CN107063784A - 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 - Google Patents
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 Download PDFInfo
- Publication number
- CN107063784A CN107063784A CN201610928785.8A CN201610928785A CN107063784A CN 107063784 A CN107063784 A CN 107063784A CN 201610928785 A CN201610928785 A CN 201610928785A CN 107063784 A CN107063784 A CN 107063784A
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- China
- Prior art keywords
- metal valve
- trap
- cold
- gas
- xenon
- Prior art date
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- Granted
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052724 xenon Inorganic materials 0.000 title claims abstract description 58
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000605 extraction Methods 0.000 title claims abstract description 51
- 238000000746 purification Methods 0.000 title claims abstract description 46
- 239000007789 gas Substances 0.000 claims abstract description 98
- 239000011521 glass Substances 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000000284 extract Substances 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims abstract description 5
- 238000009849 vacuum degassing Methods 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims description 187
- 239000002184 metal Substances 0.000 claims description 187
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 86
- 229910052802 copper Inorganic materials 0.000 claims description 86
- 239000010949 copper Substances 0.000 claims description 86
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 76
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 59
- 239000002808 molecular sieve Substances 0.000 claims description 58
- 238000005070 sampling Methods 0.000 claims description 58
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 52
- 239000010935 stainless steel Substances 0.000 claims description 35
- 229910001220 stainless steel Inorganic materials 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 229910052743 krypton Inorganic materials 0.000 claims description 24
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 24
- 150000002500 ions Chemical class 0.000 claims description 17
- 210000002445 nipple Anatomy 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 230000010355 oscillation Effects 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 8
- 230000000740 bleeding effect Effects 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 230000006641 stabilisation Effects 0.000 claims description 5
- 238000011105 stabilization Methods 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 241000544061 Cuculus canorus Species 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 238000001819 mass spectrum Methods 0.000 claims 1
- 238000000527 sonication Methods 0.000 claims 1
- 230000000155 isotopic effect Effects 0.000 abstract description 4
- 239000000523 sample Substances 0.000 description 30
- 229920001296 polysiloxane Polymers 0.000 description 17
- 238000007789 sealing Methods 0.000 description 9
- 238000012546 transfer Methods 0.000 description 7
- 229910001315 Tool steel Inorganic materials 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000003915 air pollution Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000007872 degassing Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910001423 beryllium ion Inorganic materials 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 210000000080 chela (arthropods) Anatomy 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000012611 container material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
- G01N1/34—Purifying; Cleaning
Abstract
Field is determined the invention belongs to gas dissolved water content and isotopics, specific open extraction purification system and its method for extraction and purification for being used for dissolving xenon in water, the system includes water sample and discharged and dissolved gas extraction system, and the purification for gas and piece-rate system connected with water sample release and dissolved gas extraction system;This method is as follows:Step 1, vacuum degassing is toasted to whole system;Step 2, discharge water sample and extract gas;Step 3, gas is shifted to glass cold-trap;Step 4, gas is shifted to purification system;Step 5, the gas step 6 of precipitation is further dried, the absorption of active gases is removed;Step 7, the separation of xenon.The present invention solves the vapor in xenon extracts separation process and removes not thorough, the incomplete problem of xenon separation.
Description
Technical field
Field is determined the invention belongs to gas dissolved water content and isotopics, and in particular to one kind is used for molten in water
Solve the extraction purification system and its method for extraction and purification of xenon.
Background technology
Dissolving xenon and the measure of isotopics have non-in terms of core military project and civilian nuclear power plant leakage monitoring in water
Often important Detectable effects, under conditions of air pollution is avoided, it is to complete rationally to sample and extract dissolving xenon therein completely
Xenon content and the premise of isotopics in water.
In terms of sampling, domestic basic using glass tube and in the glass valve sealing sampling of its two ends, this mode has
Two drawbacks:1) there is dead angle in valve, it is difficult to drive air bubble 2 away completely) glass container material leak rate is larger, deposits for a long time
Air can be caused, which to be exchanged with gas dissolved water, causes pollution, and external a few experiments room is sampled using copper pipe, and sampling is used after terminating
Pressing tongs compresses sealing, and this mode overcomes the shortcoming of glass container sample mode, but is compressing sealed process with pressing tongs
In, the degree of compression is difficult to grasp, and success rate is not high, it is often more important that, in copper pipe during water sample release, pressing tongs at sealing
It is to be unclamped under atmospheric environment, then again with opening copper pipe under atmospheric environment with locking pliers in 90 ° of planes of sealing surface, it is easy to
Copper pipe is damaged, causes air pollution.
In water sample in terms of xenon extraction purification, existing laboratory is removed using liquid nitrogen cold trap or alcohol-dry ice trap
Vapor, but this is it is difficult to ensure that the thorough removal of vapor, it is easy to tester is polluted;In separation inert gas
In in other gas process in addition to xenon, using the difference of gas condensation temperature, using the low temperature cold pump equipped with activated carbon
Separate successively, and xenon still has xenon to be attracted to activated carbon surface at a temperature of 325K, this temperature has reached low
The temperature upper limit of the cold pump of temperature, therefore be difficult that thoroughly will dissolve xenon in water be completely separated, this water sample also to extremely low content xenon
Test causes very big difficulty.
The content of the invention
It is used for the extraction purification system of dissolving xenon and its extraction purification side in water it is an object of the invention to provide a kind of
Method, solves security reliability of the water sample from sampling copper pipe into xenon extraction purification systematic procedure, and xenon extracts separation process
Middle vapor removes not thorough, the incomplete problem of xenon separation.
Realize the technical scheme of the object of the invention:A kind of extraction purification system for being used in water dissolve xenon, the system bag
Include water sample release and dissolved gas extraction system, and discharge with water sample and the purification for gas that connects of dissolved gas extraction system and
Piece-rate system.
Described water sample release and dissolved gas extraction system include the sampling anaerobic after threeway cutting ferrule seal nipple, pinch off
Copper pipe, copper pipe fracturing equipment, stainless steel cylinder, supersonic oscillations instrument, the first metal valve, the 3rd metal valve and first are without oil molecule
Pump group, threeway cutting ferrule seal nipple top is provided with the sampling oxygen-free copper pipe after pinch off, and threeway cutting ferrule seal nipple bottom is provided with copper
Pipe fracturing equipment, threeway cutting ferrule seal nipple right-hand member connection purification for gas piece-rate system, sampling copper pipe connects through the sealing of threeway cutting ferrule
Head, and sampling copper pipe bottom is in copper pipe fracturing equipment;Copper pipe fracturing equipment bottom is provided with stainless steel cylinder, and stainless bottom of steel cylinder is placed
In in supersonic oscillations instrument;Threeway cutting ferrule seal nipple side exit respectively with the 3rd metal valve, the first metal valve one
The outlet of end connection, the other end of the first metal valve and the first dry molecular pump group.
Described copper pipe fracturing equipment includes bellows, drive rod and glass window, and sampling copper pipe bottom is located at copper pipe pressure
Split and bellows be provided with the ram position of the drive rod of device, the housing side of copper pipe fracturing equipment, drive rod one end is located at outside housing,
The drive rod other end runs through housing, bellows;Copper pipe fracturing equipment center is provided with glass window.
Described purification for gas and piece-rate system include the first Pirani gauge, glass cold-trap, the first molecular sieve cold-trap, second
Pirani gauge, the first getter pump, activated carbon cold-trap, the second getter pump, the second molecular sieve cold-trap, ion gauge, the second molecule
Pump group, low temperature cold pump, mass spectrograph, small volume container and132The of Xe calibrating gas bottles, water sample release and dissolved gas extraction system
The other end of three metal valves one end respectively with the first Pirani gauge, the entrance of glass cold-trap are connected, the outlet point of glass cold-trap
One end, the entrance of the second molecular sieve cold-trap, one end of the first getter pump not with the first molecular sieve cold-trap are connected, the second molecule
The outlet of sieve cold-trap is connected with one end, one end of the second Pirani gauge, activated carbon cold-trap of the second getter pump;Activated carbon cold-trap
One end respectively with small volume container, mass spectrometric air inlet, one end of low temperature cold pump, one end of ion gauge, the second molecular pump
The bleeding point connection of group, the bleeding point of the second molecule pump group, ion gauge also discharge with water sample and dissolved gas extraction system goes out
Mouth connection.
Be provided with the 4th metal valve between described glass cold-trap outlet and the first molecular sieve cold-trap, the 4th metal valve with
Fifth metal valve is provided between the entrance of second molecular sieve cold-trap, is set successively between the 4th metal valve and the first getter pump
There are the 6th metal valve, the 7th metal valve;The 8th metal is sequentially provided between described activated carbon cold-trap and small volume container
Valve, the tenth metal valve;Described small volume container with132The 9th metal valve is provided between Xe calibrating gas bottles;Described
The 11st metal valve, the 16th metal valve are sequentially provided between 8th metal valve and mass spectrometric air inlet;11st
The bleeding point of the 15th metal valve, the 11st metal valve and the second molecule pump group is provided between metal valve and low temperature cold pump
Between be sequentially provided with the 14th metal valve, the 13rd metal valve;14th metal valve be located at the second molecule pump group with from
Between cuckoo, the of the 14th metal valve, the 13rd metal valve, ion gauge and water sample release and dissolved gas extraction system
It is provided with and the second metal valve between three metal valves.
A kind of to be used for the method for the extraction purification of dissolving xenon in water, this method specifically includes following steps:
Step 1, vacuum degassing is toasted to whole system;
Step 2, discharge water sample and extract gas;
Step 3, gas is shifted to glass cold-trap;
Step 4, gas is shifted to purification system;
Step 5, the gas of precipitation is further dried;
Step 6, the absorption of active gases is removed;
Step 7, the separation of xenon.
Described step 2 specifically includes following steps:The first metal valve, the 3rd metal valve are closed, copper pipe pressure break is twisted
The drive rod of device, drive rod compress bellows utilize the sampling oxygen-free copper pipe bottom after the retractility pressure break pinch off of bellows
Sealing;The water sample inflow monitored by glass window in the sampling oxygen-free copper pipe after pressure break sampling oxygen-free copper pipe, pinch off is stainless
In steel cylinder, open sonic oscillation instrument and accelerate gas evolution;
Described step 3 specifically includes following steps:Close on the 4th metal valve, glass cold-trap and put liquid nitrogen, contain
The bubbing of vapor is chilled in glass cold-trap;
Described step 4 specifically includes following steps:The liquid nitrogen on glass cold-trap is removed, it is heated, makes condensed gas
Fully gasification, glass cold-trap puts alcohol-dry ice, until the first Pirani gauge registration is down to stably, closing fifth metal valve,
6th metal valve;First molecular sieve cold-trap puts liquid nitrogen, opens the 4th metal valve, the precipitation gas containing a small amount of vapor
Body is chilled in the first molecular sieve cold-trap;
Described step 1 specifically includes following steps:Close the second metal valve, the 4th metal valve, the tenth metal
Valve, the 16th metal valve, open remaining metal valve, heating belt switch are opened, with the first dry molecular pump group and second
Dry molecular pump group is vacuumized to whole system.
Described step 5 specifically includes following steps:Close the 7th metal valve, the 8th metal valve, activated carbon cold-trap
Put liquid nitrogen, remove the liquid nitrogen on the first molecular sieve cold-trap and it is heated, the bubbing containing vapor passes through the
Two molecular sieve traps are transferred to during activated carbon, and the second molecular sieve trap carries out vapor to it and is adsorbed by drying;Remove activated carbon
Liquid nitrogen on cold-trap is simultaneously heated to it, while the liquid nitrogen on set on the first molecular sieve cold-trap, and bubbing again passes by the
Two molecular sieve traps are transferred in the first molecular sieve cold-trap, and the second molecular sieve further carries out water vapor adsorption drying to it;So
Back and forth, until the second Pirani gauge registration is down to its Lower Range, the 6th metal valve is opened, activated carbon cold-trap puts liquid nitrogen,
The residual gas of the first molecular sieve cold-trap is set to be transferred to completely in activated carbon cold-trap.
Described step 6 specifically includes following steps:After bubbing is dried, heating of Activated charcoal cold-trap is opened second and inhaled
Gas agent pump heater switch, makes it heat up, and quick adsorption removes substantial amounts of active gases beyond rare gas, opens the 7th metal valve
Door, the first getter pump further adsorbs a small amount of active gases, only remains argon gas, three kinds of inert gases of Krypton and xenon.
Described step 7 specifically includes following steps:Low temperature cold pump temperature is adjusted to K, the 14th metal valve is closed, beats
The 16th metal valve is opened, argon gas, Krypton and xenon inert gas are fully transferred in low temperature cold pump, the 16th metal is closed
Valve, low temperature cold pump first heats up to cool afterwards;The 13rd metal valve, the 14th metal valve are opened, Krypton is taken away, until ion
Advise registration and decline stabilization, Krypton is removed completely, Krypton heating, Krypton release;The 15th metal valve is opened, Krypton is taken away, directly
Stable to ion gauge registration, Krypton is removed completely, and extraction, purifying and the separating step of xenon are completed in water.
The advantageous effects of the present invention:The water sample of the present invention is under vacuum conditions, from sampling copper pipe in fracturing equipment
Discharged to system, will not be by air pollution, it is ensured that discharge the safe and reliable of process;After release to system, in connection gas analysis
In the stainless steel cylinder and the pipeline of glass cold-trap gone out, the stainless steel bar with the only poor 0.6mm of tubing internal diameter is put into, xenon can ensured
On the premise of gas transfer completely, suppress transfer of the water vapour to xenon purifies and separates system well;The glass cold-trap of design can
To monitor the amount of transfer process vapor, to prevent excessive vapor contaminated system;In normal temperature molecular sieve in purifies and separates system
Trap both sides set molecular sieve cold-trap and activated carbon cold-trap respectively, it is possible to achieve the xenon iterative cycles for being mixed with vapor are dried, and
The degree that gas removes water vapour is monitored by the second Pirani gauge;Designed between molecular sieve cold-trap and activated carbon cold-trap by the 6th
The pipeline of metal valve connection, can avoid a small amount of xenon because molecular sieve trap resistance is larger and can not thoroughly be transferred to activated carbon
The problem of trap;Design the first getter pump and the second getter pump, and air-breathing at different temperatures, it is ensured that active gases
Absorption completely;Design the stainless steel tube contacted with low temperature cold pump be not charged with activated carbon, although compared to equipped with activated carbon not
Rust steel pipe needs lower temperature condensed gas, but may insure the complete release of xenon, is particularly suitable for extremely low content molten
Solve the analysis of xenon water sample.
Brief description of the drawings
A kind of structural representation for water sampling device that Fig. 1 is carried for the present invention;
Fig. 2 is a kind of structural representation for being used in water dissolve the extraction purification system of xenon provided by the present invention.
In figure:
1 is the first silicone tube, and 2 be the cambered surface tool steel chuck of clamp, and 3 be the first stainless steel lathe dog, and 4 be sampling oxygen-free copper
Pipe, 5 be the second stainless steel lathe dog, and 6 be the second silicone tube, and 7 be the 3rd stainless steel lathe dog, and 8 be blade water pump, and 9 be the 4th stainless
Steel clamping band, 10 be the 3rd silicone tube, and 11 be the sampling oxygen-free copper pipe after pinch off, and 12 be threeway cutting ferrule seal nipple, and 13 be copper pipe
Fracturing equipment, 14 be bellows, and 15 be drive rod, and 16 be stainless steel cylinder, and 17 be glass window, and 18 be sonic oscillation instrument, and 19 are
First dry molecular pump group, 20 be the first metal valve, and 21 be the second metal valve, and 22 be the 3rd metal valve, and 23 be first
Pirani gauge, 24 be stainless steel bar, and 25 be glass cold-trap, and 26 be the 4th metal valve, and 27 be molecular sieve cold-trap, and 28 be hardware
Belong to valve, 29 be the 6th metal valve, and 30 be the second Pirani gauge, and 31 be the first getter pump, and 32 be the 7th metal valve, 33
It is the 9th metal valve for the 8th metal valve, 34,35 be the tenth metal valve, and 36 be the 11st metal valve, and 37 be activity
Charcoal cold-trap, 38 be the second getter pump, and 39 be the 12nd metal valve, and 40 be the second zeolite cold-trap, and 41 be ion gauge, and 42 be the
13 metal valves, 43 be the second molecule pump group, and 44 be the 14th metal valve, and 45 be the 15th metal valve, and 46 be the tenth
Six metal valves, 47 be mass spectrograph, and 48 be low temperature cold pump, and 49 be small volume container.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
As shown in figure 1, a kind of water sampling device for being carried of the present invention, the device includes the first silicone tube 1, clamp, the
One stainless steel lathe dog 3, sampling oxygen-free copper pipe 4, the second stainless steel lathe dog 5, the second silicone tube 6, the 3rd stainless steel lathe dog 7, blade
Water pump 8, the 4th stainless steel lathe dog 9, the 3rd silicone tube 10, the water inlet of blade water pump 8 pass through the 3rd silicone tube 10 with water sample to be measured
Connection, and the 3rd silicone tube 10 is clamped with the 4th stainless steel lathe dog 9, the delivery port of blade water pump 8 passes through the second silicone tube 6 and sampling
The one end of oxygen-free copper pipe 4 is connected, and one end of the neighbouring delivery port of blade water pump 8 is pressed from both sides with the 3rd stainless steel lathe dog 7 on the second silicone tube 6
Tightly, one end of neighbouring sampling oxygen-free copper pipe 4 is clamped with the second stainless steel lathe dog 5 on the second silicone tube 6, sampling oxygen-free copper pipe 4 and
First silicone tube 1 is clamped by the first stainless steel lathe dog 3.The cambered surface tool steel chuck 2 of clamp is located at adjacent on sampling oxygen-free copper pipe 4
The position of nearly first stainless steel lathe dog 3.
The contact surface material of the cambered surface tool steel chuck 2 of clamp and sampling oxygen-free copper pipe 4 is tool steel, and contact surface is several
What is shaped as semicircular arc.
The probe tube of sampling oxygen-free copper pipe 4 forms for 1/4inch oxygen-free copper pipes welding 1/2inch oxygen-free copper pipes, and passes through
Degassing is toasted in 600 DEG C of vacuum drying ovens.
First silicone tube 1, the second silicone tube 6, the 3rd silicone tube 10 are transparent silicon sebific duct, sampling oxygen-free copper pipe 4 and silicon
The connection of sebific duct is clamped using stainless steel lathe dog, with preventing water leakage.
As shown in figure 1, provided by the present invention a kind of using water sampling device progress water sample sampling method, this method bag
Include following steps:
Step 1, by the water sampling device connected sampling oxygen-free copper pipe 4 vertically place
It is delivery port to sample the upper end of oxygen-free copper pipe 4, and sampling oxygen-free copper pipe 4 lower end is water inlet.
The water inlet for sampling oxygen-free copper pipe 4 is 1/2inch ends, and delivery port is 1/4inch ends.
Step 2, by water sample to be measured introduce sampling oxygen-free copper pipe 4
The power supply of blade water pump 8 is opened, water sample to be measured is passed sequentially through into blade water pump 8, the 3rd silicone tube 10, the second silicone tube
6 introduce sampling oxygen-free copper pipes 4, and constantly tap sampling oxygen-free copper pipe 4 and drive bubble away, until the of sampling oxygen-free copper pipe 4 two ends
One transparent silicon sebific duct 1 and the equal bubble-free of the second transparent silicon sebific duct 6, it was demonstrated that water sample bubble-free in sampling oxygen-free copper pipe 4.
Step 3, pinch off sampling oxygen-free copper pipe 4, sampling are completed
The upper end delivery port of oxygen-free copper pipe 4 is sampled with the pinch off first of cambered surface tool steel chuck 2 of clamp, then pinch off sampling nothing
The lower end water inlet of oxygen copper pipe 4.
Gas disposal is gone because sampling oxygen-free copper pipe 4 passes through high-temperature vacuum, tube wall has good ductility and viscosity, with folder
The cambered surface tool steel chuck 2 of pincers can be directly by its pinch off, and tube wall viscosity realizes sampling oxygen-free copper pipe 4 delivery port, water inlet
Pinched-off seal at mouthful, by water seal to be measured in sampling oxygen-free copper pipe 4, sampling is completed.
After the upper end delivery port of sampling oxygen-free copper pipe 4 and lower end water inlet in pinch off Fig. 1, sampling oxygen-free copper pipe 4 is inverted
The sampling oxygen-free copper pipe 11 formed afterwards after pinch off as shown in Figure 2.
As shown in Fig. 2 a kind of extraction purification system for being used in water dissolve xenon, the system includes water sample and discharges and dissolve
Gas extraction system, purification for gas and piece-rate system.Water sample discharges and dissolved gas extraction system includes the sealing of threeway cutting ferrule and connect
First 12, after pinch off sampling oxygen-free copper pipe 11, copper pipe fracturing equipment 13, stainless steel cylinder 16, supersonic oscillations instrument 18, the first metal valve
The 20, the 3rd metal valve 22 of door and the first dry molecular pump group 19.What the upper end connection clip of threeway cutting ferrule seal nipple 12 was had no progeny takes
Sample oxygen-free copper pipe 11, the lower end connecting copper pipe fracturing equipment 13 of threeway cutting ferrule seal nipple 12, the right-hand member of threeway cutting ferrule seal nipple 12 connects
Connect purification for gas piece-rate system.Sample the ram position that the bottom of copper pipe 11 is located at the drive rod 15 of copper pipe fracturing equipment 13, copper pipe pressure
Splitting device 13 includes being provided with bellows 14, drive rod in housing, bellows 14, drive rod 15 and glass window 17, housing side
15 one end are located at outside housing, and the other end of drive rod 15 runs through housing, bellows 14;Drive rod 15 is carbon steel material, drive rod 15
By screw drive, sampled using the retractility pressure break of bellows 14 at the sealing of the bottom of copper pipe 11;The center of copper pipe fracturing equipment 13 is set
There is glass window 17, glass window 17 is welded on the metal flange of housing, metal flange leans on copper with copper pipe fracturing equipment 13
Packing ring is sealed.Copper pipe fracturing equipment 13 is connected and sealed with the stainless steel cylinder 16 positioned at its housing bottom by snap joint,
The stainless bottom of steel cylinder 16 is positioned in supersonic oscillations instrument 18.The side exit of threeway cutting ferrule seal nipple 12 by pipeline respectively with
One end connection of 3rd metal valve 22, the first metal valve 20, the other end of the first metal valve 20 passes through pipeline and first
The outlet of dry molecular pump group 19.
As shown in Fig. 2 purification for gas and piece-rate system include the first Pirani gauge 23, the second metal valve 21, stainless steel
Rod 24, alcohol-dry ice glass cold-trap 25, the 4th metal valve 26, the first molecular sieve cold-trap 27, fifth metal valve the 28, the 6th
Metal valve 29, the second Pirani gauge 30, the first getter pump 31, the 7th metal valve 32, the 8th metal valve 33, the 9th gold medal
Belong to valve 34, the tenth metal valve 35, the 11st metal valve 36, activated carbon cold-trap 37, the second getter pump 38, the 12nd gold medal
Belong to valve 39, the second molecular sieve cold-trap 40, ion gauge 41, the 13rd metal valve 42, the second molecule pump group 43, the 14th metal
Valve 44, the 15th metal valve 45, the 16th metal valve 46, low temperature cold pump 48, mass spectrograph 47, the and of small volume container 49132Xe calibrating gas bottles 50.The other end of 3rd metal valve 22 of water sample release and dissolved gas extraction system is distinguished by pipeline
The other end, the air inlet of the first Pirani gauge 23, the air inlet of glass cold-trap 25 with the second metal valve 21 are connected, stainless steel bar
24 are located in the pipeline between threeway metal ferrule seal nipple 12 and glass cold-trap 25, and the gas outlet of glass cold-trap 25 passes through pipeline
Connected with one end of the 4th metal valve 26, the other end of the 4th metal valve 26 by pipeline respectively with the first molecular sieve cold-trap
27th, one end of fifth metal valve 28, one end connection of the 6th metal valve 29.The other end of fifth metal valve 28 passes through pipe
Road is connected with the second molecular sieve cold-trap 40, and the second molecular sieve cold-trap 40 is connected by one end of pipeline and the 12nd metal valve 39
It is logical, the other end of the 12nd metal valve 39 by pipeline respectively with the air inlet of the second getter pump 38, the second Pirani gauge 30
Air inlet, activated carbon cold-trap 37 connects.Activated carbon cold-trap 37 by pipeline respectively with the other end of the 6th metal valve 29, the 7th
One end of metal valve 32, one end connection of the 8th metal valve 33, the other end of the 7th metal valve 32 pass through pipeline and the
The air inlet of one getter pump 31 is connected.The other end of 8th metal valve 33 by pipeline respectively with the tenth metal valve 35,
One end connection of 11 metal valves 36;The other end of tenth metal valve 35 is connected by the gas outlet of pipeline and small volume container 49
Logical, the air inlet of small volume container 49 is connected by pipeline with one end of the 9th metal valve 34, the 9th metal valve 34 it is another
One end passes through pipeline132The gas outlet connection of Xe calibrating gas bottles 50.The other end of 11st metal valve 36 by pipeline respectively with
14th metal valve 44, the 15th metal valve 45, one end connection of the 16th metal valve 46, the 16th metal valve 46
The other end connected by pipeline with the air inlet of mass spectrograph 47.The other end of 15th metal valve 45 passes through pipeline and low temperature
Cold pump 48 is connected.Air inlet, ten three metal of the other end of 14th metal valve 44 by pipeline respectively with ion gauge 41
One end of valve 42, the other end connection of the second metal valve 21, the other end of the 13rd metal valve 42 pass through pipeline and the
The bleeding point connection of two molecule pump groups 43.
Whole system pipeline all 316L stainless steel materials in addition to glass cold-trap 25, pipeline inner wall passes through special polishing entirely
Processing, each metal vacuum part is connected using VCR ultrahigh vacuum seal modes.
The two ends of glass cold-trap 25 have metal transfer to cut down to be connected with other metal tubes respectively.
The external diameter of stainless steel bar 24 is 4mm, long 5mm, is placed horizontally in 1/4inch stainless steel tubes.
Molecular sieve bore diameter is 5A in the first molecular sieve cold-trap 27, and the molecular sieve bore diameter of the second molecular sieve cold-trap 40 is 3A.
The low temperature cold pump 48 is that the cold-trap of condensed gas is the stainless steel tube for not placing activated carbon.
As shown in Fig. 2 a kind of enter to dissolve xenon in water-filling using the above-mentioned extraction purification system for being used for dissolving xenon in water
Extraction purification method, this method specifically includes following steps:
Step 1, vacuum degassing is toasted to whole system
The second metal valve 21, the 4th metal valve 26, the tenth metal valve 35, the 16th metal valve 46 are closed, is beaten
Remaining metal valve is opened, heating belt switch is opened, with 43 pairs of the whole series of the first dry molecular pump group 19 and the second dry molecular pump group
System vacuumizes 24h.
Step 2, discharge water sample and extract gas
The first metal valve 20, the 3rd metal valve 22 are closed, the drive rod 15 of copper pipe fracturing equipment 13 is twisted, drive rod 15 is pressed
Contracting bellows 14, utilizes the sealing of sampling oxygen-free copper pipe 11 bottom after the retractility pressure break pinch off of bellows 14;Pass through glass
The water sample in sampling oxygen-free copper pipe 11 after the monitoring pressure break sampling oxygen-free copper pipe 11 of observation window 17, pinch off flows into stainless steel bottle 16
It is interior, open sonic oscillation instrument 18 and accelerate gas evolution.
Step 3, gas is shifted to glass cold-trap 25
Close on the 4th metal valve 26, glass cold-trap 25 and put liquid nitrogen, the bubbing containing a large amount of vapor is cold
Freeze to glass cold-trap 25, transfer time 5min.
Step 4, gas is shifted to purification system
The liquid nitrogen on glass cold-trap 25 is removed, it is heated, condensed gas is fully gasified, glass cold-trap 25 puts wine
Essence-dry ice, until the first Pirani gauge shows that 23 numbers are down to stabilization, closes fifth metal valve 28, the 6th metal valve 29;First
Molecular sieve cold-trap 27 puts liquid nitrogen, opens the 4th metal valve 26, and the bubbing containing a small amount of vapor is chilled to the
In one molecular sieve cold-trap 27, transfer time about 5min.
Step 5, the gas of precipitation is further dried
The 7th metal valve 32, the 8th metal valve 33 are closed, activated carbon cold-trap 37 puts liquid nitrogen, removes the first molecular sieve
Liquid nitrogen on cold-trap 27 is simultaneously heated to it, and the bubbing containing a small amount of vapor is transferred to by the second molecular sieve trap 40
During activated carbon, the second molecular sieve trap 40 carries out vapor to it and is adsorbed by drying;Remove the liquid nitrogen on activated carbon cold-trap 37
And it is heated, while liquid nitrogen on being covered on the first molecular sieve cold-trap 27, bubbing again passes by the second molecular sieve trap
40 are transferred in the first molecular sieve cold-trap 27, and the second molecular sieve 40 further carries out water vapor adsorption drying to it;And so on,
Until the second Pirani gauge registration is down to its Lower Range, the 6th metal valve 29 is opened, activated carbon cold-trap 37 puts liquid nitrogen, made
The residual gas of first molecular sieve cold-trap 27 is transferred in activated carbon cold-trap 37 completely.
Step 6, the absorption of active gases is removed
After bubbing is dried, heating of Activated charcoal cold-trap 37 is opened the heater switch of the second getter pump 38, is allowed to warm to
450 DEG C, quick adsorption removes substantial amounts of active gases, about 10min beyond rare gas, opens the 7th metal valve 32, first
Getter pump 31 further adsorbs a small amount of active gases, and about 10min only remains argon gas, three kinds of inert gases of Krypton and xenon.
Step 7, the separation of xenon
The temperature of low temperature cold pump 48 is adjusted to 45K, the 14th metal valve 44 is closed, the 16th metal valve 46 is opened, will
Argon gas, Krypton and xenon inert gas are fully transferred in low temperature cold pump 48, keep 3min, close the 16th metal valve 46,
Low temperature cold pump 48 is warming up to 200K, keeps 3min, is then cooled to 60K, keeps 3min;Open the 13rd metal valve 42,
14 metal valves 44, take substantial amounts of Krypton away, until the registration of ion gauge 41 declines stabilization, Krypton is removed completely, Krypton heating
To 140K, Krypton release keeps 3min;The 15th metal valve 45 is opened, a small amount of Krypton is taken away, until the registration of ion gauge 41 is steady
Fixed, Krypton is removed completely, and extraction, purifying and the separating step of xenon are completed in water.
The first molecular sieve cold-trap 27 and activated carbon cold-trap 37 are heated to be metal heating coil in above-mentioned step, remaining pipe
Road is using the heating of common heating band.
The second molecular sieve trap 40 only adsorbs water vapour under normal temperature condition in above-mentioned steps, without covering liquid nitrogen frozen.
250 DEG C of baking degassings of whole system, are closed behind heating tape, the first Pirani gauge registration is less than 1.0 in above-mentioned steps
×10-3Mbar, ion gauge registration is less than 1.0 × 10-8mbar。
The purpose of stainless steel bar 24 in above-mentioned steps before glass cold-trap 25 in pipeline is that gas transfer process suppresses vapor
Pass through.
The first asepwirator pump 31 is operates in above-mentioned steps under normal temperature, primary attachment hydrogen, and the second zirconium aluminium pump 38 is at 450 DEG C
Operation, other active gases of primary attachment;
Active gases in the step refers to all gas in addition to inert gas.
The present invention is explained in detail above in conjunction with drawings and examples, but the present invention is not limited to above-mentioned implementation
Example, in the knowledge that those of ordinary skill in the art possess, can also make on the premise of present inventive concept is not departed from
Go out various change.The content not being described in detail in the present invention can use prior art.
Claims (13)
1. a kind of extraction purification system for being used in water dissolve xenon, it is characterised in that:The system includes water sample and discharges and dissolve
Gas extraction system, and the purification for gas and piece-rate system connected with water sample release and dissolved gas extraction system.
2. a kind of extraction purification system for being used in water dissolve xenon according to claim 1, it is characterised in that:Described
Water sample discharge and dissolved gas extraction system include threeway cutting ferrule seal nipple (12), pinch off after sampling oxygen-free copper pipe (11),
Copper pipe fracturing equipment (13), stainless steel cylinder (16), supersonic oscillations instrument (18), the first metal valve (20), the 3rd metal valve
(22) and the first dry molecular pump group (19), threeway cutting ferrule seal nipple (12) top is provided with the sampling oxygen-free copper pipe after pinch off
(11), threeway cutting ferrule seal nipple (12) bottom is provided with copper pipe fracturing equipment (13), the connection of threeway cutting ferrule seal nipple (12) right-hand member
Purification for gas piece-rate system, sampling copper pipe (11) runs through threeway cutting ferrule seal nipple (12), and sampling copper pipe (11) bottom is located at
In copper pipe fracturing equipment (13);Copper pipe fracturing equipment (13) bottom is provided with stainless steel cylinder (16), and stainless steel cylinder (16) bottom is positioned over super
In sonication instrument (18);Threeway cutting ferrule seal nipple (12) side exit respectively with the 3rd metal valve (22), the first metal
The outlet of one end connection of valve (20), the other end of the first metal valve (20) and the first dry molecular pump group (19).
3. a kind of extraction purification system for being used in water dissolve xenon according to claim 2, it is characterised in that:Described
Copper pipe fracturing equipment (13) includes bellows (14), drive rod (15) and glass window (17), and sampling copper pipe (11) bottom is located at
Bellows is provided with the ram position of the drive rod (15) of copper pipe fracturing equipment (13), the housing side of copper pipe fracturing equipment (13)
(14), drive rod (15) one end is located at outside housing, and drive rod (15) other end runs through housing, bellows (14);Copper pipe fracturing equipment
(13) center is provided with glass window (17).
4. a kind of extraction purification system for being used in water dissolve xenon according to claim 3, it is characterised in that:Described
Purification for gas and piece-rate system include the first Pirani gauge (23), glass cold-trap (25), the first molecular sieve cold-trap (27), the second skin
La Ni rule (30), the first getter pump (31), activated carbon cold-trap (37), the second getter pump (38), the second molecular sieve cold-trap
(40), ion gauge (41), the second molecule pump group (43), low temperature cold pump (48), mass spectrograph (47), small volume container (49) and132Xe
Calibrating gas bottle (50), water sample release and dissolved gas extraction system the 3rd metal valve (22) the other end respectively with the first skin
The La Ni rule one end of (23), the entrance connection of glass cold-trap (25), glass cold-trap (25) outlet respectively with the first molecular sieve cold-trap
(27) one end, the entrance of the second molecular sieve cold-trap (40), one end connection of the first getter pump (31), the second molecular sieve cold-trap
(40) outlet is connected with one end, one end of the second Pirani gauge (30), activated carbon cold-trap (37) of the second getter pump (38);
Activated carbon cold-trap (37) one end respectively with small volume container (49), the air inlet of mass spectrograph (47), the one of low temperature cold pump (48)
End, one end of ion gauge (41), the second molecule pump group (43) bleeding point connection, the bleeding point of the second molecule pump group (43), from
Cuckoo (41) also with water sample discharge and dissolved gas extraction system outlet.
5. a kind of extraction purification system for being used in water dissolve xenon according to claim 4, it is characterised in that:Described
Glass cold-trap (25) is exported is provided with the 4th metal valve (26), the 4th metal valve (26) between the first molecular sieve cold-trap (27)
Fifth metal valve (28), the 4th metal valve (26) and the first air-breathing are provided between the entrance of the second molecular sieve cold-trap (40)
The 6th metal valve (29), the 7th metal valve (32) are sequentially provided between agent pump (31);Described activated carbon cold-trap (37) with
The 8th metal valve (33), the tenth metal valve (35) are sequentially provided between small volume container (49);Described small volume container
(49) with132The 9th metal valve (34) is provided between Xe calibrating gas bottles (50);The 8th described metal valve (33) and mass spectrum
The 11st metal valve (36), the 16th metal valve (46) are sequentially provided between the air inlet of instrument (47);11st metal valve
The 15th metal valve (45), the 11st metal valve (36) and the second molecular pump are provided between door (36) and low temperature cold pump (48)
The 14th metal valve (44), the 13rd metal valve (42) are sequentially provided between the bleeding point of group (43);14th metal valve
Door (44) is located between the second molecule pump group (43) and ion gauge (41), the 14th metal valve (44), the 13rd metal valve
(42), it is provided with and the second gold medal between ion gauge (41) and water sample release and the 3rd metal valve (22) of dissolved gas extraction system
Belong to valve (21).
6. enter to dissolve xenon in water-filling using a kind of extraction purification system for being used for dissolving xenon in water described in claim 5
Extraction purification method, it is characterised in that this method specifically includes following steps:
Step 1, vacuum degassing is toasted to whole system;
Step 2, discharge water sample and extract gas;
Step 3, gas is shifted to glass cold-trap (25);
Step 4, gas is shifted to purification system;
Step 5, the gas of precipitation is further dried;
Step 6, the absorption of active gases is removed;
Step 7, the separation of xenon.
7. the method for the extraction purification of xenon is dissolved in water according to claim 6, it is characterised in that described step 1
Specifically include following steps:
Close the second metal valve (21), the 4th metal valve (26), the tenth metal valve (35), the 16th metal valve
(46) remaining metal valve, is opened, heating belt switch is opened, with the first dry molecular pump group (19) and the second dry molecular pump group
(43) whole system is vacuumized.
8. the method for the extraction purification of xenon is dissolved in water according to claim 7, it is characterised in that described step 2
Specifically include following steps:
The first metal valve (20), the 3rd metal valve (22) are closed, the drive rod (15) of copper pipe fracturing equipment (13), drive rod is twisted
(15) compress bellows (14), utilize the close of sampling oxygen-free copper pipe (11) bottom after the retractility pressure break pinch off of bellows (14)
Envelope;The water in the sampling oxygen-free copper pipe (11) after pressure break sampling oxygen-free copper pipe (11), pinch off is monitored by glass window (17)
Sample is flowed into stainless steel cylinder (16), is opened sonic oscillation instrument (18) and is accelerated gas evolution.
9. the method for the extraction purification of xenon is dissolved in water according to claim 8, it is characterised in that described step 3
Specifically include following steps:
The 4th metal valve (26) is closed, glass cold-trap puts liquid nitrogen on (25), and the bubbing containing vapor is chilled to
In glass cold-trap (25).
10. the method for the extraction purification of xenon is dissolved in water according to claim 9, it is characterised in that described step 4
Specifically include following steps:
The liquid nitrogen on glass cold-trap (25) is removed, it is heated, condensed gas is fully gasified, glass cold-trap (25) puts wine
Essence-dry ice, until the first Pirani gauge shows that (23) number is down to stabilization, closes fifth metal valve (28), the 6th metal valve
(29);First molecular sieve cold-trap (27) puts liquid nitrogen, opens the 4th metal valve (26), the precipitation gas containing a small amount of vapor
Body is chilled in the first molecular sieve cold-trap (27).
11. the method for the extraction purification of xenon is dissolved in water according to claim 10, it is characterised in that described step
5 specifically include following steps:
The 7th metal valve (32), the 8th metal valve (33) are closed, activated carbon cold-trap (37) puts liquid nitrogen, removes the first molecule
Sieve the liquid nitrogen on cold-trap (27) and it is heated, the bubbing containing vapor, which passes through the second molecular sieve trap (40), to be shifted
To activated carbon, the second molecular sieve trap (40) carries out vapor to it and is adsorbed by drying;Remove on activated carbon cold-trap (37)
Liquid nitrogen and it is heated, while putting liquid nitrogen on the first molecular sieve cold-trap (27), bubbing again passes by second
Molecular sieve trap (40) is transferred in the first molecular sieve cold-trap (27), and the second molecular sieve (40) further carries out water vapor adsorption to it
Dry;And so on, until the second Pirani gauge registration is down to its Lower Range, the 6th metal valve (29), activated carbon are opened
Cold-trap (37) puts liquid nitrogen, the residual gas of the first molecular sieve cold-trap (27) is transferred to completely in activated carbon cold-trap (37).
12. the method for the extraction purification of xenon is dissolved in water according to claim 11, it is characterised in that described step
Rapid 6 specifically include following steps:
After bubbing is dried, heating of Activated charcoal cold-trap (37) opens the second getter pump (38) heater switch, it is heated up,
Quick adsorption removes substantial amounts of active gases beyond rare gas, opens the 7th metal valve (32), the first getter pump (31)
A small amount of active gases is further adsorbed, argon gas, three kinds of inert gases of Krypton and xenon are only remained.
13. the method for the extraction purification of xenon is dissolved in water according to claim 12, it is characterised in that described step
7 specifically include following steps:
Low temperature cold pump (48) temperature is adjusted to (45) K, the 14th metal valve (44) is closed, the 16th metal valve is opened
(46), argon gas, Krypton and xenon inert gas are fully transferred in low temperature cold pump (48), the 16th metal valve is closed
(46), low temperature cold pump (48) first heats up cools afterwards;The 13rd metal valve (42), the 14th metal valve (44) are opened, is taken away
Krypton, until ion gauge (41) registration declines stabilization, Krypton is removed completely, Krypton heating, Krypton release;Open the 15th metal
Valve (45), takes Krypton away, until ion gauge (41) registration is stable, Krypton is removed completely, the extraction of xenon in water, purifying and point
Completed from step.
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