding position are closed after the vacuumization is completed.
8. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: when the archive bottle is vacuumized, the control system controls the vacuum pump, the valve AC, the valve AE and the valve AB to be opened, then vacuumizes a plurality of archive bottles, and after vacuumization is finished, controls the vacuum pump, the valve AC, the valve AE and the valve AB to be closed; when xenon in the source room is transferred to the file bottle, the transfer can be completed by controlling the opening of the valve AB and the valve Z through the control system.
9. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: the method also comprises a control method for re-concentrating the sample gas in the archive bottle, and the control method is as follows: the first buffer group of the secondary buffer mechanism is vacuumized by controlling the vacuum pump, the valve AC and the valve M to be opened, the vacuum pump and the corresponding program-controlled valve are closed after the vacuumization is completed, then the valve AB and the valve AE are controlled to be opened, the valve AB is closed after xenon in the archives is transferred to the first buffer group, and then the archives are transferred to the archives for preservation after the secondary purification and the tertiary purification, so that the reconcentration of the sample gas is completed.
10. The method for controlling a multimode enrichment analysis device for xenon background according to claim 1, wherein: the control method for high-frequency rapid sampling monitoring is also included, and the specific method is as follows: the working time of one working period of the multi-mode enrichment analysis device is set, the gas taking enrichment device is controlled to take gas for pre-enrichment and then is conveyed to the first-stage xenon separation column A or the first-stage xenon separation column B, and the control system controls the first-stage xenon separation column A and the first-stage xenon separation column B to alternately carry out gas adsorption and separation column desorption regeneration of the pure nitrogen membrane product rich in xenon; when the first-stage xenon separation column A is adsorbed, the control system controls the first-stage xenon separation column B to carry out desorption for 20-40 min, activation for 40-60 min and cooling for 20-40 min; when the first-stage xenon separation column B is adsorbed, the control system controls the first-stage xenon separation column A to carry out desorption for 20-40 min, activation for 40-60 min and cooling for 20-40 min; the control system controls the valve B, the first-stage xenon separation column B, the valve G, the second mass flow controller, the valve I, the valve C, the valve K, the valve M, the valve R, the valve Q and the pressure regulator I to be opened for carrying out the first-stage xenon separation column B to adsorb the first-stage xenon separation column A for desorbing the second-stage adsorption for 20 to 40 minutes, or controls the valve A, the valve F, the second mass flow controller, the valve J, the valve D, the valve L, the valve M, the valve R, the valve Q and the pressure regulator I to be opened for carrying out the first-stage xenon separation column A to adsorb the first-stage xenon separation column B for desorbing the second-stage adsorption for 20 to 40 minutes; then controlling the valve O, the valve S, the valve R, the valve X and the pressure regulator II to be opened, introducing carrier gas into the three-stage xenon separation column, and carrying out secondary desorption and three-stage adsorption for 10-40 min; after the secondary desorption is finished, controlling an induced draft fan and an on-off device to be opened, and introducing cold air of a refrigerator seed through the induced draft fan to cool the three-stage xenon separation column to the adsorption temperature; then the control system controls the vacuum pump, the valve R and the valve Z to be opened to vacuumize the source chamber, and the vacuum pump is closed after vacuumization; then the control system controls the three-stage xenon separation column to carry out vacuum desorption for 10-40 min, then controls the valve U and the valve W to be opened, and the three-stage xenon separation column is emptied and then closed after the source preparation is completed; then control three stages The xenon separation column is activated in vacuum for 40-60 min and then cooled for 40-60 min until reaching the adsorption temperature, and the next sample is subjected to three-stage adsorption; the simultaneous control system controls twoThe coincidence measuring device is used for receiving three-level desorption gas in a round manner, and measuring the activity of radioactive xenon after the source preparation is completed; 20-30 min before the next sample gas is received in the source chamber, the control system controls the measurement of the radioactivity of the sample gas before the end of the measurement and transfers the measurement to an archive bottle for storage, the total concentration of xenon is analyzed by a thermal conductivity detector TCD, the effective sampling volume is calculated by the stable xenon background in the air, and the 133Xe activity concentration or the minimum detectable activity concentration MDC in the air is calculated by combining the actual measured radioactivity 133Xe net activity; after the number of the samples is 40-80, the control system controls the adsorption columns at each level to perform vacuum activation for 2-3 h, and cooling for 20-40 min to complete regeneration.
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