CN102508285B - Method and device for enriching and sampling xenon in atmosphere at low temperature - Google Patents
Method and device for enriching and sampling xenon in atmosphere at low temperature Download PDFInfo
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Abstract
The invention relates to a method and device for enriching and sampling xenon in atmosphere at low temperature. The method comprises the following steps of: enriching the xenon in the atmosphere at low temperature, and realizing enrichment concentration of the xenon by using four levels of adsorbing columns at the same time and removing other impurities synchronously. According to the method for enriching and sampling the xenon in the atmosphere at low temperature, disclosed by the invention, active carbon serves as an adsorbing agent, thus the complexity and the realization difficulty of the method are reduced, and no spare time exists; in addition, the device disclosed by the invention can be used for carrying out continuous sampling and has a simple structure; and the method disclosed by the invention is simple and convenient, and is large in sampling amount.
Description
Technical field
The invention belongs to nuclear environment monitoring method, be specifically related to the concentration and separation of rare gas xenon in atmosphere.
Background technology
Radio nuclide monitoring system technology is that four kinds of the Comprehensive Nuclear Test Ban Treaty (CTBT) regulation are verified one of gordian technique.Nuclear activity produces and the Characteristic radionuclides of release plays conclusive effect to the qualitative identification of suspicious event in CTBT verifies, and is the emphasis of radio nuclide monitoring system technical research for the sample analysis technology of these nucleic always.In international radio nuclide monitoring system system, interested radioactivity rare gas is that radioactive xenon isotope (mainly comprises
131mxe,
133mxe,
133xe,
135xe).
In air, the volume fraction of rare gas xenon is 8.7 × 10
-8(v/v), wherein the content of radioactive xenon isotope is lower, is difficult to Direct Analysis.The sampling of radgas xenon is separation and concentration xenon isotope from ambient atmosphere, and make its quantitative detection sensitivity that reaches total xenon analytical instrument and the requirement of radioactivity survey instrument to radioactive xenon isotope content, therefore must from a large amount of air, (be greater than 10m
3) xenon is concentrated to a very little volume (several to hundreds of ml).
Literature search information: the people's such as 63653 Zhou Chongyang of army of the Chinese People's Liberation Army invention, number be the patent of CN201728039U " a kind of tripping device of enriched gas xenon ", adopt one-level 5A molecular sieve removal of impurities post, one-level active carbon adsorption column, secondary 5A molecular sieve to add that activated charcoal removal of impurities post, secondary active carbon adsorption column, three grades of 5A molecular sieve add activated charcoal removal of impurities post, three grades of active carbon adsorption columns carry out concentration and separation xenon, 6 adsorption columns are altogether used, relate to the adsorbent of 2 kinds of each 2 specifications, and can not realize serial sampling.Another invention of the people such as Zhou Chongyang, number be the CN 101985080 A patents of " a kind of activated charcoal is used for the enrichment and separation method of xenon ", only can concentration for the treatment of the xenon calibrating gas that is 10～1000ppm, can not directly from air, sample.What Sweden A.Ringbom etc. delivered on the 508th phase (2003) at periodical " Nuclear Instruments and Methods in Physics Research A " is entitled as " SAUNA-a system for automatic sampling, processing, and analysis of radioactive xenon " article, adopt two cover 4A molecular sieve adsorption posts in parallel and active carbon adsorption column to carry out enrichment, follow-up series winding 4A molecular sieve adsorption post, active carbon adsorption column, 3A molecular sieve adsorption post, 5A molecular sieve adsorption post, 5A molecular sieve chromatography post, carbonaceous molecular sieve adsorption column carrys out separation and purification xenon, 8 grades of adsorption columns are altogether used, relate to 3A, 4A, 5A molecular sieve, carbonaceous molecular sieve, 5 kinds of adsorbents such as activated charcoal.
Summary of the invention
The object of the invention is to provide a kind of low temperature enrichment sampling method and device of xenon in atmosphere, its under cryogenic conditions by airborne xenon enrichment, use altogether 4 grades of adsorption columns to realize concentrated other impurity of also simultaneously removing of enrichment of xenon, adsorbent only uses activated charcoal one, energy serial sampling, simple in structure, method is easy, and sampling amount is large.
A low temperature enrichment sampling method for xenon in atmosphere, comprises the following steps:
1] cryosorption high temperature desorption:
Adopt the first order charcoal absorption desorption unit xenon in condensed air remove other impurity at low temperatures, adsorption temp is-70～-40 DEG C, and desorption temperature is 50～200 DEG C;
2] three grades of normal temperature absorbing high temp desorptions:
The charcoal absorption desorption unit that adopts three cascades xenon in condensed air remove other impurity step by step at normal temperatures, adsorption temp is 10～30 DEG C, desorption temperature is 50～200 DEG C;
3] sample collection:
Afterbody adsorption column desorption xenon is out pressurized to sample bottle through barrier film, completes collection.
Above-mentioned steps is first carried out heat-activated to the acticarbon loading in adsorption columns at different levels before being also included in the concentrated sampling of enrichment.
Above-mentioned first order adsorption/desorption unit is the active carbon adsorption column of two cover parallel connections, and described two covers active carbon adsorption column in parallel is realized alternately adsorption and desorption by valve.
A kind of low temperature enrichment sampler of xenon in atmosphere, comprise compressed air source, the adsorption/desorption unit of level Four cascade operation, sample collection bottle, carrier gas source, vacuum pump, described every grade of adsorption/desorption unit comprises active carbon adsorption column and is arranged on the adsorption column heating arrangement of active carbon adsorption column periphery, described compressed air source is connected with the inlet end pipeline of first order adsorption/desorption unit, the outlet side of described afterbody adsorption/desorption unit is connected with sample collection bottle pipeline through diaphragm booster pump, described carrier gas source is connected with the inlet end of level Four adsorption/desorption unit with valve by pipeline, described vacuum pump is connected with the outlet side of level Four adsorption/desorption unit with valve by vacuum pipe, its special character is: between described compressed air source and first order adsorption/desorption unit, be provided with gas cooler, described first order adsorption/desorption unit comprises two parallel connections and replaces the active carbon adsorption column of adsorption/desorption.
Above-mentioned activated charcoal is 14～25 order cocoanut active charcoals; The carrier gas of described carrier gas source is nitrogen or helium.
Advantage of the present invention is:
1, air drying, cooling processing, temperature is brought down below-70 DEG C, directly upper prop absorption, column temperature is at-70～-40 DEG C, enrichment xenon at low temperatures, adsorption column volume is little, and sampling amount is large.
2, use the xenon in condensed air remove other impurity step by step of 4 grades of active carbon adsorption columns altogether, rear three grades of activated-charcoal column adsorbs xenon all at normal temperatures (10～30 DEG C) are carried out, only use a kind of adsorbent and only have not absorption at normal temperatures of one-level, reduced the complicacy of method and realized difficulty.
3, use the parallel one-level adsorption column Ca1 of two covers and alternately sampling of Cb1, make sampling process uninterrupted continuously, be applicable to the long term monitoring of atmospheric environment, the representativeness of institute's sample thief is strong, not free empty window.
4, the present invention is greater than 5 × 10 to the enrichment factor of xenon
6, the decontamination factor of radon is greater than 1 × 10
5, efficient sampling volume can be greater than to 100m
3airborne xenon (volume fraction 8.7 × 10
-8), separation and concentration is the sample (xenon concentration is greater than 40%) of volume 20ml, measures the requirement to sample considerably beyond total xenon measurement and radioactive xenon isotope, is specially adapted to the extremely low environmental monitoring of radioactive xenon isotope content in air.
5, the present invention is not only applicable to the monitoring of atmosphere nuclear environment, is equally applicable to the small-scale production of xenon.
6, the thought that the uninterrupted sampling continuously that the present invention adopts and level Four adsorption column concentrate step by step, can be extended to the design of other types of gases sampler.
Brief description of the drawings
Fig. 1 is the structure principle chart of the continuous sampling system of low temperature enrichment xenon in atmosphere;
As shown in the figure: 1-air compressor machine, 2-dryer, 3-gas cooler, 4-membrane pump, 5-vacuum pump, 6-carrier gas steel cylinder, 7-sample collection bottle, RH-gas dew point meter, MFC-gas mass flow controller, T-temperature sensor, V-valve, P-pressure unit, C-adsorption column.
Embodiment
Apparatus of the present invention course of work:
Air drying, cooling processing, dew point is less than-40 DEG C of Td, and temperature is brought down below-70 DEG C, directly upper prop absorption, column temperature is at-70～-40 DEG C; Use the xenon in condensed air remove other impurity step by step of 4 grades of active carbon adsorption columns altogether, rear three grades of activated-charcoal columns all adsorb at normal temperatures to xenon, all adsorption columns to xenon all at high temperature (50～200 DEG C) carry out desorption; Use the parallel one-level adsorption column Ca1 of two covers and alternately sampling of Cb1, the saturated rear switching Cb1 of Ca1 absorption adsorbs, Ca1 carries out desorption and regeneration simultaneously, after Cb1 absorption is saturated, switching Ca1 adsorbs again, Cb1 carries out desorption and regeneration simultaneously, repeatedly carry out, ensure the uninterrupted continuously of one-level adsorption process.Select 14～25 object cocoanut active charcoals, as the adsorbent of adsorption columns at different levels, one-level adsorption column is (70～-40 DEG C) adsorbs xenon at low temperatures, rear three grades of adsorption columns are (10～30 DEG C) adsorbs xenon at normal temperatures, all at high temperature (50～200 DEG C) desorption xenon, carrier gas is nitrogen or helium.
Air pretreatment unit: blast dryer 2, gas dew point meter RH, gas mass flow controller MFC0, gas cooler 3 are installed on the connecting tube exporting at air compressor machine 1 successively, and gas cooler is connected temperature sensor T0, valve V1, Va11, Vb11 by a four-way with a three-way connection;
One-level absorbing unit: Va11 is by two threeways or four-way connection Bonding pressure transmitter Pa1, a valve Va12 and one-level adsorption column Ca1, and the outlet of Ca1 is through connecting valve Va13, Va14, Va15 by two threeways or a four-way connection after filtrator; Vb11 is by two threeways or four-way connection Bonding pressure transmitter Pb1, a valve Vb12 and one-level adsorption column Cb1, and the outlet of Cb1 is through connecting valve Vb13, Vb14, Vb15 by two threeways or a four-way connection after filtrator; Between Va12, Vb12, connect the outlet of gas mass flow controller MFC1 by a three-way connection, the entrance of MFC1 connects carrier gas channel, between Va14, Vb14, connect valve V2 and V3 by two threeways or a four-way connection, V3 connects valve V21, between Va15, Vb15, connects vacuum pipe by a three-way connection;
Secondary absorption unit: V21 is by four-way connection Bonding pressure transmitter P2, a valve V22 and secondary absorption post C2, the outlet of C2 is through connecting valve V23, V24, V25 by a four-way connection after filtrator, V22 connects the outlet of gas mass flow controller MFC2, the entrance of MFC2 connects carrier gas channel, V24 connects valve V31, and V25 connects vacuum pipe;
Three grades of absorbing unit: V31 are by four-way connection Bonding pressure transmitter P3, a valve V32 and three grades of adsorption column C3, the outlet of C3 is through connecting valve V33, V34, V35 by a four-way connection after filtrator, V32 connects the outlet of gas mass flow controller MFC3, the entrance of MFC3 connects carrier gas channel, V34 connects valve V41, and V35 connects vacuum pipe;
Level Four absorbing unit: V41 is by four-way connection Bonding pressure transmitter P4, a valve V42 and level Four adsorption column C4, the outlet of C4 is through connecting valve V43, V44, V45 by a four-way connection after filtrator, V42 connects the outlet of gas mass flow controller MFC4, the entrance of MFC4 connects carrier gas channel, V44 connects miniature diaphragm supercharge pump 4, and V45 connects vacuum pipe;
Source unit processed: barrier film delivery side of pump connects valve V46, V46 is by four-way connection Bonding pressure transmitter P5, a valve V48 and the sample collection bottle 7 with valve V47, and V48 connects vacuum pipe; Vacuum pipe is all connected with vacuum pump 5, and carrier gas channel is all connected with carrier gas steel cylinder 6.In source procedure processed, use miniature diaphragm supercharge pump, level Four adsorption column desorption xenon out, transfers in sample bottle through membrane pump.
The present invention is greater than 5 × 10 to the enrichment factor of xenon
6, the decontamination factor of radon is greater than 1 × 10
5, efficient sampling volume can be greater than to 100m
3airborne xenon (volume fraction 8.7 × 10
-8), separation and concentration is the sample (xenon concentration is greater than 40%) of volume 20ml.
Principle of work of the present invention:
The present invention proposes the method and apparatus of the serial sampling of enrichment xenon in atmosphere under a kind of cryogenic conditions, the method is dry by air, cooling rear upper prop absorption, use 4 grades of adsorption columns xenon in enrichment condensed air step by step, one-level adsorption column is (70～-40 DEG C) absorption at low temperatures, rear three grades of adsorption columns are (10～30 DEG C) absorption at normal temperatures, one-level adsorption column adopts two cover parallel organizations, alternation, realize continuously uninterrupted sampling, use a kind of adsorbent of activated charcoal, the method is reasonable in design, simple in structure, easy and simple to handle, sampling amount is large, can be used for the sampling to rare gas xenon in surrounding air.
Below in conjunction with embodiment, the invention will be further described:
According to the annexation shown in Fig. 1, set up the continuous sampling system of low temperature enrichment xenon in atmosphere.
Wherein: one-level absorption column length 1m, internal diameter 50mm, the long series winding of available 2 500mm; Secondary absorption column length 400mm, internal diameter 20mm; Three grades of absorption column length 280mm, internal diameter 10mm; Level Four absorption column length 150mm, internal diameter 4.6mm; External heater power is respectively 800,200,100,100W.Filling 14～25 order cocoanut active charcoals.Carrier gas is nitrogen or helium.
Before sampling, need to carry out heat-activated to the acticarbon loading in adsorption columns at different levels, be beneficial to the enrichment of activated charcoal to xenon in air.
Concrete grammar is: open vacuum pump and valve Va15, Vb15, V25, V35, V45, adsorption columns at different levels are vacuumized, to pressure Pa 1, Pb1, P2, the equal < 1kPa of P3, P4.Open the well heater on adsorption columns at different levels, be warmed up to 200 DEG C and keep 30min after stop heating, close vacuum pump and all valves after being down to 30 DEG C of <.The flow of setting mass flow controller MFC1, MFC2, MFC3, MFC4 is respectively 200,50,20,10mL/min, opens MFC1, MFC2, MFC3, MFC4 and valve Va12, Vb12, V22, V32, V42, adds carrier gas protection.When after pressure Pa 1, Pb1, P2, the equal > 110kPa of P3, P4, close all mass flow controllers and valve.
Operation steps:
(1) air pretreatment
The flow of setting mass flow controller MFC0 is 150～200L/min, opens air compressor machine, instrument air dryer, MFC0 and valve V1, after gas dew point meter RH shows that dew point is lower than-40 DEG C of Td, opens gas cooler.After temperature sensor T0 displays temperature is lower than-70 DEG C, valve-off V1.
(2) one-level adsorption column Ca1 enrichment
Open valve Va11, Va13, by one-level adsorption column, Ca1 samples, and stops sampling, valve-off Va11, Va13 after 4h.Open valve Vb11, Vb13, be switched to one-level adsorption column Cb1 sampling.
(3) one-level adsorption column Ca1 desorption purifying
Open MFC1 and valve Va12, Va14, V2, and open the well heater on one-level adsorption column Ca1, when being warming up to valve-off V2 after 110 DEG C.Open valve V3, V21, V23, one-level adsorption column Ca1 is heated to 200 DEG C and keep 20min, close MFC1 and valve Va12, Va14, V3, V21.Open vacuum pump and valve Va15, keep 200 DEG C of 30min of one-level adsorption column Ca1 temperature.Valve-off Va15, stops heating one-level adsorption column Ca1, is cooled to 30 DEG C of <.This process makes the xenon of desorption in one-level adsorption column Ca1 be transferred to secondary absorption post C2.
(4) secondary absorption post C2 desorption purifying
Open MFC2 and valve V22, open the well heater on secondary absorption post C2 simultaneously, when be warming up to 80 DEG C and keep 5min after valve-off V23.Open valve V24, V31, V33, two adsorption column C2 are heated to 160 DEG C and keep 10min, close MFC2 and valve V22, V24, V31, V33.Open valve V25, two adsorption column C2 are heated to 200 DEG C and keep 30min.Valve-off V25, stops heating secondary absorption post C2, is cooled to 30 DEG C of <.This process makes the xenon of desorption in secondary absorption post C2 be transferred to three grades of adsorption column C3.
(5) one-level adsorption column Cb1 enrichment
After one-level adsorption column Cb1 sampling 4h, stop sampling, valve-off Vb11, Vb13.Open valve Va11, Va13, be switched to one-level adsorption column Ca1 sampling.
(6) one-level adsorption column Cb1 desorption purifying
Open MFC1 and valve Vb12, Vb14, V2, and open the well heater on one-level adsorption column Cb1, when being warming up to valve-off V2 after 110 DEG C.Open valve V3, V21, V23, one-level adsorption column Cb1 is heated to 200 DEG C and keep 20min, close MFC1 and valve Vb12, Vb14, V3, V21.Open valve Vb15, keep 200 DEG C of 30min of one-level adsorption column Cb1 temperature.Valve-off Vb15, stops heating one-level adsorption column Cb1, is cooled to 30 DEG C of <.This process makes the xenon of desorption in one-level adsorption column Cb1 be transferred to secondary absorption post C2.
Repeating step (4), makes the xenon of desorption in secondary absorption post C2 be transferred to three grades of adsorption column C3.
Repeat aforementioned all processes 3 times, total is carried out step (2), (3), (5), (6) each 3 times, step (4) totally 6 times, carrying out one-level adsorption column Ca1 and Cb1 samples each 3 times, shift each 3 times to secondary absorption post C2, C2 shifts 6 times to three grades of adsorption column C3.
(7) three grades of adsorption column C3 desorption purifying
Open MFC3 and valve V32, V33, open the well heater of three grades of adsorption column C3 simultaneously, when being warming up to valve-off V33 after 50 DEG C.Open valve V34, V41, V43, three grades of adsorption column C3 are heated to 160 DEG C and keep 5min, close MFC3 and valve V32, V34, V41, V43.Open valve V35, three adsorption column C3 are heated to 200 DEG C and keep 30min.Valve-off V35, stops heating three grades of adsorption column C3, is cooled to 30 DEG C of <.This process makes the xenon of desorption in three grades of adsorption column C3 be transferred to level Four adsorption column C4.
(8) level Four adsorption column C4 desorption, source processed
Open valve V48, V47, sample bottle is vacuumized, to pressure P 5 < 1kPa, valve-off V47, V48.Open the well heater of level Four adsorption column C4, be warming up to 200 DEG C and keep 5min, open valve V44, V46, V47 and membrane pump, while no longer rising to P5 value, close membrane pump.Open MFC4 and valve V42, while being about 100kPa to pressure P 4 values, valve-off V42, open membrane pump, while no longer rising to P5 value, close membrane pump, this process repeatedly, while being about 100kPa, closes the well heater of membrane pump, MFC4, C4 and valve V44, V46, V47 to P5 value.Open valve V45, keep 200 DEG C of 30min of level Four adsorption column C4 temperature.Valve-off V45, stops heating level Four adsorption column C4, is cooled to 30 DEG C of <.This process is sample bottle source procedure processed.
In sample bottle, concentrated xenon sample is sent to and is carried out that radioactive xenon isotope is measured and total xenon concentration is measured, and obtains radioactivity and total xenon amount of xenon isotope in sample, and then calculates the activity concentration of radioactive xenon isotope in got surrounding air.
Sample bottle is the carbon window substrate stainless steel source capsule that can directly carry out γ measurement, the about 20ml of volume, and the concentration of xenon approximately 50% (v/v) in sample, obtains the about 10ml of total xenon amount (mark condition), effectively the about 115m of air sampling volume
3, the enrichment times of xenon is greater than to 5 × 10
6.
Aforementioned process is that the sampling process of a 24h adds follow-up concentrated, source processed and measuring process, according to this method operation, can realize long-term, serial sampling monitoring to radioactivity rare gas xenon in surrounding air.
This method has been used to develop movably split type atmosphere xenon sampler and movably atmospheric radioactivity nucleic monitoring station, serves the study on monitoring of atmosphere nuclear environment and prohibits the verification of core examination nucleic and study.
Claims (3)
1. a low temperature enrichment sampling method for xenon in atmosphere, is characterized in that: comprise the following steps:
1] cryosorption high temperature desorption:
Adopt the first order charcoal absorption desorption unit xenon in condensed air remove other impurity at low temperatures, adsorption temp is-70～-40 DEG C, desorption temperature is 110～200 DEG C, first order charcoal absorption desorption unit is warming up to after 110 DEG C, its desorption gas to second level adsorption column shift absorption, be heated to 200 DEG C and keep 20min after stop;
2] three grades of normal temperature absorbing high temp desorptions:
The adsorption column that adopts three cascades xenon in condensed air remove other impurity step by step at normal temperatures, adsorption temp is 10～30 DEG C, desorption temperature is 50～160 DEG C, second level adsorption column is warming up to 80 DEG C and keep after the 5min time, its desorption gas to third level adsorption column shift absorption, be heated to 160 DEG C and keep 10min after stop; Third level adsorption column is warming up to after 50 DEG C, its desorption gas to fourth stage adsorption column shift absorption, be heated to 160 DEG C and keep 5min after stop;
3] sample collection:
Afterbody adsorption column desorption xenon is out transferred to sample bottle through barrier film supercharging, completes collection.
2. the low temperature enrichment sampling method of xenon in atmosphere according to claim 1, is characterized in that: the acticarbon loading in first to adsorption columns at different levels before the concentrated sampling of enrichment carries out heat-activated.
3. the low temperature enrichment sampling method of xenon in atmosphere according to claim 1 and 2, it is characterized in that: described first order charcoal absorption desorption unit is the active carbon adsorption column of two cover parallel connections, described two covers active carbon adsorption column in parallel is realized alternately adsorption and desorption by valve.
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| 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 |
| CN107861145B (en) * | 2017-10-20 | 2023-06-16 | 苏州热工研究院有限公司 | Continuous monitoring system for radioactive inert gas in ambient air |
| CN109900845A (en) * | 2017-12-08 | 2019-06-18 | 南京天成环境科技工程有限公司 | A kind of Thermal desorption module of double cold-traps |
| CN109665506B (en) * | 2018-12-21 | 2020-11-06 | 北京放射性核素实验室 | Atmospheric xenon enrichment and purification method and device |
| CN109665505B (en) * | 2018-12-21 | 2020-11-06 | 北京放射性核素实验室 | Atmospheric xenon enrichment and purification method and device |
| CN109939538B (en) * | 2019-04-12 | 2020-07-28 | 中国原子能科学研究院 | System and method for rapidly separating Kr and Xe in complex fission product |
| CN112557158B (en) * | 2021-02-28 | 2021-05-28 | 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 |
| CN112557157B (en) * | 2021-02-28 | 2021-05-04 | 中国工程物理研究院核物理与化学研究所 | Method for separating, purifying and collecting xenon in air sample based on specific device |
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