CN112557157A - Method for separating, purifying and collecting xenon in air sample based on specific device - Google Patents

Method for separating, purifying and collecting xenon in air sample based on specific device Download PDF

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CN112557157A
CN112557157A CN202110221952.6A CN202110221952A CN112557157A CN 112557157 A CN112557157 A CN 112557157A CN 202110221952 A CN202110221952 A CN 202110221952A CN 112557157 A CN112557157 A CN 112557157A
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column
xenon
transfer
separation
collection
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CN112557157B (en
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王茜
翁蔡平
侯建平
罗飞
向永春
古梅
张伟
田阔
刘强
龚有进
吴晓楠
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/405—Concentrating samples by adsorption or absorption
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/167—Measuring radioactive content of objects, e.g. contamination

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Abstract

The invention discloses a method for separating, purifying and collecting xenon in an air sample based on a specific device, which comprises the following steps: a) activating and regenerating the column; b) transferring xenon in the pre-concentrated air sample; c) and (3) separating, purifying and collecting xenon in the air sample in the transfer column. The invention adopts high-low temperature transfer technology, peak cutting technology and micro-flow control technology, realizes the rapid and efficient transfer, purification, separation and collection of milliliter-scale xenon in hectolitre-scale pre-concentration air samples obtained from cubic meter-scale air samples, meets the measurement requirement of a gas detector on a small amount of radioactive xenon in a large amount of air samples, and solves the urgent need of monitoring radioactive xenon isotopes.

Description

Method for separating, purifying and collecting xenon in air sample based on specific device
Technical Field
The invention belongs to the technical field of radioactive xenon monitoring, and particularly relates to a method for separating, purifying and collecting xenon in an air sample based on a specific device.
Background
Because the content of radioactive xenon isotopes in the atmosphere is very low, samples meeting the radioactive measurement requirements can be obtained only by sampling, adsorbing and enriching xenon in the atmosphere and then separating and purifying. At present, the international xenon monitoring system adopts different technical lines to separate and purify adsorbed and enriched xenon, for example, multi-stage active carbon is adopted to separate and purify the adsorbed and enriched xenon, and finally, a sample is collected in a low-temperature active carbon column; or separating with secondary activated carbon, purifying with caustic soda asbestos silica gel and 5A molecular sieve column, and collecting the sample in low temperature activated carbon column; or after the 4A molecular sieve is adopted for preliminary purification, the active carbon column is used for separation, and then the 3A molecular sieve and the 5A molecular sieve are used for further purification; or separating and purifying with three-stage active carbon column. However, the separation, purification and collection techniques used in the above-mentioned techniques all have the disadvantages of large volume of the separation and purification device, complicated separation and purification process and long time required.
Disclosure of Invention
In view of the above, the present invention is directed to a method for separating, purifying and collecting xenon in an air sample based on a specific device, which has the characteristics of being suitable for efficiently and rapidly transferring, purifying, separating and collecting a small amount of xenon in a large amount of air samples.
The invention specifically adopts the following technical scheme:
a method for separating, purifying and collecting xenon in an air sample based on a specific device is characterized in that the specific device comprises: the device comprises a transfer unit, a separation and purification unit, a collection unit and auxiliary units, wherein the transfer unit is connected with the separation and purification unit, the separation and purification unit is connected with the collection unit, and the auxiliary units are respectively connected to the transfer unit, the separation and purification unit and the collection unit;
the transfer unit comprises a high-low temperature box of a transfer column and the transfer column arranged in the high-low temperature box of the transfer column, and refrigerant conveying pipes and heating pipes are tightly arranged on two sides of the transfer column;
the separation and purification unit comprises a thermal conductivity detection module, a reserved column heating furnace, a purification column heating furnace, a separation column heating furnace, and reserved columns, purification columns and separation columns which are respectively arranged in the reserved column heating furnace, the purification column heating furnace and the separation column heating furnace;
the collecting unit comprises a collecting column heating furnace and a collecting column arranged in the collecting column heating furnace;
the auxiliary unit comprises a vacuum pump connected with the transfer unit, the separation and purification unit and the collection unit, a steel bottle connected with the flow washing gas and a file bottle connected with the collection column;
the method specifically comprises the following steps: a) activating and regenerating the column; b) transferring xenon in the pre-concentrated air sample; c) separating, purifying and collecting xenon in an air sample in the transfer column;
wherein, the step a) comprises the following steps:
a1) introducing carrier gas and flowing through a mass flow controller MF1, and setting the flow of a mass flow controller MF 1;
a2) switching on a power supply of the separation, purification and collection device, and switching a valve to discharge carrier gas from a valve V7 after the carrier gas flows through the thermal conductivity detection module, the transfer column, the purification column, the separation column and the collection column;
a3) respectively setting the activation temperatures of the transfer column, the purification column, the separation column and the collection column, and heating the transfer column, the purification column, the separation column and the collection column; after reaching the respective activation temperature of the transfer column, the purification column, the separation column and the collection column, preserving the heat until the activation is complete, and stopping heating;
a4) cooling the temperature of the transfer column, the purification column, the separation column and the collection column to room temperature, switching valves to enable the transfer column, the purification column, the separation column and the collection column to be in a closed state, and preparing to enter a transfer process of xenon in the pre-concentrated air sample;
the step b) comprises the following steps:
b1) starting refrigeration of a high-low temperature box of the transfer column, resetting the flow rate of a mass flow controller MF1, and starting a power supply of a thermal conductivity detection module to be in a state to be analyzed;
b2) when the temperature of the transfer column reaches the set xenon adsorption temperature, the three-way valve TV2 is in a state of connecting the external pre-concentrated air sample with the transfer column, the xenon in the external pre-concentrated air sample is adsorbed to the transfer column, the three-way valve TV3 is switched to an emptying state so as to completely adsorb the xenon in the external pre-concentrated air sample into the transfer column, meanwhile, 90% -95% of non-xenon gas components in the external pre-concentrated air sample are emptied, and the rest of the non-xenon gas components are adsorbed in the transfer column; b3) the refrigeration of a high-temperature box and a low-temperature box of the transfer column is closed, three-way valves TV2 and TV3 are switched to be connected with a six-way valve SV2, and the flow of separating, purifying and collecting xenon in an air sample entering the transfer column is prepared;
the step c) specifically comprises the following steps:
c1) when the temperature of the transfer column reaches-40 ℃ to-10 ℃, alternately switching on and off the valves V6 and V16, evacuating a pipeline by using a vacuum pump, carrying out pipeline buffer type pressure relief on the transfer column, and then closing the valves V6 and V16;
communicating the transfer column with a valve V7 through a four-way valve FV1, an FV2 and a six-way valve SV3, washing the transfer column with high-purity helium carrier gas flow, and starting online monitoring of effluent gas components of the transfer column by a thermal conductivity detection module to ensure that 90-95% of non-xenon gas components in the transfer column in the step b 2) are evacuated;
c3) setting the desorption temperature of the transfer column, switching four-way valves FV1 and FV2, connecting the purification column and the separation column in series after the transfer column in turn, purifying xenon and the residual non-xenon gas component in the transfer column through the purification column, and separating through the separation column; the thermal conductivity detection module continuously monitors the effluent gas components of the purification column and the separation column on line, and completely empties the residual non-xenon gas components;
c4) when the transfer column reaches the desorption temperature, switching a six-way valve SV3 to connect the collection column in series to the position where the measurement component of the thermal conductivity detection module flows out, and collecting the xenon separated in the step c 3) into the collection column;
c5) when the thermal conductivity detection module monitors that the xenon component is completely collected on line, the collection is stopped and the heating of the transfer column is stopped, so that the separation, purification and collection of xenon in the air sample of the transfer column are completed.
Further, the method comprises the following steps:
d) and (3) a desorption and inflation process of the xenon sample in the collecting column. The step d) comprises the following steps:
d1) switching a three-way valve TV4, enabling the flow washing gas to flow through a mass flow controller MF2, opening valves V8, V13 and V15, alternately switching valves V9 and V16, opening a vacuum pump to enable the vacuum pump to evacuate a pipeline, relieving pressure of a collecting column to be below 1kPa, then closing the vacuum pump, and closing valves V8, V9, V13, V15 and V16;
d2) setting the desorption temperature of a collection column, heating to the desorption temperature, keeping the temperature, setting the flow rate of a mass flow controller MF2, opening valves V8, V9 and V12, slowly washing the collection column by flowing and washing gas, filling high-purity xenon in the collection column into a gas detector, enabling the pressure of a pressure sensor P5 to slowly rise at the speed of hundred pascals per second, closing valves V8, V9 and V12 when a pressure sensor P5 shows that the pressure is 94-96 kPa, stopping heating the collection column, and ending the filling.
Further, in the steps b 2) to b 3) and the steps c 2) to c 5), the high-low temperature transfer technology is adopted to transfer xenon in the hectolitre level pre-concentrated air sample from the outside and obtained from the cubic meter level air sample, and the specific processes of rapidness, high efficiency and easy operation are as follows: the transfer post is the nonrust steel pipe of built-in active carbon, nonrust steel pipe is installed in the high low temperature case of transfer post, the high low temperature incasement of transfer post is equipped with a pair of U type groove aluminum plate, closely laminates tightly with two U type groove aluminum plates with the refrigerant conveyer pipe and the heating pipe of transfer post both sides with transfer post and distribution and presss from both sides tightly, and wherein the low temperature conduction oil is chooseed for use to the refrigerant, and the heating pipe adopts electrical heating for the refrigeration and the intensification of transfer post are simple easily obtained, convenient operation.
Further, in the step d 2), the desorption temperature is 300-350 ℃.
Further, in the step d 2), the flow rate is 1-5 ml/min.
The method for separating, purifying and collecting xenon in the air sample, which is developed by the invention, adopts a high-low temperature transfer technology, a peak cutting technology and a micro-flow control technology, and solves the problems of complex processing process and long time consumption of a small amount of xenon in the cubic meter-level air sample in the traditional technology. The method for separating, purifying and collecting the xenon in the air sample can transfer, purify, separate and collect the milliliter xenon in hundred liters of samples pre-concentrated to the air sample of ten cubic meters within 1 hour, meets the requirement of a gas detector on sample measurement, realizes the quick and efficient sampling of the xenon in the air sample of the cubic meter level, and provides a solid technical support for the emergency monitoring of the radioactive xenon by the radioactive xenon isotope sampling monitoring with short response time and large dynamic range.
Drawings
FIG. 1 is a schematic diagram of a specific apparatus used in the method for separating, purifying and collecting xenon in an air sample according to the present invention;
FIG. 2 is a flow chart of the method for separating, purifying and collecting xenon in an air sample according to the present invention;
FIG. 3 is a flow chart of a separation, purification and collection method for xenon in an air sample comprising a desorption and gas filling process for a xenon sample in a collection column
In the figure, 1, a thermal conductivity detection module 2, a reserved column 3, a transfer column 4, a purification column 5, a separation column 6, a collection column 7, a reserved column heating furnace 8, a high-low temperature box 9 of the transfer column, a purification column heating furnace 10, a separation column heating furnace 11, a collection column heating furnace 12, a vacuum pump 13, a small steel cylinder 14 and a filing bottle.
Detailed Description
The present invention will be described in further detail with reference to the following examples and accompanying FIGS. 1 to 3.
As shown in FIG. 2, the method for separating, purifying and collecting xenon in an air sample based on a specific device comprises the following steps:
a) activation regeneration treatment of column
The step a) specifically comprises the following steps:
a1) introducing carrier gas and flowing through a mass flow controller MF1, and setting the flow rate of a mass flow controller MF 1;
a2) switching on the power supply of the separation, purification and collection device, and switching the valve to discharge the carrier gas from the valve V7 after the carrier gas flows through the transfer column 3, the purification column 4, the separation column 5 and the collection column 6;
a3) heating temperatures of the transfer column 3, the purification column 4, the separation column 5 and the collection column 6 are respectively set, and carrier gas is introduced, heated, activated and regenerated to the transfer column 3, the purification column 4, the separation column 5 and the collection column 6; after reaching the temperature required by the activation regeneration of the transfer column 3, the purification column 4, the separation column 5 and the collection column 6 respectively, preserving the heat until the activation is complete, and stopping heating;
a4) and when the temperature is reduced to the room temperature, switching the valves to enable the transfer column 3, the purification column 4, the separation column 5 and the collection column 6 to be in a closed state, and preparing to enter a transfer process of the xenon in the pre-concentrated air sample.
b) Transfer of xenon from a preconcentrated air sample
The step b) comprises the following steps:
b1) starting refrigeration of a high-low temperature box 8 of the transfer column, resetting the flow rate of a mass flow controller MF1, and starting a power supply of the thermal conductivity detection module 1 to be in a state to be analyzed;
b2) when the temperature of the transfer column 3 reaches a designated temperature, the three-way valve TV2 is in a state of connecting a hectoliter-level pre-concentration air sample obtained from a cubic meter-level air sample from the outside with the transfer column 3, xenon in the pre-concentration air sample from the outside is adsorbed to the transfer column, the three-way valve TV3 is switched to an emptying state so as to completely adsorb xenon in the pre-concentration air sample from the outside into the transfer column, meanwhile, 90% -95% of non-xenon gas components in the pre-concentration air sample from the outside are emptied, and the rest of non-xenon gas components are adsorbed in the transfer column;
b3) after the transfer of the hectolitre pre-concentrated air sample from the outside, which is obtained from the cubic meter-level air sample, is completed, the refrigeration of the high-low temperature box 8 of the transfer column is turned off, and the three-way valves TV2 and TV3 are switched to the state connected to the six-way valve SV 2. Thus completing the transfer of xenon in the hectoliter level pre-concentration air sample and preparing to enter the flow of separation, purification and collection of xenon in the air sample in the transfer column 3.
c) Separation, purification and collection of xenon from air samples in transfer columns
The step c) specifically comprises the following steps:
c1) when the temperature of the transfer column 3 reaches-40 ℃ to-10 ℃, alternately switching on and off the valves V6 and V16, evacuating the pipeline by using a vacuum pump 12, carrying out pipeline buffer type pressure relief on the transfer column 3, and closing the valves V6 and V16;
c2) setting the heating temperature of the transfer column 3 to be 0 ℃, alternately switching on and off the valves V6 and V16 again, evacuating the pipeline by using the vacuum pump 12, continuing to perform pipeline buffer type pressure relief on the transfer column 3, then switching over the six-way valve SV2 to enable the transfer column to be communicated with the valve V7 through the four-way valve FV1, FV2 and the six-way valve SV3, washing the transfer column by using high-purity helium carrier gas flow, and starting online monitoring on the effluent gas component of the transfer column by using a thermal conductivity detection module to ensure that 90% -95% of the non-xenon gas component in the transfer column in the step b 2) is evacuated;
c3) setting the desorption temperature of the transfer column 3, switching four-way valves FV1 and FV2, connecting a purification column and a separation column in series after the transfer column in turn, purifying xenon and the rest non-xenon gas components in the transfer column through the purification column, and separating through the separation column; the thermal conductivity detection module continuously monitors the effluent gas components of the purification column and the separation column on line, and completely empties the residual non-xenon gas components;
c4) when the transfer column reaches the desorption temperature, switching a six-way valve SV3 to connect the collection column in series to the position where the measurement component of the thermal conductivity detection module flows out, and collecting the xenon separated in the step c 3) into the collection column;
c5) when the thermal conductivity detection module monitors that the xenon component is completely collected on line, the collection is stopped and the heating of the transfer column is stopped, so that the separation, purification and collection of xenon in the air sample of the transfer column are completed.
Further, as shown in fig. 3, the method further includes the steps of:
d) a desorption and inflation process for collecting a xenon sample in the column, wherein the step d) specifically comprises the following steps:
d1) switching a three-way valve TV4 to enable the flow washing gas to flow through a mass flow controller MF2, opening valves V8, V13 and V15, alternately switching valves V9 and V16, opening a vacuum pump to enable the vacuum pump to evacuate a pipeline, and relieving pressure of a collecting column to be below 1kPa to ensure that impurity gas in the inflation pipeline is minimum and influence on subsequent measurement is minimum; then the vacuum pump is closed, and the valves V8, V9, V13, V15 and V16 are closed;
d2) setting the desorption temperature of the collection column 6, heating to the desorption temperature, keeping the temperature, setting the flow rate of a mass flow controller MF2, opening valves V8, V9 and V12, slowly washing the collection column 6 by flowing washing gas, filling the high-purity xenon in the collection column 6 into a gas detector, closing valves V8, V9 and V12 when a pressure sensor P5 shows that the pressure sensor is 94-96 kPa, stopping heating the collection column, and ending inflation. The flow rate of xenon gas detector(s) is used for subsequent measurements of xenon by the gas detector(s). The step d) of the invention adopts a micro-flow control technology to realize the high-efficiency transfer of the pure xenon sample.
Further, in the steps b 2) to b 3) and the steps c 2) to c 5), the high-low temperature transfer technology is adopted to transfer xenon in the hectolitre level pre-concentrated air sample from the outside and obtained from the cubic meter level air sample, and the specific processes of rapidness, high efficiency and easy operation are as follows: the transfer column 3 is a phi 1/2U-shaped stainless steel tube filled with activated carbon and is arranged in a high-low temperature box 8 of the transfer column, the high-low temperature box 8 of the transfer column is specially used for rapid heating and refrigeration of the transfer column 3, a pair of U-shaped groove aluminum plates are arranged in the transfer column, the transfer column 3 and refrigerant conveying pipes and heating pipes which are distributed on two sides of the transfer column 3 are tightly attached and clamped by two U-shaped groove aluminum plates, wherein low-temperature heat conduction oil is selected for the refrigerant, and the heating pipes are electrically heated, so that the required high and low temperature of the transfer column 3 in the transfer process is rapidly and easily obtained. The invention adopts a high-low temperature transfer technology, realizes the requirements of low-temperature adsorption, high-temperature desorption and transfer of xenon in a hectolitre level pre-concentrated air sample from an external cubic meter level air sample within the range of-30 ℃ to 300 ℃, can also accurately control the desorption temperature, completely desorbs xenon adsorbed by a transfer column, and does not desorb radon possibly existing, thereby not only meeting the requirement of xenon adsorption capacity, but also ensuring that the adsorption, desorption and transfer operations of xenon are simple and easy, effectively reducing the filling amount of active carbon of the transfer column 3, reducing the volume of a high-low temperature box 8 of the transfer column, reducing the power consumption and saving the processing time of the whole flow.
In the steps c 2) to c 4), the thermal conductivity detection module 1 is used for monitoring the component condition of the effluent gas on line, the peak cutting technology is adopted, a large amount of non-xenon gas components in the pre-concentrated air sample can be evacuated in time by switching valves according to the outflow sequence and retention time of different components in the pre-concentrated air sample through the transfer column 3, the purification column 4 and the separation column 5, so that the aims of quickly and efficiently transferring, purifying, separating and collecting milliliter-level xenon in the hectolitre-level pre-concentrated air sample obtained from the cubic meter-level air sample are fulfilled, and the preparation is made for the retransfer and measurement of the xenon sample in the subsequent collection column.
Further, in the step d 2), the desorption temperature is 300-350 ℃.
Further, in the step d 2), the flow rate is 1-5 ml/min.
The peak cutting technology adopted by the thermal conductivity detection module 1 can timely evacuate a large amount of non-xenon gas components in the sample, and the specific process is as follows: firstly, in the process of transferring a hectolitre-level pre-concentrated air sample from an external cubic meter-level air sample to a transfer column 3 at low temperature, directly exhausting a large amount of non-xenon gas components in the pre-concentrated air sample, starting a vacuum pump 12 after the low-temperature transfer is finished, performing pipeline buffer type pressure relief on the transfer column 3 at low temperature, connecting the transfer column 3 into a chromatographic main flow path, and monitoring the gas outflow component of the transfer column on line by a thermal conductivity detection module 1; washing the heated transfer column 3 with high-purity helium carrier gas, directly emptying a large amount of non-xenon gas components adsorbed in the transfer column, switching four-way valves FV1 and FV2 when a chromatogram shows that an air peak in an air sample returns to a chromatographic baseline, sequentially connecting a purification column 4 and a separation column 5 in series behind the transfer column 3, further purifying and separating xenon in the transfer column and the rest non-xenon gas sample through the purification column 4 and the separation column 5 under normal temperature conditions, adsorbing water vapor and carbon dioxide, separating the xenon from the non-xenon components, and continuously emptying the non-xenon gas components directly; then, when the transfer column 3 is at the xenon desorption temperature, the collection column 6 is connected in series to the measuring component outflow part of the thermal conductivity detection module 1 by switching the six-way valve SV3, the collection column 6 is used for collecting xenon in the air sample after passing through the purification column and the separation column, and finally the residual non-xenon gas components are completely emptied; when the thermal conductivity detection module 1 detects that the effluent component xenon peak of the transfer column 3 returns to the chromatographic baseline on line, the collection is stopped.
In the step d), a micro-flow control technology is adopted, so that the gas filling process of the high-purity xenon sample is accurately controlled, and the method specifically comprises the following steps: firstly, a pipeline is evacuated by a vacuum pump, and pipeline buffer type pressure relief is carried out on a collecting column, so that the impurity gas in an inflation pipeline is ensured to be minimum, and the influence on subsequent measurement is minimum; then, heating the collecting column to a desorption temperature, keeping the temperature, setting the flow of a mass flow controller MF2, adopting a micro-flow control technology, opening valves V8, V9 and V12, slowly washing the collecting column by flowing washing gas, filling high-purity xenon in the collecting column into a gas detector, enabling the pressure of a pressure sensor P5 to slowly rise at a speed of hundred pascals per second, closing V8, V9 and V12 when a pressure sensor P5 shows that the pressure is slightly lower than the normal pressure, stopping heating the collecting column, setting the flow rate of the mass flow controller MF2 to be 0, and enabling the xenon filled in the gas detector to be used for measuring the subsequent xenon. The use of micro-flow control technology not only ensures the sufficient desorption of xenon in the collecting column, but also can be fully filled into the gas detector, and meets the pressure use requirement of the gas detector.
The invention also provides a special device special for the method for separating, purifying and collecting xenon in the air sample, namely a separating, purifying and collecting device special for the method for separating, purifying and collecting xenon in the air sample, as shown in figure 1, in the figure, V1-V17 are ball valves, P1-P7 are pressure sensors, TV 1-TV 4 are three-way valves, FV 1-FV 2 are four-way valves, and SV 1-SV 3 are six-way valves, and specifically, the device comprises: the device comprises a transfer unit, a separation and purification unit, a collection unit and auxiliary units, wherein the transfer unit is connected with the separation and purification unit, the separation and purification unit is connected with the collection unit, and the auxiliary units are respectively connected to the transfer unit, the separation and purification unit and the collection unit;
the transfer unit comprises a high-low temperature box 8 of the transfer column and the transfer column 3 arranged in the high-low temperature box of the transfer column, and refrigerant conveying pipes and heating pipes are tightly arranged on two sides of the transfer column 3;
the separation and purification unit comprises a thermal conductivity detection module 1, a reserved column heating furnace 7, a purification column heating furnace 9, a separation column heating furnace 10, and a reserved column 2, a purification column 4 and a separation column 5 which are respectively arranged in the reserved column heating furnace, the purification column heating furnace and the separation column heating furnace;
the collecting unit comprises a collecting column heating furnace 11 and a collecting column 6 arranged in the collecting column heating furnace;
the auxiliary units comprise a vacuum pump 12 connected with the transfer unit, the separation and purification unit and the collection unit, a small steel bottle 13 connected with the flow washing gas and a storage bottle 14 connected with the collection column.
Furthermore, the thermal conductivity detection module 1 works on the principle that different gas components and concentrations have different thermal conductivity coefficients with the carrier gas, the change of the heat conductivity coefficient can cause the change of the output signal of the chromatographic detection module, can clearly indicate the change of the components of the gas sample to be detected, and is used for the on-line monitoring of the separation, purification and collection process, according to the outflow sequence and retention time of different gas components in the air sample from the transfer column 3, the purification column 4 and the separation column 5, a peak cutting technology is adopted, and the switching of valves is utilized, so that a large amount of non-xenon gas components in the pre-concentrated air sample can be emptied in time, the aims of quickly and efficiently transferring, purifying, separating and collecting millilitre xenon in a hectoliter pre-concentrated air sample obtained from a cubic meter air sample are fulfilled, and the preparation is made for the retransfer and measurement of the xenon sample in the subsequent collection column 6. Firstly, during the low-temperature transfer process of a hectolitre level pre-concentrated air sample from an external cubic meter level air sample to a transfer column 3, a large amount of non-xenon gas components are directly exhausted, after the low-temperature transfer is finished, a vacuum pump 12 is started, after the transfer column 3 at low temperature is subjected to pipeline buffer type pressure relief, the transfer column 3 is connected into a chromatographic main flow path, and a thermal conductivity detection module 1 monitors the effluent gas components of the transfer column on line; then, washing the desorbed transfer column 3 with high-purity helium carrier gas, continuously and directly emptying the non-xenon gas components, continuously monitoring the effluent gas component condition of the transfer column 3 on line by the thermal conductivity detection module 1, switching four-way valves FV1 and FV2 when a chromatogram shows that a large amount of non-xenon gas components in an air sample are emptied, sequentially connecting the purification column 4 and the separation column 5 in series behind the transfer column 3, further purifying and separating the rest transfer column air sample through the purification column 4 and the separation column 5 under the normal temperature condition, continuously monitoring the effluent gas component condition of the separation column 5 on line by the thermal conductivity detection module 1, and continuously and directly emptying the non-xenon gas components; then, when the transfer column 3 is at the xenon desorption temperature, the collection column 6 is connected in series to the measuring component outflow part of the thermal conductivity detection module 1 by switching the six-way valve SV3, the purified and separated xenon is collected by the collection column 6, and redundant non-xenon gas components are emptied; and finally, when the thermal conductivity detection module 1 detects that the xenon component in the transfer column 3 is completely desorbed on line and no xenon component flows out from the separation column 5, stopping collection.
The thermal conductivity detection module greatly reduces the treatment capacity of the purification column and the separation column, reduces the column material filling capacity of the purification column and the separation column, saves the treatment time of the whole process, enables the collection column to collect a small amount of pure xenon in the pre-concentrated air sample in time, optimizes the column material filling capacity of the collection column, reduces the xenon loss, improves the xenon recovery rate, and is favorable for the retransfer and physical measurement of the xenon sample in the later-stage collection column; when the device is used for quantitative analysis, the full-process yield of the separation, purification and collection device can be determined, so that technical support is provided for optimizing the process operation parameters.
Furthermore, the structure of the reserved column 2 is a stainless steel hollow pipe, preferably in a U shape, the volume of the reserved column is equal to the volume of pure xenon contained in the pre-concentrated air sample, the reserved column can be used for quantitative analysis of a thermal conductivity detection module, when the flow of separating, purifying and collecting xenon in the actual air sample is simulated, the initial content of the pure xenon is provided, the concentration of the xenon desorbed into an archive bottle by the collecting column is measured, the recovery amount of the pure xenon in the simulated flow is obtained, the full-flow yield of the separating, purifying and collecting device is determined, and substantial technical support is provided for optimizing the operation parameters of the flow. The specific process of determining the process yield of the separation, purification and collection device by the reserved column comprises the following steps: firstly, simulating the purification, separation and collection processes of xenon in an actual air sample, selecting a reserved column with the volume equal to that of pure xenon contained in the air sample, introducing the pure xenon sample from the outside under the normal temperature condition, enabling the pure xenon sample to flow through a purification column and a separation column, and then collecting the pure xenon sample by a collection column; then simulating the desorption and inflation process of the xenon sample in the collecting column, heating the collecting column to the desorption temperature, slowly eluting the pure xenon sample desorbed from the collecting column with high-purity helium and filling the pure xenon sample into a filing bottle, finally measuring the concentration of xenon in the filing bottle to obtain the recovery amount of the pure xenon in the simulation process, and calculating the process yield of the separation and purification collecting device by dividing the total volume of the recovered pure xenon by the total volume of the pure xenon sample introduced into the other parts, thereby providing technical support for optimizing the process operation parameters.
Furthermore, the transfer column 3 is a phi 1/2 stainless steel tube filled with activated carbon, preferably in a U shape, and is installed in a high-low temperature box 8 of the transfer column, the high-low temperature box of the transfer column is specially used for rapidly increasing and decreasing the temperature of the transfer column, a pair of U-shaped groove aluminum plates are arranged in the high-low temperature box, the transfer column and refrigerant conveying pipes and heating pipes which are distributed on two sides of the transfer column are tightly attached and clamped by two U-shaped groove aluminum plates, wherein low-temperature heat conducting oil is filled in the refrigerant conveying pipes, and the heating pipes are electrically heated, so that refrigeration and temperature increase of the transfer column are simple and easy to obtain, and. The requirements of low-temperature adsorption, high-temperature desorption and transfer of xenon in a hectolitre level pre-concentrated air sample from an external cubic meter level air sample are met within the temperature range of-40 ℃ to 300 ℃, the desorption temperature can be accurately controlled, xenon adsorbed by a transfer column is completely desorbed, radon possibly existing is not desorbed, the requirement on xenon adsorption capacity is met, the xenon adsorption, desorption and transfer operations are simple and easy, the active carbon filling amount of the transfer column 3 is effectively reduced, the volume of a high-low temperature box 8 of the transfer column is reduced, the power consumption is reduced, and the processing time of the whole process is saved.
Further, the purification column 4 is a phi 1/4 stainless steel tube filled with a 4A molecular sieve, preferably a spiral type, which is beneficial to miniaturization of the device and realizes adsorption of impurity gases such as water vapor, carbon dioxide and the like in the sample at normal temperature.
Further, the separation column 5 is a phi 1/4 stainless steel tube filled with a 5A molecular sieve, preferably a spiral type, which is beneficial to the miniaturization of the device, realizes the separation of xenon from other impurity gases at normal temperature, and makes the collection of high-purity xenon samples possible.
Furthermore, the collecting column 6 is a phi 1/8 stainless steel tube filled with active carbon, preferably a U-shaped stainless steel tube, which is beneficial to the miniaturization of the device and realizes the collection of milliliter-scale high-purity xenon at normal temperature.
Furthermore, the temperature rise rate of the reserved column heating furnace 7, the purification column heating furnace 9, the separation column heating furnace 10 and the collection column heating furnace 11 is 25 ℃/min-40 ℃/min, and the moderate heating power is favorable for accurately controlling the temperature of the purification column, the separation column and the collection column during heating, ventilating, activating and regenerating, so that the effectiveness and the high efficiency of activating and regenerating are ensured; the collecting column is favorable for rising to the desorption temperature in a short time when being heated and desorbed, the temperature can not overshoot greatly, the collecting column can be controlled accurately, xenon adsorbed by the collecting column can be completely desorbed, radon which possibly exists can not be desorbed, the accuracy and precision of the later-stage radioactive xenon physical measurement are ensured, and the processing time of the whole process is also shortened.
Further, the pumping speed of the vacuum pump 12 is several liters per second, for example, 4 liters per second, so that the separation, purification and collection device can be quickly pumped to the expected vacuum degree, and the processing time of the whole process is saved.
Furthermore, the small steel cylinder 13 is a stainless steel cylinder and is used for cleaning the gas detector, the volume of the small steel cylinder is about 125 times of the volume of the gas detector, high-purity helium with the internal volume being slightly lower than the highest using pressure of the gas detector is filled in the small steel cylinder, the pressure impact of the flow scrubbing gas on the gas detector is reduced through the decompression cache of the high-purity helium, the safe use of the gas detector is ensured, the requirement of miniaturization of the device is met, the gas detector can be continuously cleaned for more than 30 times at the pressure slightly higher than the normal pressure, the influence of the memory effect on the measuring accuracy of the gas detector is eliminated in a short time, and the influence of the cleaning operation on other functional operations of the separation, purification and collection device is reduced to the minimum; below 100kPa, the microcylinder is replenished with high purity helium gas to a pressure slightly below the maximum use pressure of the gas detector.
Further, the storage bottle 14 is a stainless steel bottle for temporarily storing the pure xenon sample when the collection column 6 is heated for desorption, and the volume of the storage bottle is several times, such as 10 to 20 times, of the volume of the gas detector.
Example 1
In this embodiment 1, the separation, purification and collection device for xenon in the air sample is formed by connecting a stainless steel pipe, a valve, a mass flow controller and a pressure sensor according to a flow diagram, wherein the stainless steel pipe is an inner polished stainless steel pipe, and the mass flow controller MF1 has a flow range of 0-1L/min and a precision of 0.1%; the flow range of the mass flow controller MF2 is 0-70 mL/min, and the precision is 0.1%; the pressure ranges of the absolute pressure sensors P1, P2, P3, P4 and P6 are 0-600 kPa, the pressure range of the absolute pressure sensor P5 is 0-200 kPa, and P7 is a vacuum gauge; the integral vacuum degree of the device is not more than 10Pa, and the pressure drop is not more than 0.5kPa.h under the positive pressure condition of 0.5MPa-1This embodiment is rationally distributed, easy to maintain and change. The temperature control ranges of the reserved column heating furnace 7, the purification column heating furnace 9, the separation column heating furnace 10 and the collection column heating furnace 11 are 15-400 ℃, the temperature rise rate is 25-40 ℃/min, and the temperature control precision is not more than +/-5 ℃.
The device of the embodiment is used for the device with the volume of 10m3The separation, purification and collection of xenon in an air sample of (1), comprising the steps of:
a. activation regeneration treatment of column
a1) Introducing carrier gas and flowing through a mass flow controller MF1, and setting the flow rate of the mass flow controller MF1 to be 50 ml/min;
a2) switching on a main power supply of the separation and purification collecting device, switching a six-way valve SV2, a four-way valve FV1, an FV2 and a six-way valve SV3, switching three-way valves TV2 and TV3 to the direction of communicating the six-way valve SV2, switching a three-way valve TV1 to the direction of communicating a thermal conductivity detection module 1, opening a valve V7, and discharging carrier gas from a V7 after the carrier gas flows through the thermal conductivity detection module 1, a transfer column 3, a purification column 4, a separation column 5 and a collecting column 6;
a3) respectively setting the activation temperatures of the transfer column 3, the purification column 4, the separation column 5 and the collection column 6 as 300 ℃, 350 ℃ and 300 ℃, connecting the power supplies of the high-low temperature box 8 of the transfer column, the purification column heating furnace 9, the separation column heating furnace 10 and the collection column heating furnace 11, and connecting carrier gas to heat and activate the regeneration transfer column 3, the purification column 4, the separation column 5 and the collection column 6; after reaching the respective activation temperature of the transfer column 3, the purification column 4, the separation column 5 and the collection column 6, preserving the heat until the activation is complete, and stopping heating;
a4) when the temperatures of the transfer column 3, the purification column 4, the separation column 5 and the collection column 6 are all reduced to room temperature, the six-way valve SV2, the four-way valve FV1, the FV2 and the six-way valve SV3 are switched to enable the transfer column 3, the purification column 4, the separation column 5 and the collection column 6 to be in a closed state, and the transfer process is ready to enter.
b. Transfer of xenon from a preconcentrated air sample
b1) Opening the high-low temperature box 8 of the transfer column for refrigeration, setting the flow rate of the mass flow controller MF1 to be 200 ml/min, and opening the power supply of the thermal conductivity detection module 1 to be in a state to be analyzed;
b2) when the temperature of the transfer column 3 reaches below-30 ℃, the three-way valve TV2 is in a state that a hectolitre level pre-concentration air sample obtained from a cubic meter level air sample from the outside is connected with the transfer column, a xenon flow in the pre-concentration air sample is washed to the transfer column by using high-purity helium carrier gas, the three-way valve TV3 is switched to an emptying state after being delayed for a few seconds so as to completely adsorb xenon in the pre-concentration air sample from the outside into the transfer column, meanwhile, 90% -95% of non-xenon gas components in the pre-concentration air sample from the outside are emptied, and the rest of the non-xenon gas components are adsorbed in the transfer column;
b3) the refrigeration of a high-temperature box and a low-temperature box of the transfer column is closed, three-way valves TV2 and TV3 are switched to be connected with a six-way valve SV2, and the flow of separating, purifying and collecting xenon in an air sample in the transfer column is prepared; .
c. Separation, purification and collection of xenon from air samples in transfer columns
c1) When the transfer column 3 is at-30 ℃, alternately switching on and off the valves V6 and V16, evacuating the pipeline by using a vacuum pump 12, performing pipeline buffer type pressure relief on the transfer column 3 until a vacuum gauge P7 shows that the pressure is below 20kPa, and closing V6 and V16; in the step c, setting the pumping speed of the vacuum pump to be 2L/s;
c2) setting the heating temperature of the transfer column 3 to be 0 ℃, alternately switching on and off V6 and V16 again when the pressure sensor P2 shows that the pressure exceeds 100kPa, evacuating the pipeline by using a vacuum pump 12, performing pipeline buffer type pressure relief on the transfer column 3 until a vacuum gauge P7 shows that the pressure is below 20kPa, then switching over a six-way valve SV2 to enable the transfer column to be communicated with a valve V7 through four-way valves FV1 and FV2 and a six-way valve SV3, washing the transfer column by using high-purity helium carrier gas flow, and starting online monitoring of outflow gas components of the transfer column by a thermal conductivity detection module to ensure that 92% of non-xenon gas components in the transfer column in the step b 2) are emptied;
c3) setting the desorption temperature of the transfer column to be 300 ℃, when the chromatogram shows that the air peak is in a completely descending trend, indicating that a large amount of non-xenon gas components in the air sample are emptied, switching four-way valves FV1 and FV2, sequentially connecting the purification column and the separation column in series behind the transfer column, purifying xenon and the residual non-xenon gas in the transfer column through the purification column, and separating through the separation column; the thermal conductivity detection module continuously monitors the effluent gas components of the purification column and the separation column on line, and completely empties the residual non-xenon gas;
c4) when the temperature of the transfer column 3 reaches 300 ℃, switching a six-way valve SV3 to connect the collecting column in series to the position where the measuring component of the thermal conductivity detection module flows out, and collecting the xenon separated in the step c 3) into a collecting column 6;
c5) when the thermal conductivity detection module monitors that the xenon component is completely collected on line, namely, the xenon peak is reduced to a baseline level, the six-way valve SV3 is switched to stop collecting, and the transfer column 3 stops heating. Thus completing the separation, purification and collection of xenon in the air sample of the transfer column.
Further, in order to transfer the xenon in the separated and purified air sample to a gas detector for a subsequent xenon measurement process, the method of the embodiment further comprises the following steps:
d. desorption and inflation process for xenon sample in collecting column
d1) Switching a three-way valve TV4 to make the flow washing gas flow through a mass flow controller MF2, opening valves V8, V13 and V15, alternately switching valves V9 and V16, opening a vacuum pump to enable the vacuum pump to evacuate a pipeline, and relieving the pressure of a collecting column to be below 1 kPa; the vacuum pump is closed, and the valves V8, V9, V13, V15 and V16 are closed;
d2) setting the desorption temperature of the collecting column 6 to 300 ℃, heating to 300 ℃, setting the flow of a mass flow controller MF2 in the range of 1 ml/min-5 ml/min, adopting a micro-flow control technology, opening valves V8, V9 and V12 to enable the flow-scrubbing gas high-purity helium to slowly flow and scrub the collecting column 6, filling the high-purity xenon of the collecting column 6 into a gas detector, closing the valves V8, V9 and V12 when a pressure sensor P5 shows that the pressure is about 95kPa, stopping heating the collecting column 6, and finishing the gas filling. The flow rate of the mass flow controller MF2 was set to 0 and the xenon charged by the gas detector was used for subsequent xenon measurements.
The embodiment pair is composed of 10m3The time for transferring the pre-concentrated air sample of about one hundred liters obtained from the air sample to the transfer column can be controlled within 1h, and the time for separating, purifying and collecting the xenon in the air sample in the transfer column does not exceed 40 min. Therefore, compared with the problems of complex processing process and long consumed time of a small amount of xenon in a cubic meter-level air sample in the traditional technology, the device realizes the rapid and efficient transfer, purification, separation and collection of milliliter-level xenon in a hectoliter-level pre-concentrated air sample obtained from the cubic meter-level air sample, meets the measurement requirement of a gas detector on a small amount of radioactive xenon in a large amount of air samples, and solves the urgent need of monitoring radioactive xenon isotopes.
The described embodiment of the invention is only one of the possibilities that is easy to implement. All relevant embodiments are exemplary and not exhaustive, and the invention is in no way limited to only these embodiments. Many modifications and variations are possible and apparent without departing from the scope and spirit of embodiments of the invention.

Claims (5)

1. A method for separating, purifying and collecting xenon in an air sample based on a specific device, which is characterized in that the specific device comprises: the device comprises a transfer unit, a separation and purification unit, a collection unit and auxiliary units, wherein the transfer unit is connected with the separation and purification unit, the separation and purification unit is connected with the collection unit, and the auxiliary units are respectively connected to the transfer unit, the separation and purification unit and the collection unit;
the transfer unit comprises a high-low temperature box (8) of the transfer column and the transfer column (3) arranged in the high-low temperature box of the transfer column, and refrigerant conveying pipes and heating pipes are tightly arranged on two sides of the transfer column (3);
the separation and purification unit comprises a thermal conductivity detection module (1), a reserved column heating furnace (7), a purification column heating furnace (9), a separation column heating furnace (10), and reserved columns (2), purification columns (4) and separation columns (5) which are respectively arranged in the reserved column heating furnace, the purification column heating furnace and the separation column heating furnace;
the collecting unit comprises a collecting column heating furnace (11) and a collecting column (6) arranged in the collecting column heating furnace;
the auxiliary unit comprises a vacuum pump (12) connected with the transfer unit, the separation and purification unit and the collection unit, a steel bottle (13) connected with the flow scrubbing gas and a storage bottle (14) connected with the collection column;
the method specifically comprises the following steps:
a) the activation and regeneration treatment of the column is carried out,
b) the transfer of xenon from the pre-concentrated air sample,
c) separating, purifying and collecting xenon in an air sample in the transfer column;
wherein, the step a) specifically comprises the following steps:
a1) introducing carrier gas and flowing through a mass flow controller MF1, and setting the flow rate of a mass flow controller MF 1;
a2) switching on a power supply of the separation, purification and collection device, switching a valve, and enabling the carrier gas to flow through the thermal conductivity detection module, the transfer column, the purification column, the separation column and the collection column and be discharged from a valve V7;
a3) respectively setting the activation temperatures of the transfer column, the purification column, the separation column and the collection column, and heating the transfer column, the purification column, the separation column and the collection column; after reaching the respective activation temperature of the transfer column, the purification column, the separation column and the collection column, preserving the heat until the activation is complete, and stopping heating;
a4) cooling the temperature of the transfer column, the purification column, the separation column and the collection column to room temperature, switching valves to enable the transfer column, the purification column, the separation column and the collection column to be in a closed state, and preparing to enter a transfer process of xenon in the pre-concentrated air sample;
the step b) specifically comprises the following steps:
b1) starting refrigeration of a high-low temperature box of the transfer column, resetting the flow rate of a mass flow controller MF1, and starting a power supply of a thermal conductivity detection module to be in a state to be analyzed;
b2) when the temperature of the transfer column reaches the set adsorption temperature of xenon, the three-way valve TV2 is in a state of connecting the external pre-concentrated air sample with the transfer column, the xenon in the external pre-concentrated air sample is adsorbed to the transfer column, the three-way valve TV3 is switched to an emptying state so as to completely adsorb the xenon in the external pre-concentrated air sample into the transfer column, meanwhile, 90% -95% of non-xenon gas components in the external pre-concentrated air sample are emptied, and the rest of the non-xenon gas components are adsorbed in the transfer column;
b3) the refrigeration of a high-temperature box and a low-temperature box of the transfer column is closed, three-way valves TV2 and TV3 are switched to be connected with a six-way valve SV2, and the flow of separating, purifying and collecting xenon in an air sample in the transfer column is prepared;
the step c) specifically comprises the following steps:
c1) when the temperature of the transfer column reaches-40 ℃ to-10 ℃, alternately switching on and off the valves V6 and V16, evacuating a pipeline by using a vacuum pump to release the pressure of the transfer column, and closing the valves V6 and V16;
c2) setting the heating temperature of the transfer column to be 0 ℃, alternately switching on and off the valves V6 and V16 again, evacuating the pipeline by using a vacuum pump, continuously decompressing the transfer column, switching over the six-way valve SV2 to enable the transfer column to be communicated with the valve V7 through the four-way valves FV1 and FV2 and the six-way valve SV3, washing the transfer column by using high-purity helium carrier gas flow, and starting online monitoring of the effluent gas component of the transfer column by using a thermal conductivity detection module to ensure that 90-95% of non-xenon gas components in the transfer column in the step b 2) are evacuated;
c3) setting the desorption temperature of the transfer column, switching four-way valves FV1 and FV2, connecting the purification column and the separation column in series after the transfer column in turn, purifying xenon and the residual non-xenon gas component in the transfer column through the purification column, and separating through the separation column; the thermal conductivity detection module continuously monitors the effluent gas components of the purification column and the separation column on line, and completely empties the residual non-xenon gas components;
c4) when the transfer column reaches the desorption temperature, switching a six-way valve SV3 to connect the collection column in series to the position where the measurement component of the thermal conductivity detection module flows out, and collecting the xenon separated in the step c 3) into the collection column;
c5) when the thermal conductivity detection module monitors that the xenon component is completely collected on line, the collection is stopped and the heating of the transfer column is stopped, so that the separation, purification and collection of xenon in the air sample of the transfer column are completed.
2. The device-specific air sample xenon separation, purification and collection method according to claim 1, further comprising the steps of:
d) a flow of desorbing and inflating the xenon sample in the collecting column;
the step d) comprises the following steps:
d1) switching a three-way valve TV4 to make the flow washing gas flow through a mass flow controller MF2, opening valves V8, V13 and V15, alternately switching valves V9 and V16, opening a vacuum pump to enable the vacuum pump to evacuate a pipeline, and relieving the pressure of a collecting column to be below 1 kPa; the vacuum pump is closed, and the valves V8, V9, V13, V15 and V16 are closed;
d2) setting the desorption temperature of the collection column, heating to the desorption temperature, keeping the temperature, setting the flow rate of a mass flow controller MF2, opening valves V8, V9 and V12, washing the collection column by flowing washing gas, filling xenon in the collection column into a gas detector, enabling the pressure of a pressure sensor P5 to be displayed and increased at the speed of hundred pascals per second, closing valves V8, V9 and V12 when a pressure sensor P5 is displayed and is 94-96 kPa, stopping heating the collection column, and ending inflation.
3. The method for separating, purifying and collecting xenon in the air sample based on the specific device according to claim 1 or 2, wherein in the steps b 2) to b 3) and c 2) to c 5), the transfer column is a stainless steel tube filled with activated carbon, the stainless steel tube is installed in a high-temperature box and a low-temperature box of the transfer column, a pair of U-shaped groove aluminum plates are arranged in the high-temperature box and the low-temperature box of the transfer column, and the transfer column, a refrigerant conveying pipe and a heating pipe which are distributed on two sides of the transfer column are tightly attached and clamped by the two U-shaped groove aluminum plates, wherein the refrigerant is low-temperature heat conducting oil, and the heating pipe is electrically heated.
4. The specific apparatus based method for separating, purifying and collecting xenon in the air sample according to claim 2, wherein the desorption temperature in step d 2) is 300 ℃ to 350 ℃.
5. The specific device-based method for separating, purifying and collecting xenon in the air sample according to claim 2, wherein in the step d 2), the flow rate is 1-5 ml/min.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112557158A (en) * 2021-02-28 2021-03-26 中国工程物理研究院核物理与化学研究所 Separation, purification and collection device for xenon in air sample

Citations (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1196331A (en) * 1997-04-17 1998-10-21 张鸿逵 Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon.
CN1404413A (en) * 2000-10-20 2003-03-19 日本酸素株式会社 Gas separating and purifying method and its apparatus
CN1554946A (en) * 2003-12-19 2004-12-15 �й����������о�Ժ�������뻯ѧ�о� Method and system for quick separating and measuring 37 Ar
JP3822886B2 (en) * 2004-06-22 2006-09-20 核燃料サイクル開発機構 Tag gas sealing device for internal pressure creep test piece
JP3869831B2 (en) * 2004-03-01 2007-01-17 大陽日酸株式会社 Gas separation method and apparatus
CN101634515A (en) * 2009-08-13 2010-01-27 上海启元科技发展有限公司 Method for extracting high-yield pure krypton and pure xenon by full distillation
CN202052451U (en) * 2011-01-21 2011-11-30 中国人民解放军63653部队 Device for enriching and separating xenon in air through carbon molecular sieves
CN102359895A (en) * 2011-08-15 2012-02-22 西北核技术研究所 Normal temperature enrichment and sampling method for xenon in air, and apparatus thereof
CN102489108A (en) * 2011-11-28 2012-06-13 西北核技术研究所 Method for separating and purifying xenon in atmosphere by use of active carbon and device thereof
CN102508285A (en) * 2011-11-28 2012-06-20 西北核技术研究所 Method and device for enriching and sampling xenon in atmosphere at low temperature
CN103949159A (en) * 2014-05-15 2014-07-30 中国工程物理研究院核物理与化学研究所 Separation method of radioisotope 14C
CN104310325A (en) * 2014-10-24 2015-01-28 武汉钢铁(集团)公司 Krypton-xenon gas purification method and device
CN105181841A (en) * 2015-09-08 2015-12-23 中国人民解放军63653部队 Instrumented rapid purification system device for xenon
CN107063784A (en) * 2016-10-31 2017-08-18 核工业北京地质研究院 It is a kind of to be used for the extraction purification system and its method for extraction and purification of dissolving xenon in water
US10226731B2 (en) * 2016-09-02 2019-03-12 Battelle Memorial Institute Xenon collection method and system
CN109665505A (en) * 2018-12-21 2019-04-23 北京放射性核素实验室 A kind of preparation method of atmosphere xenon enrichment and purification method, device and carbon molecular sieve
CN109939538A (en) * 2019-04-12 2019-06-28 中国原子能科学研究院 The Quick Separation System and method of Kr and Xe in complicated fission product
CN111065872A (en) * 2017-09-05 2020-04-24 普莱克斯技术有限公司 System and method for recovering non-condensable gases such as neon, helium, xenon, and krypton from an air separation unit
CN212060095U (en) * 2020-01-14 2020-12-01 中广核研究院有限公司 Separation and purification device for ultralow radioactivity krypton and xenon in gaseous effluent of nuclear power station

Patent Citations (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1196331A (en) * 1997-04-17 1998-10-21 张鸿逵 Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon.
CN1404413A (en) * 2000-10-20 2003-03-19 日本酸素株式会社 Gas separating and purifying method and its apparatus
CN1554946A (en) * 2003-12-19 2004-12-15 �й����������о�Ժ�������뻯ѧ�о� Method and system for quick separating and measuring 37 Ar
JP3869831B2 (en) * 2004-03-01 2007-01-17 大陽日酸株式会社 Gas separation method and apparatus
JP3822886B2 (en) * 2004-06-22 2006-09-20 核燃料サイクル開発機構 Tag gas sealing device for internal pressure creep test piece
CN101634515A (en) * 2009-08-13 2010-01-27 上海启元科技发展有限公司 Method for extracting high-yield pure krypton and pure xenon by full distillation
CN202052451U (en) * 2011-01-21 2011-11-30 中国人民解放军63653部队 Device for enriching and separating xenon in air through carbon molecular sieves
CN102359895A (en) * 2011-08-15 2012-02-22 西北核技术研究所 Normal temperature enrichment and sampling method for xenon in air, and apparatus thereof
CN102489108A (en) * 2011-11-28 2012-06-13 西北核技术研究所 Method for separating and purifying xenon in atmosphere by use of active carbon and device thereof
CN102508285A (en) * 2011-11-28 2012-06-20 西北核技术研究所 Method and device for enriching and sampling xenon in atmosphere at low temperature
CN103949159A (en) * 2014-05-15 2014-07-30 中国工程物理研究院核物理与化学研究所 Separation method of radioisotope 14C
CN104310325A (en) * 2014-10-24 2015-01-28 武汉钢铁(集团)公司 Krypton-xenon gas purification method and device
CN105181841A (en) * 2015-09-08 2015-12-23 中国人民解放军63653部队 Instrumented rapid purification system device for xenon
US10226731B2 (en) * 2016-09-02 2019-03-12 Battelle Memorial Institute Xenon collection method and system
CN107063784A (en) * 2016-10-31 2017-08-18 核工业北京地质研究院 It is a kind of to be used for the extraction purification system and its method for extraction and purification of dissolving xenon in water
CN111065872A (en) * 2017-09-05 2020-04-24 普莱克斯技术有限公司 System and method for recovering non-condensable gases such as neon, helium, xenon, and krypton from an air separation unit
CN109665505A (en) * 2018-12-21 2019-04-23 北京放射性核素实验室 A kind of preparation method of atmosphere xenon enrichment and purification method, device and carbon molecular sieve
CN109939538A (en) * 2019-04-12 2019-06-28 中国原子能科学研究院 The Quick Separation System and method of Kr and Xe in complicated fission product
CN212060095U (en) * 2020-01-14 2020-12-01 中广核研究院有限公司 Separation and purification device for ultralow radioactivity krypton and xenon in gaseous effluent of nuclear power station

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
SHAN ZHONG: "ZIF-Derived Nitrogen-Doped Porous Carbons for Xe Adsorption and Separation", 《SCIENTIFIC REPORTS》 *
V. L. BONDARENKO: "AUTOMATED CRYOGENIC UNIT FOR XENON EXTRACTION FROM CONCENTRATED MIXTURES", 《CHEMICAL AND PETROLEUM ENGINEERING》 *
徐常昆: "乏燃料溶解尾气中氙的取样分离及稳定同位素比的测量", 《核化学与放射化学》 *
熊顺顺: "放射性惰性气体分离与分离材料研究进展", 《核化学与放射化学》 *
王亚龙: "国际监测系统中大气氙取样器的设计方法探讨", 《第七届核化学与放射化学学术讨论会》 *
王茜: "大气中放射性氙的分离纯化系统研制", 《中国测试》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112557158A (en) * 2021-02-28 2021-03-26 中国工程物理研究院核物理与化学研究所 Separation, purification and collection device for xenon in air sample

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