CN106855473A - A kind of method for preparing the fluid sample of carbon 14 in live graphite - Google Patents
A kind of method for preparing the fluid sample of carbon 14 in live graphite Download PDFInfo
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- CN106855473A CN106855473A CN201611090947.1A CN201611090947A CN106855473A CN 106855473 A CN106855473 A CN 106855473A CN 201611090947 A CN201611090947 A CN 201611090947A CN 106855473 A CN106855473 A CN 106855473A
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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
Abstract
The invention discloses a kind of method for preparing the fluid sample of carbon 14 in live graphite, the method includes：The reaction vessel of one sealing is provided, there is a device of vapor sorption containing HTO in the reaction vessel, so as to the inner space of the reaction vessel is divided into the first space and second space；Live graphite sample is provided with first space, carbon dioxide absorbent solution is provided with the second space；Combustion-supporting gas is filled with reaction vessel to the sealing, the air pressure in the reaction vessel is reached 1MPa 4MPa by force；The live graphite sample is burnt in combustion-supporting gas, steam containing HTO and carbon dioxide are formed in first space；Kept for a period of time, the steam containing HTO and carbon dioxide is spread to the second space by the adsorbent equipment, the steam containing HTO is absorbed by the suctions, and the carbon dioxide by the absorbing liquid；Reaction vessel to the sealing is exhausted.
Description
Technical field
The present invention relates to nuclear industry technical field, more particularly to a kind of prepare carbon-14 fluid sample in live graphite
Method.
Background technology
Substantial amounts of graphite material, graphite can be used in nuclear industry can carry radioactivity after being subject to neutron irradiation.For treatment is put
Penetrating property graphite, it is necessary to set up contained radioactive analysis method in graphite, particularly will accurately determine containing for wherein carbon-14
Amount.The difficult point of carbon-14 analysis is that the carbon-14 in solid graphite material is prepared into fluid sample, is easy to follow-up using accurate
Radioassay instrument carbon-14 is analyzed.
Widely used at present is the fluid sample that " burning-absorption process " prepares carbon-14.That is, by the graphite containing carbon-14
Lighted in the combustion-supporting gas such as air or oxygen, make carbon conversion for carbon dioxide, then using absorbing liquid absorbing carbon dioxide.Due to putting
Also contain another radionuclide --- tritium in penetrating property graphite.The vapor containing tritium can be formed in combustion, also can be by
Absorbing liquid absorbs, therefore, the radioactivity survey to follow-up carbon-14 produces severe jamming.So before absorbing liquid, will there is one
The process of the individual vapor for going water removal to contain tritium.For example, Qiu Yongmei etc. is in reactor decommissioning graphite14C analyzes sample preparation experimental system
Develop (atomic energy science and technology, 2010, Vol.44 (suppl.)：The preparation method of continuous carbon-14 119-123) is reported in a text
And experimental provision.It prepares carbon-14 sample method and may be summarized to be：Graphite is heated into burning under oxygen atmosphere, gas passes through
Condenser pipe and silica gel drier are removed containing HTO, and carbon-14 fluid sample is prepared by the absorbing liquid in collector.However, should
Method and apparatus have as a drawback that：(1) equipment is complicated, part is more, volume is big, integrated level is poor；(2) be difficult to standardization,
Majority is the interim experimental provision built, and is unfavorable for large-scale production and promotes the use of；(3) control difficult：Gas flow rate is too small
When be unfavorable for that carbon dioxide is absorbed by liquid absorption completely when being unfavorable for that graphite burns completely, gas flow rate is too big；(4) radiate
Property waste is more：Whole pipeline can all be stain by carbon-14, tritium；(5) the dangerous property of equipment：Powdered graphite specific surface area is big, with oxygen
Gas mixing is easily exploded.
In order to partly solve the shortcoming of the above method, particularly for the consideration of safe operation, one kind is there is also at present to be made
The technology of carbon-14 sample is prepared with high pressure resistant sample combustion device (oxygen bomb).This kind of technology and as described before sample preparation side
Method is differed from：Introduce a kind of special sample combustion device (oxygen bomb).Specifically, the method is：It is close at one
Closing makes graphite generate carbon dioxide and steam containing HTO with oxygen combustion in high pressure resistant sample combustion device；Then by burner
Valve open, will burning generation carbon dioxide and steam containing HTO guide to similar to offers such as Qiu Yongmei except vapor and
In the device of absorbing carbon dioxide.However, the method and device still have as a drawback that：(1) in addition to sample combustion device, need
It is further provided with the device except steam containing HTO and absorbing carbon dioxide：Equipment is complicated, integrated level is poor, most needs are built temporarily
Water removal and absorbing carbon dioxide device, be unfavorable for that device is promoted the use of.If without corollary apparatus, the dry of detritiation cannot be gone
Disturb, it is difficult to for the accurate analysis of C-14；(2) bleed air operation of sample combustion device must control manually, working strength it is big：Sample
The operation that product burner is deflated is, it is necessary to reconcile a vent valve according to internal residual pressure, holding deflation speed is slowly steady
It is fixed.This operation at present can only be by manually controlling spiral vent valve to complete, and staff needs continuous a few hours to hold
Continuous to reconcile, working strength is very big；(3) manual bleed air operation causes to absorb unstable, and experimental error is big：Sample combustion device is released
Gas also require that and be slowly introducing HTO sorbing material and sodium hydroxide solution, the absorption by speed to HTO and carbon dioxide
Effect has a direct impact.Particularly, when that by excessive velocities absorptivity can be caused to decline, the carbon-14 content for determining is influenceed.But it is logical
The mode of remarkable industry control spiral vent valve adjusts deflation speed, and deflation velocity perturbation is big, the unstable, experimental error of absorption
Greatly, result poor repeatability.
Therefore it provides a kind of method of the simple and effective fluid sample for preparing carbon-14 in live graphite turns into current
The technical issues that need to address.
The content of the invention
The present invention provides a kind of simple and effective method for preparing carbon-14 fluid sample in live graphite.
A kind of method for preparing carbon-14 fluid sample in live graphite, the method includes：The reaction for providing a sealing is held
Device, has a device of vapor sorption containing HTO in the reaction vessel, so as to the inner space of the reaction vessel is divided into one the
One space and a second space；Live graphite sample is provided with first space, two are provided with the second space
Carbonoxide absorbing liquid；Combustion-supporting gas is filled with reaction vessel to the sealing, the air pressure in the reaction vessel is reached 1- by force
4MPa；The live graphite sample is burnt in combustion-supporting gas, steam containing HTO and two are formed in first space
Carbon oxide gas；Kept for a period of time, make the steam containing HTO and carbon dioxide by the adsorbent equipment to described
Second space spreads, and the steam containing HTO is by the suctions, and the carbon dioxide is by the absorbing liquid
Absorb；And the reaction vessel of the sealing is exhausted.
The method for preparing carbon-14 fluid sample in live graphite described above, wherein, the reaction vessel bag of the sealing
Include：One pressure-bearing steel cylinder, a top end cover, a closure, two electrodes and an ignition wire；The top end cover inserts the pressure-bearing
Within the open top of steel cylinder, be fixed on the top end cover on the pressure-bearing steel cylinder by the closure；Described two electrodes
It is arranged at intervals in the top end cover, and the pressure-bearing interior of steel bottle is extended to from outside, described two electrodes extends to institute
The one end for stating pressure-bearing interior of steel bottle is electrically connected by the ignition wire；The live graphite sample is set to be burnt in combustion-supporting gas
Method be to the ignition wire be powered.
The described above method for preparing carbon-14 fluid sample in live graphite, wherein, the adsorbent equipment includes one the
One breathable membrane, one are arranged at first breathable membrane with spaced second breathable membrane of first breathable membrane, one
And the second water vapor adsorption material and a rubber seal ring between breathable membrane.
The method for preparing carbon-14 fluid sample in live graphite described above, wherein, the inwall of the pressure-bearing steel cylinder is
Cylinder, the adsorbent equipment is cylinder or truncated cone-shaped, and its side is fitted with the inwall of the pressure-bearing steel cylinder, and close by rubber
Seal ring realizes side wall sealing.
The method for preparing carbon-14 fluid sample in live graphite described above, wherein, the water vapor adsorption material is
Bibulous Silica Gel.
The method for preparing carbon-14 fluid sample in live graphite described above, wherein, on the inwall of the pressure-bearing steel cylinder
Form step or set raised, so that the adsorbent equipment is fixed in the step or high spot.
The described above method for preparing carbon-14 fluid sample in live graphite, wherein, described two electrodes and ignition wire
It is arranged at first space；The Air inflating and exhausting valve is arranged on the pressure-bearing steel cylinder and is connected directly with the second space；
The method that combustion-supporting gas is filled with the reaction vessel of the sealing is to be filled with purity oxygen by the Air inflating and exhausting valve.
The method for preparing carbon-14 fluid sample in live graphite described above, wherein, the absorbing liquid is NaOH
Solution.
The method for preparing carbon-14 fluid sample in live graphite described above, wherein, a magnetic is placed in the absorbing liquid
Power rotor；It is described to make what the steam containing HTO and carbon dioxide were spread by the adsorbent equipment to the second space
Step is further included：Reaction vessel is put on a magnetic stirring apparatus, magnetic rotor is driven to the suction by magnetic force
Liquid is received to be stirred.
The method for preparing carbon-14 fluid sample in live graphite described above, wherein, what the absorbing liquid was stirred
Time is 5-10 minutes.
Compared to prior art, the method for the present invention makes the carbon dioxide after reaction in gas be diffused into up to absorbing alkali lye table
Face, it is to avoid the difficulty of the manual control deflation course guided by conduit, is not only reduced working strength, substantially increases sample
The efficiency of preparation, and artificial experimental error and uncertainty is reduced, improve the reliability of Sample Preparation Procedure.
Other features and advantages of the present invention will be illustrated in the following description, also, the partly change from specification
Obtain it is clear that or being understood by implementing the present invention.The purpose of the present invention and other advantages can be by the explanations write
Specifically noted structure is realized and obtained in book, claims and accompanying drawing.
Below by drawings and Examples, technical scheme is described in further detail.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, with reality of the invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the knot of the experimental provision of the fluid sample for preparing carbon-14 in live graphite provided in an embodiment of the present invention
Structure schematic diagram.
Fig. 2 is the method flow diagram of the fluid sample for preparing carbon-14 in live graphite provided in an embodiment of the present invention.
Drawing reference numeral explanation
| Experimental provision | 10 |
| Pressure-bearing steel cylinder | 101 |
| Top end cover | 102 |
| Closure | 103 |
| Electrode | 104 |
| Ignition wire | 105 |
| Sample crucible | 106 |
| Air inflating and exhausting valve | 107 |
| Beaker | 108 |
| Absorb alkali lye | 109 |
| Adsorbent equipment | 110 |
| First breathable membrane | 111 |
| Water vapor adsorption material | 112 |
| Second breathable membrane | 113 |
| Rubber seal ring | 114 |
| First space | 115 |
| Second space | 116 |
| Magnetic rotor | 117 |
Specific embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that preferred reality described herein
Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Refer to Fig. 1, the experimental provision of the fluid sample for preparing carbon-14 in live graphite provided in an embodiment of the present invention
10 include：One pressure-bearing steel cylinder 101, a top end cover 102,103, two electrodes 104 of a closure, an ignition wire 105, a sample
Crucible 106, an Air inflating and exhausting valve 107, a beaker 108, the device of vapor sorption containing HTO of carbon dioxide absorption alkali lye 109 and one
110。
The shape and size of the pressure-bearing steel cylinder 101 are not limited, and can be arranged as required to.It is appreciated that the pressure-bearing steel
Bottle 101 can also be the container that can bear high pressure prepared using other metal materials.In the present embodiment, the pressure-bearing steel cylinder
101 is cylinder, its side and sealed bottom, open top and with the screw thread coordinated with the closure 103.
It is that the top end cover 102 is used to constituting sealing with the pressure-bearing steel cylinder 101 and can bear the anti-of high pressure
Answer chamber.When using, the top end cover 102 is inserted within the open top of the pressure-bearing steel cylinder 101.
The closure 103 is used to for the top end cover 102 to be fixed on the pressure-bearing steel cylinder 101.The closure
103 structure can be arranged as required to.In the present embodiment, the closure 103 has the top with the pressure-bearing steel cylinder 101
The screw thread of cooperation, and the closure 103 is structure as a whole with the top end cover 102.When using, the closure 103 leads to
Cross spiral to be fixedly connected with the pressure-bearing steel cylinder 101, so as to push down the top end cover 102, it is ensured that sealing is intact.
Described two electrodes 104 are arranged at intervals in the top end cover 102, and extend to the pressure-bearing steel cylinder from outside
Inside 101.One end that described two electrodes 104 are exposed on the external is used to be connected with external power source, extends to the pressure-bearing steel cylinder 101
Internal one end is used for applied voltage, so as to realize igniting.The mode of the igniting is not limited, and can be arc discharge etc..Can be with
Understand, the set location of described two electrodes 104 is not limited in the top end cover 102, it is also possible to be arranged at the pressure-bearing steel
On bottle 101, as long as extending to the inside of the pressure-bearing steel cylinder 101 from outside.In the present embodiment, described two electrodes 104 prolong
The one end inside the pressure-bearing steel cylinder 101 is extended to be electrically connected by an ignition wire 105.In the case of external power source energization, pass through
Described two electrodes 104 and ignition wire 105 constitute a loop, and the ignition wire 105 can instantaneous ignition and itself fusing.It is described
Ignition wire 105 can ignite the graphite testing sample in the sample crucible 106, sample combustion is gasified.It is appreciated that the electricity
Pole 104 and ignition wire 105 are alternative construction, and the present invention can also realize igniting by other firing devices or ignition way, example
Such as whole reaction vessel is heated.
The sample crucible 106 is arranged in the pressure-bearing steel cylinder 101, for carrying graphite testing sample.The sample
Crucible 106 can be arranged in the fixing device in the pressure-bearing steel cylinder 101.In the present embodiment, the sample crucible 106 is consolidated
Due on an electrode 104, and the electrode 104 is arranged in the top end cover 102, such that it is able to open the top end
The sample crucible 106 is taken out from the pressure-bearing steel cylinder 101 while lid 102, to be mounted in sample.It is appreciated that institute
State sample crucible 106 and be not limited to crucible, as long as can be with resistant to elevated temperatures sample bearing device.
The Air inflating and exhausting valve 107 be used to burn before to being filled with the combustion-supporting gas such as oxygen in the pressure-bearing steel cylinder 101, burning and inhale
Harvest into the waste gas in the rear discharge pressure-bearing steel cylinder 101.The Air inflating and exhausting valve 107 can be arranged at the pressure-bearing steel cylinder 101
Above or in the top end cover 102.Preferably, the Air inflating and exhausting valve 107 is arranged on the pressure-bearing steel cylinder 101 and positioned at described
The back side of sample crucible 106, can so avoid in gas replenishment process, and air-flow blows the sample inside the sample crucible 106
Dissipate.The vent charge of existing apparatus is generally disposed in the top end cover 102, and just to the sample crucible of loading sample.
When device is filled with oxygen, charge air flow may blow away sample.In the present embodiment, the Air inflating and exhausting valve 107 is arranged at described
Pressure-bearing steel cylinder 101 is on the side wall of bottom.
It is described to be arranged in the pressure-bearing steel cylinder 101 containing adsorbent equipment 110, so as to by the inside of the pressure-bearing steel cylinder 101
Space is divided into one first space 115 and a second space 116.The sample crucible 106 is arranged at first space 115
It is interior.The adsorbent equipment 110 has multiple through holes, and the second space 116 of first space 115 and is only by the absorption dress
Put 110 connections.The steam containing HTO and carbon dioxide of reaction production can be by the absorption in first space 115
Device 110 spreads to the second space 116, and the steam containing HTO can be by the vapor in the adsorbent equipment 110
Sorbing material absorbs.The adsorbent equipment 110 includes that one first breathable membrane 111, sets with first breathable membrane 111 interval
The second breathable membrane 113, put is arranged at the vapor between the breathable membrane 113 of first breathable membrane 111 and second
The rubber seal ring 114 of sorbing material 112 and.Preferably, to be fixed on the rubber close at the edge of the second breathable membrane 113
In seal ring 114, so that a container is formed, to place the water vapor adsorption material 112.In the present embodiment, the adsorbent equipment
110 is cylinder or truncated cone-shaped, and its side is fitted with the inwall of the pressure-bearing steel cylinder 101, and realizes side by rubber seal ring 114
Wall is sealed.Step can be formed on the inwall of the pressure-bearing steel cylinder 101 or raised (not shown) is set, so that the absorption dress
Putting 110 can fix in the step or high spot.The water vapor adsorption material 112 can be Bibulous Silica Gel etc..The water suction
There are a large amount of spaces in the materials such as silica gel itself, when piling up with the common structure of first breathable membrane, 111 and second breathable membrane 113
Into the passage of gas free flow between the second space 116 of first space 115 and.
The beaker 108 is arranged in the second space 116 inside the pressure-bearing steel cylinder 101, for holding the absorption
Alkali lye 109.The absorption alkali lye 109 is used for absorbing carbon dioxide.It is appreciated that the beaker 108 can also hold for other
Absorb the container of alkali lye 109.In the present embodiment, the beaker 108 is arranged at the bottom of pressure-bearing steel cylinder 101.The absorption alkali
Liquid 109 is sodium hydrate aqueous solution.
Further, a magnetic rotor 117 can also be included in the beaker 108.The magnetic rotor 117 is used to stir institute
Absorption alkali lye 109 is stated, so as to accelerate absorption of the absorption alkali lye 109 to carbon dioxide.It is appreciated that the magnetic rotor
117 is alternative construction.
It is appreciated that the beaker 108, sample crucible 106 and carbon dioxide absorption alkali lye 109 generally not with other
Element production and sales together, are only put into the fluid sample of carbon-14 during the experimental provision 10 prepares live graphite, because
This, the beaker 108, sample crucible 106 and carbon dioxide absorption alkali lye 109 can be not understood to the one of the experimental provision 10
Part.
Fig. 2 is referred to, the embodiment of the present invention further provides for a kind of fluid sample for preparing carbon-14 in live graphite
Method.The method is comprised the following steps：
S11, there is provided the reaction vessel of a sealing, has a device of vapor sorption containing HTO 110 in the reaction vessel, so that
The inner space of the reaction vessel is divided into one first space 115 and a second space 116；Set in first space 115
It is equipped with live graphite sample, the second space 116 and is provided with carbon dioxide absorption alkali lye 109；
S12, is filled with the combustion-supporting gas of oxygen etc. in the reaction vessel to the sealing, make the air pressure in the reaction vessel strong
Reach 1-4MPa；
S13, makes the live graphite sample be burnt in combustion-supporting gas, is formed in first space 115 and contains tritium
Vapor and carbon dioxide；
S14, is kept for a period of time, make the steam containing HTO and carbon dioxide pass through the adsorbent equipment 110 to
The second space 116 spreads, and the steam containing HTO is absorbed by the adsorbent equipment 110, and the carbon dioxide quilt
The absorption alkali lye 109 absorbs；And
S15, the reaction vessel to the sealing is exhausted.
It is appreciated that in the step S14, the absorption with absorption alkali lye 109 to carbon dioxide, the He of the first space 115
In second space 116 carbon dioxide can spontaneous diffusion, after certain hour so that absorb alkali lye 109 in pressure-bearing steel cylinder 101 own
Carbon dioxide is fully absorbed.And in the prior art, gas after reaction is discharged from pressure-bearing reaction vessel, then guided by conduit
Steam containing HTO is absorbed in alkali lye by the adsorbent equipment and carbon dioxide.The method needs manual regulating flow, keeps
Flow is sufficiently small, it is to avoid produce influence to absorption detritiation effect, carbon dioxide absorption effect.And, with reaction vessel
Air pressure is gradually reduced, it is necessary to sustained manual adjusts to ensure stability of flow.In the step S14, can also further to described
Absorb alkali lye 109 to be stirred, so as to accelerate absorption of the absorption alkali lye 109 to carbon dioxide.
It is appreciated that experimental provision of the invention 10 and method, can not only prepare the liquid of carbon-14 in live graphite
Sample, it generates two or more gas with various after can be used for any reaction, and the gas having needs to be removed, and some gas is needed
The experiment to be collected.
The specific embodiment of the fluid sample method of carbon-14 in live graphite is below prepared for the present invention.
Embodiment 1
In the present embodiment, the method that the fluid sample of carbon-14 in live graphite is prepared using experimental provision 10 is as follows：
(1) closure 103 of the experimental provision 10 is opened, top end cover 102 is taken out；
(2) put well on the inner support below the top end cover 102 and load quality in sample crucible 106, product crucible 106
0.05-0.2g live graphite samples to be measured, and connect ignition wire 105；
(3) beaker 108 that will be equipped with fixed volume 5.0-20.0ml NaOH absorption alkali lye 109 is put into the pressure-bearing steel cylinder
101 bottoms；
(4) proper silica gel water vapor adsorption material 112, closing are loaded in HTO vapor sorption apparatus 110 as needed
After be put into inside the pressure-bearing steel cylinder 101, it is ensured that the inwall surrounding of the pressure-bearing steel cylinder 101 is sealed by the adsorbent equipment 110；
(5) top end cover 102 is reinstalled, loading electrode 104, ignition wire 105, sample crucible 106 and sample to be combusted should
In pressure-bearing steel cylinder 101；
(6) the helixseal lid 103 is sealed；
(7) appropriate high pressure oxygen is filled with from the Air inflating and exhausting valve 107, the internal pressure of pressure-bearing steel cylinder 101 is reached 1MPa-
4MPa；
(8) whole experimental provision 10 is placed in cold water domain, leak detection ensures that experimental provision 10 is sealed；
(9) connection electrode 104 arrives external power source, by external power source igniting lead fire silk 105 and graphite sample to be combusted
Product；
(10) after sample combustion is completed and is lowered the temperature, experimental provision 10 is put on a magnetic stirring apparatus, by magnetic
Magnetic rotor 117 pairs absorbs the stirring of alkali lye 109 5-10 minutes during power drives beaker 108, promotes the absorption alkali lye 109 in gas
The absorption of carbon dioxide；
(11) after carbon dioxide absorption is complete, the gas in the pressure-bearing steel cylinder 101 is discharged by the Air inflating and exhausting valve 107,
The velocity of discharge need not be considered, deflation course can be rapidly completed；
(12) closure 103 is opened, beaker 108 is taken out, the NaOH in beaker 108 absorbs alkali lye 109 after
Continuous analysis sample.
Absorb in experimental provision of the invention 10 and preparation method suction of the alkali lye 109 to carbon dioxide in gas to detect
Receipts situation, in the present embodiment, during the gas in the pressure-bearing steel cylinder 101 is discharged by the Air inflating and exhausting valve 107, by leading
The second NaOH that be first slowly introducing the gas of exclusion in another beaker by pipe is absorbed in alkali lye, is that second NaOH is inhaled
Receive alkali lye and further absorb the remaining carbon dioxide of gas.Result finds that second NaOH absorbs two of absorption in alkali lye
Carbonoxide is almost nil.As can be seen here, absorbing alkali lye 109 in experimental provision of the invention 10 and preparation method can be by the pressure-bearing
Carbon dioxide in steel cylinder 101 is fully absorbed.
The present invention has advantages below：Device of the invention will contain HTO vapor adsorption, carbon dioxide absorption and sample
The functions such as burning are all integrated in pressure-bearing interior of steel bottle, simple to operate；The method of the present invention makes the carbon dioxide in gas after reaction
It is diffused into up to absorbing alkali lye surface, it is to avoid the difficulty of the manual control deflation course guided by conduit, not only reduces work
Intensity, the efficiency of sample preparation is substantially increased, and reduce artificial experimental error and uncertainty, improve sample system
The reliability of standby process.
Obviously, those skilled in the art can carry out various changes and modification without deviating from essence of the invention to the present invention
God and scope.So, if these modifications of the invention and modification belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising these changes and modification.
Claims (10)
1. a kind of method for preparing carbon-14 fluid sample in live graphite, the method includes：
The reaction vessel of sealing is provided, there is in the reaction vessel device of vapor sorption containing HTO, so that by the reaction vessel
Inner space is divided into the first space and second space；Live graphite sample, described second are provided with first space
Carbon dioxide absorbent solution is provided with space；
Combustion-supporting gas is filled with reaction vessel to the sealing, the air pressure in the reaction vessel is reached 1MPa-4MPa by force；
The live graphite sample is burnt in combustion-supporting gas, steam containing HTO and dioxy are formed in first space
Change carbon gas；
Kept for a period of time, make the steam containing HTO and carbon dioxide by the adsorbent equipment to the second space
Diffusion, the steam containing HTO is absorbed by the suctions, and the carbon dioxide by the absorbing liquid；
Reaction vessel to the sealing is exhausted.
2. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 1, it is characterised in that described close
The reaction vessel of envelope includes：Pressure-bearing steel cylinder, top end cover, closure, two electrodes and ignition wire；The top end cover inserts institute
State within the open top of pressure-bearing steel cylinder, be fixed on the top end cover on the pressure-bearing steel cylinder by the closure；Described two
Individual electrode gap is arranged in the top end cover, and extends to the pressure-bearing interior of steel bottle from outside, and described two electrodes prolong
The pressure-bearing interior of steel bottle is extended, is electrically connected by the ignition wire；The live graphite sample is set to be fired in combustion-supporting gas
The method of burning is to be powered to the ignition wire.
3. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 2, it is characterised in that the suction
Adsorption device includes the first breathable membrane and spaced second breathable membrane of first breathable membrane, is arranged at described first
Water vapor adsorption material and rubber seal ring between breathable membrane and the second breathable membrane.
4. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 3, it is characterised in that described to hold
The inwall of compressed steel bottle is cylinder, and the adsorbent equipment is cylinder or truncated cone-shaped, and its side is pasted with the inwall of the pressure-bearing steel cylinder
Close, and realize that side wall is sealed by rubber seal ring.
5. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 3, it is characterised in that the water
Vapor-adsorbing materials are Bibulous Silica Gel.
6. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 2, it is characterised in that described to hold
Step is formed on the inwall of compressed steel bottle or sets raised, so that the adsorbent equipment is fixed in the step or high spot.
7. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 2, it is characterised in that described two
Individual electrode and ignition wire are arranged at first space；The Air inflating and exhausting valve be arranged on the pressure-bearing steel cylinder and directly with it is described
Second space is connected；The method that combustion-supporting gas is filled with the reaction vessel of the sealing is to be filled with purity oxygen by the Air inflating and exhausting valve.
8. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 1, it is characterised in that the suction
Receipts liquid is sodium hydroxide solution.
9. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 1, it is characterised in that the suction
A magnetic rotor is placed in receipts liquid；It is described to make the steam containing HTO and carbon dioxide by the adsorbent equipment to described
The step of second space spreads further includes：Reaction vessel is put on a magnetic stirring apparatus, magnetic is driven by magnetic force
Power rotor is stirred to the absorbing liquid.
10. the method for preparing carbon-14 fluid sample in live graphite as claimed in claim 9, it is characterised in that the suction
The time that receipts liquid is stirred is 5-10 minutes.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611090947.1A CN106855473A (en) | 2016-12-01 | 2016-12-01 | A kind of method for preparing the fluid sample of carbon 14 in live graphite |
| PCT/CN2017/113937 WO2018099428A1 (en) | 2016-12-01 | 2017-11-30 | Method for preparing liquid sample of carbon-14 in radioactive graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611090947.1A CN106855473A (en) | 2016-12-01 | 2016-12-01 | A kind of method for preparing the fluid sample of carbon 14 in live graphite |
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| Publication Number | Publication Date |
|---|---|
| CN106855473A true CN106855473A (en) | 2017-06-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611090947.1A Pending CN106855473A (en) | 2016-12-01 | 2016-12-01 | A kind of method for preparing the fluid sample of carbon 14 in live graphite |
Country Status (2)
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| WO (1) | WO2018099428A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018099428A1 (en) * | 2016-12-01 | 2018-06-07 | 清华大学 | Method for preparing liquid sample of carbon-14 in radioactive graphite |
| WO2018099429A1 (en) * | 2016-12-01 | 2018-06-07 | 清华大学 | Experimental device for preparing liquid sample of carbon-14 in radioactive graphite |
| CN110672778A (en) * | 2019-10-31 | 2020-01-10 | 上海屹尧仪器科技发展有限公司 | Oxygen combustion reaction kettle capable of being ignited by microwave |
| CN113295498A (en) * | 2021-06-09 | 2021-08-24 | 广州海洋地质调查局 | Organic sulfur's extraction element in kerogen |
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| WO2018099429A1 (en) * | 2016-12-01 | 2018-06-07 | 清华大学 | Experimental device for preparing liquid sample of carbon-14 in radioactive graphite |
| CN110672778A (en) * | 2019-10-31 | 2020-01-10 | 上海屹尧仪器科技发展有限公司 | Oxygen combustion reaction kettle capable of being ignited by microwave |
| CN110672778B (en) * | 2019-10-31 | 2022-03-01 | 上海屹尧仪器科技发展有限公司 | Oxygen combustion reaction kettle capable of being ignited by microwave |
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| WO2018099428A1 (en) | 2018-06-07 |
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