CN107132095A - A kind of source system processed measured for carbon 14 - Google Patents
A kind of source system processed measured for carbon 14 Download PDFInfo
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- CN107132095A CN107132095A CN201710468189.0A CN201710468189A CN107132095A CN 107132095 A CN107132095 A CN 107132095A CN 201710468189 A CN201710468189 A CN 201710468189A CN 107132095 A CN107132095 A CN 107132095A
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- source system
- system processed
- reaction vessel
- state
- carbon
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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 belongs to environment measuring field, and in particular to it is a kind of for carbon 14 measure source system processed, including successively closed connection to generate CO2Generating means, to dry CO2Drying device, to determine CO2The detector of amount and to absorb CO2Form the absorption plant of sample source, second channel of the detector at least with the first passage being connected with the outlet side of the drying device and with the first passage independence, provided with the conversion equipment that can be switched between the first state and a second state between the detector and the absorption plant, when the conversion equipment is in first state, absorption plant absorbs CO2, when the conversion equipment is in the second state, absorption plant stops absorbing CO2, after above technical scheme, CO can be realized2Quantitative adsorption, the sample source of carbon 14 of stable obtained different content, whole-process automatic control and implementation prevent the influence of human factor, detection efficient is high, easy to operate, and stability is high.
Description
Technical field
The invention belongs to environment measuring field, and in particular to a kind of source system processed measured for carbon-14, applied to sky
The detection of carbon-14 in gas and water and biological sample.
Background technology
14One of C is a kind of natural radionuclide, while be also the topmost radionuclide of nuclear facilities discharge, half
The phase declined for 5730, launches pure beta ray, the keV of ceiling capacity 156.Consider14C energy is relatively low, and most suitably used measuring method is
Spectrometer is dodged by liquid to measure.In consideration of it, traditional14C sources method is that precipitation of calcium carbonate is mixed with scintillation solution, and colloidal sample is made
Source, this method advantage is can be quantitatively adding calcium carbonate powder, it is ensured that measurement system is consistent, simple to operate, has the disadvantage detection efficient
Low, the Sample storage time is relatively short.In recent years, another set of source method processed is proposed, passes through organic base/inorganic Alkali absorption CO2Afterwards
Sample source is made, this method advantage is that detection efficient is high, and the holding time is long, has the disadvantage complex operation, CO2Uptake is unstable,
Cause detection limit and uncertainty fluctuation larger.
The content of the invention
The invention aims to make up the defect of existing measuring method, thus provide it is a kind of for carbon-14 measure
Full automatic source system processed, whole process passes through programme-control and implementation, it is possible to achieve CO2Quantitative adsorption, easy to operate, stability
It is high.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of source system processed measured for carbon-14, bag
Include closed connection successively to generate CO2Generating means, to dry CO2Drying device, to determine CO2The spy of amount
Survey device and to absorb CO2The absorption plant of sample source is formed, the detector at least has to go out with the drying device
The connected first passage in gas end and the second channel with the first passage independence, the detector and the absorption plant it
Between provided with the conversion equipment that can switch between the first state and a second state, when the conversion equipment is in first state
When, the inlet end of the outlet side of the first passage, the absorption plant and the second channel is sequentially connected logical；Work as institute
When stating conversion equipment in the second state, the conversion equipment is directly by the outlet side of the first passage and the second channel
Inlet end be connected.
Further, the source system processed also includes with the conversion device signal being connected and controlling the conversion equipment to exist
The control device switched between the first state and second state, when the detector detect through described
The CO that one passage enters2Amount and the CO flowed out from the second channel2When difference between amount is less than preset value, the converting means
Put in the first state；The CO entered through the first passage detected when the detector2Amount with from described second
The CO of passage outflow2When difference between amount reaches preset value, the conversion equipment is changed to second state.
Further, the conversion equipment is plane four-way valve, and the absorption plant is provided with air inlet pipe and escape pipe, described
Wherein two mouths of pipe of plane four-way valve outlet side respectively with the first passage, the inlet end of the second channel are connected, institute
Other two mouth of pipe for stating plane four-way valve is connected with the air inlet pipe and escape pipe of the absorption plant respectively.
Further, the CO2Generating means includes reaction vessel, is connected with the reaction vessel and is used to described anti-
Addition absorption in container is answered to have CO2NaOH absorbing liquids the first reagent bottle and be connected with the reaction vessel and be used to
The second reagent bottle of HCl solution is added in the reaction vessel, provided with the between first reagent bottle and the reaction vessel
One peristaltic pump, between second reagent bottle and the reaction vessel be provided with the second peristaltic pump, the source system processed also include with
The reaction vessel is connected to the 3rd peristaltic pump by the waste liquid discharge after terminating is reacted.
Further, the source system processed also includes the inert gas feeding mechanism being connected with the reaction vessel, described
Gas flowmeter is provided between inert gas feeding mechanism and the reaction vessel.
Further, pH sensors are additionally provided with the reaction vessel, the exterior bottom of the reaction vessel, which is provided with, to be stirred
Mix device.
Further, the absorption plant include liquid flashing counting bottle, detachable cover located at the liquid flashing counting bottle top will
Scintillation solution and CO are provided with the sealed seal of liquid flashing counting bottle, the liquid flashing counting bottle2Absorbing liquid.
Further, the absorption plant also includes the semiconductor cooler and temperature located at liquid flashing counting bottle outer wall
Sensor.
Further, the absorption plant also includes the Motorized lift device located at liquid flashing counting bottle exterior bottom,
The Motorized lift device includes to the lifting platform of support liquid flashing counting bottle and the stepping electricity to drive lifting of lifting table
Provided with the position-sensing switch being connected with the stepper motor in machine, the lifting platform.
Further, the source system processed also includes the feeding device to be fed into the absorption plant, institute
Stating feeding device is included to contain the 3rd reagent bottle of scintillation solution, to contain CO2The 4th reagent bottle, the Yi Jiyi of absorbing liquid
End and the 3rd reagent bottle and the 4th reagent bottle be respectively connected with that the other end and the liquid flashing counting bottle be connected it is automatic enter
Sample pump.
Due to the utilization of above-mentioned technical proposal, the present invention has following advantages compared with prior art：The present invention will absorb
There is CO2NaOH solution be transferred to reaction vessel, pass through pH sensors control add HCl solution speed, inert gas supply
Device is by the CO of desorption2Carry away and sequentially pass through drying device, CO2First passage, absorption plant and the CO of detector2Visit
The second channel of device is surveyed, by the real time measure by first passage and the CO of second channel2Amount, absorption plant suction can be measured in real time
The CO of receipts2Amount, when the uptake of absorption plant reaches setting value, control device switch transition device makes the outlet side of first passage
It is connected with the inlet end of second channel, residual gas is expelled directly out without absorption plant, so as to realize CO2Quantitative adsorption,
And the carbon-14 sample source that different content is made can be stablized, detection efficient is high.Whole-process automatic control of the present invention and implementation, Du
The influence of exhausted human factor, operating in a key is easy to operate, and stability is high.
Brief description of the drawings
Accompanying drawing 1 is used for the structural representation for the source system processed that carbon-14 is measured for a kind of of the present invention.
Wherein, 1, generating means；101st, reaction vessel；102nd, the first reagent bottle；103rd, the second reagent bottle；104th, stirring dress
Put；105th, the first peristaltic pump；106th, the second peristaltic pump；107th, the 3rd peristaltic pump；108th, pH sensors；2nd, drying device；3rd, visit
Survey device；301st, first passage；302nd, second channel；4th, absorption plant；401st, liquid flashing counting bottle；402nd, semiconductor cooler；
403rd, temperature sensor；404th, Motorized lift device；5th, plane four-way valve；6th, inert gas feeding mechanism；7th, gas flowmeter；
8th, feeding device；801st, the 3rd reagent bottle；802nd, the 4th reagent bottle；803rd, auto injection pump；804th, plane triple valve.
Embodiment
Below in conjunction with the accompanying drawings and embodiment the invention will be further described.
As shown in figure 1, it is a kind of for carbon-14 measure source system processed, including successively closed connection to generate CO2's
Generating means 1, to dry CO2Drying device 2, to determine CO2The detector 3 of amount and to absorb CO2Form sample
The absorption plant 4 in product source, the detector 3 at least have the first passage 301 that is connected with the outlet side of the drying device 2 with
And the second channel 302 independent with the first passage 301, provided with can be the between the detector 3 and the absorption plant 4
The conversion equipment switched between one state and the second state.
When the conversion equipment is in first state, the outlet side of the first passage 301, the absorption plant 4, with
And the inlet end of the second channel 302 is sequentially connected logical, the now absorption of absorption plant 4 CO2；When the conversion equipment is in the
The outlet side of the first passage 301 is directly connected by two-state, the conversion equipment with the inlet end of the second channel 302
It is logical, CO2It is no longer pass through absorption plant 4.
The source system processed also includes with the conversion device signal being connected and controlling the conversion equipment described first
The control device switched between state and second state（Do not indicated in figure）.When the He of first passage 301 of detector 3
The CO that second channel 302 passes through2When the difference of amount is less than preset value, the controlled device control of conversion equipment is in first state,
CO2Pass sequentially through first passage 301, absorption plant 4 and second channel 302.The real time measure is logical by first passage 301 and second
The CO in road 3022Amount, the CO passed through when first passage 301 and second channel 3022When the difference of amount reaches preset value, conversion equipment
The control of controlled device simultaneously switches to the second state, and absorption plant 4 stops absorbing CO2。
Conversion equipment in the present embodiment is a plane four-way valve 5, and the absorption plant 4 is provided with air inlet pipe and outlet
Pipe, wherein two mouths of pipe of the plane four-way valve 5 outlet sides respectively with the first passage 301, the second channel 302
Inlet end is connected, the air inlet pipe and escape pipe phase of other two mouth of pipe of the plane four-way valve 5 respectively with the absorption plant 4
Even.First passage 301 is used to measure CO in container2Total amount, second channel 302 is used to measure unabsorbed CO2Amount.
Drying device 2 includes drying tube and the discoloration silica gel being arranged in drying tube, and discoloration silica gel is to absorb what is passed through
Vapor in gas.
CO2Generating means 1 includes reaction vessel 101, is connected with the reaction vessel 101 and is used to the reaction vessel
Absorption is added in 101 CO2NaOH absorbing liquids the first reagent bottle 102 and be connected and be used to the reaction vessel 101
The second reagent bottle 103 of HCl solution is added into reaction vessel 101.
Accurately to control the transfer rate and conveying capacity of NaOH absorbing liquids and HCl solution, in the first reagent bottle 102 and reaction
First peristaltic pump 105 is set between container 101, second peristaltic pump is set between the second reagent bottle 103 and reaction vessel 101
106。
The pH in pH sensors 108, the reaction vessel 101 that pH sensors 108 are measured in real time is additionally provided with reaction vessel 101
Value is to control the 3rd peristaltic pump 107 to add HCl speed and conveying total amount into reaction vessel 101.
In addition, being also provided with the 3rd peristaltic pump 107 being connected with reaction vessel 101, the 3rd peristaltic pump 107 will be that will react
Waste liquid after end is discharged from reaction vessel 101.
To make, reactant is well mixed, accelerate reaction speed, and agitating device is installed in the exterior bottom of reaction vessel 101
104.Agitating device 104 in the present embodiment is magnetic stirring apparatus.
The source system processed also includes the inert gas feeding mechanism 6 being connected with the reaction vessel 101, the indifferent gas
Gas flowmeter 7 is provided between body feeding mechanism 6 and the reaction vessel 101.Inert gas in the present embodiment uses nitrogen.
The absorption plant includes liquid flashing counting bottle, detachable cover and the liquid is dodged into meter located at liquid flashing counting bottle top
Scintillation solution and CO are provided with several bottles of sealed seals, the liquid flashing counting bottle2Absorbing liquid.
Absorption plant 4 includes liquid flashing counting bottle 401 and detachable cover above liquid flashing counting bottle 401 by institute
State in liquid flashing counting 401 sealed seals of bottle, liquid flashing counting bottle 401 and be provided with scintillation solution and CO2Absorbing liquid.In the present embodiment
CO2Absorbing liquid is Carbsorb absorbing liquids.
Liquid flashing counting bottle 401 outer wall be provided with semiconductor cooler 402 and temperature sensor 403, temperature sensor 403 with
Semiconductor cooler 402 is connected and controls semiconductor system by the temperature of measured liquid flashing counting 401 internal liquids of bottle
Cooler 402 works.The temperature range that liquid in liquid flashing counting bottle 401 is controlled in the present embodiment is -10 ~ 0 DEG C, it is possible to reduce flicker
Liquid and the volatilization of Carbsob absorbing liquids, while improving CO2Absorption efficiency.
It is preferred that, the lower end of the air inlet pipe of absorption plant 4 is located at scintillation solution and CO2Below the liquid level of absorbing liquid, it will absorb
The lower end of the escape pipe of device 4 is located at scintillation solution and CO2Above the liquid level of absorbing liquid, so as to further improve CO2Absorption efficiency.
Liquid flashing counting 401 exterior bottoms of bottle are additionally provided with Motorized lift device 404.Motorized lift device 404 includes support liquid
Dodge and be provided with and stepper motor phase in the lifting platform of counting vial 401 and the stepper motor to drive lifting of lifting table, lifting platform
Position-sensing switch even, so that it is guaranteed that liquid flashing counting bottle 401 reaches specified location and is connected with seal, now liquid flashing counting bottle
401 bottle sealing.
The source system processed also includes the feeding device 8 fed into the absorption plant 4.Feeding device 8 includes using
To contain the 3rd reagent bottle 801 of scintillation solution, to contain CO24th reagent bottle 802 of absorbing liquid and one end and described the
Three reagent bottles 801 and the 4th reagent bottle 802 are respectively connected with the auto injection pump that the other end is connected with the absorption plant 4
803.In the present embodiment, lead between the 3rd reagent bottle 801, the 4th reagent bottle 802 and absorption plant 4 and auto injection pump 803
Plane triple valve 804 is crossed to be connected.
Agitating device 104, the first peristaltic pump 105, the second peristaltic pump 106, the 3rd peristaltic pump 107, pH in the present embodiment
Sensor 108, detector 3, semiconductor cooler 402, temperature sensor 403, Motorized lift device 404, plane four-way valve 5,
Inert gas feeding mechanism 6, auto injection pump 803 and plane triple valve 804 are electrically connected with control device, so that whole
By programme-control and implementation, prevent the influence of human factor, easy to operate, stability is high.
Explanation produces the detailed process for the measuring sample source of carbon-14 using the source system processed of the present embodiment below.
It should be noted that following steps are only to produce a certain specific embodiment of carbon-14 measurement sample source, it is impossible in this, as
Restriction to the function, structure or performance that are used for the source system processed that carbon-14 is measured of the present invention.
Step 1：The NaOH absorbing liquids that sample preparation is obtained are added in the first reagent bottle 102, are added in the second reagent bottle 103
2mol/L HCl solution, scintillation solution is added in the 3rd reagent bottle 801, and Carbsorb is added in the 4th reagent bottle 802 and is absorbed
Liquid flashing counting bottle 401 is placed on liquid, electric lifting platform.
Step 2：Start control program, by electric lifting platform by liquid flashing counting bottle 401 rise to be connected with seal and
Make bottle sealing, open inert gas feeding mechanism 6, nitrogen enters system by gas flowmeter 7, and gas flow control is
10mL/min, is purged more than 5 minutes, the air in removing system.
Step 3：NaOH absorbing liquids are added by reaction vessel 101 by the first peristaltic pump 105, start magnetic stirrer, control
Rotating speed processed is 600r/min；Start CO2Detector 3, starts to walk baseline；Semiconductor cooler 402 is controlled by liquid flashing counting bottle 401
Interior temperature is down to -10 DEG C；Auto injection pump 803 is controlled to extract 11.00mL scintillation solutions from the 3rd reagent bottle 801 respectively, from the
9.00mL Carbsorb absorbing liquids are extracted in four reagent bottles 802 into liquid flashing counting bottle 401.
Step 4：When temperature sensor 403 shows -10 DEG C, added by the second peristaltic pump 106 into reaction vessel 101
HCl solution, until the reading of pH sensors 108 is shown as 7.0.
Step 5：While starting the second peristaltic pump 106, CO2Detector 3 starts measurement and record data, now plane four
Port valve 5 is in first state, i.e. gas from CO2The first passage 301 of detector 3 is flowed into, and enters liquid flashing counting through plane four-way valve 5
Bottle 401, then enter CO through plane four-way valve 52The second channel 302 of detector 3 flows out.
Step 6：Treat CO2Uptake reaches aim parameter, the state of switching surface four-way valve 5 to the second, i.e., gas is without liquid
Dodge counting vial 401 and be directly entered CO2The second channel 302 of detector 3 flows out.
Step 7：When the registration of pH sensors 108 is, the 3rd peristaltic pump 107 is closed, binary channels is stopped after being kept for 10 minutes
CO2The data acquisition of detector 3.
Step 8：The second peristaltic pump 106 is opened, waste liquid is discharged, liquid flashing counting bottle 401, lid are removed by electric lifting platform
Upper bottle cover, it is to be measured.
Step 9：Close semiconductor cooler 402, EP (end of program).Close inert gas feeding mechanism 6.
After above technical scheme, the present invention is by inert gas feeding mechanism 6 by the CO of desorption2Carry away and according to
Secondary process drying device 2, CO2First passage 301, absorption plant 4 and the CO of detector 32The second channel 302 of detector 3, leads to
The real time measure is crossed by first passage 301 and the CO of second channel 3022Amount, the CO of the absorption of absorption plant 4 can be measured in real time2Amount,
When the uptake of absorption plant 4 reaches setting value, control device switch transition device to the second state, so that first passage
301 outlet side is connected with the inlet end of second channel 302, and residual gas is expelled directly out without absorption plant 4, so as to realize
CO2Quantitative adsorption, and the carbon-14 sample source that different content is made can be stablized, detection efficient is high.The present invention is whole-process automatic
Control and implementation, prevent the influence of human factor, operating in a key is easy to operate, and stability is high.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent change or modification that Spirit Essence is made, should all be included within the scope of the present invention.
Claims (10)
1. a kind of source system processed measured for carbon-14, it is characterised in that：Including closed connection successively to generate CO2Hair
Generating apparatus, to dry CO2Drying device, to determine CO2The detector of amount and to absorb CO2Form sample source
Absorption plant, the detector at least has the first passage that is connected with the outlet side of the drying device and with described first
The second channel of passage independence, being provided between the detector and the absorption plant can be between the first state and a second state
The conversion equipment switched over, when the conversion equipment is in first state, the outlet side of the first passage, the absorption
The inlet end of device and the second channel is sequentially connected logical；When the conversion equipment is in the second state, the conversion
The outlet side of the first passage is directly connected by device with the inlet end of the second channel.
2. a kind of source system processed measured for carbon-14 according to claim 1, it is characterised in that：The source system processed
Also include being connected with the conversion device signal and control the conversion equipment the first state and second state it
Between the control device that switches over, the CO entered through the first passage detected when the detector2Amount with from described the
The CO of two passages outflow2When difference between amount is less than preset value, the conversion equipment is in the first state；Visited when described
Survey the CO entered through the first passage that device is detected2Amount and the CO flowed out from the second channel2Difference between amount reaches
During preset value, the conversion equipment is changed to second state.
3. a kind of source system processed measured for carbon-14 according to claim 1 or 2, it is characterised in that：The converting means
Plane four-way valve is set to, the absorption plant is provided with air inlet pipe and escape pipe, and wherein two mouths of pipe of the plane four-way valve are distinguished
Outlet side, the inlet end of the second channel with the first passage are connected, other two mouth of pipe point of the plane four-way valve
It is not connected with the air inlet pipe and escape pipe of the absorption plant.
4. a kind of source system processed measured for carbon-14 according to claim 1 or 2, it is characterised in that：The CO2Occur
Device, which includes reaction vessel, is connected with the reaction vessel and is used to the addition absorption into the reaction vessel, CO2NaOH
First reagent bottle of absorbing liquid and it is connected with the reaction vessel and is used into the reaction vessel add HCl solution
Second reagent bottle, is provided with the first peristaltic pump, second reagent bottle and institute between first reagent bottle and the reaction vessel
State and the second peristaltic pump is provided between reaction vessel, the source system processed is also included being connected with the reaction vessel to will reaction knot
3rd peristaltic pump of the waste liquid discharge after beam.
5. a kind of source system processed measured for carbon-14 according to claim 4, it is characterised in that：The source system processed
Also include the inert gas feeding mechanism being connected with the reaction vessel, the inert gas feeding mechanism and the reaction vessel
Between be provided with gas flowmeter.
6. a kind of source system processed measured for carbon-14 according to claim 4, it is characterised in that：The reaction vessel
In be additionally provided with pH sensors, the exterior bottom of the reaction vessel is provided with agitating device.
7. a kind of source system processed measured for carbon-14 according to claim 1, it is characterised in that：The absorption plant
Liquid flashing counting bottle top is located at by the sealed seal of liquid flashing counting bottle, institute including liquid flashing counting bottle, detachable cover
State in liquid flashing counting bottle and be provided with scintillation solution and CO2Absorbing liquid.
8. a kind of source system processed measured for carbon-14 according to claim 7, it is characterised in that：The absorption plant
Also include the semiconductor cooler and temperature sensor located at liquid flashing counting bottle outer wall.
9. a kind of source system processed measured for carbon-14 according to claim 7 or 8, it is characterised in that：It is described to absorb dress
Putting also includes the Motorized lift device located at liquid flashing counting bottle exterior bottom, and the Motorized lift device includes being used to support
It is provided with and the stepping in the lifting platform of liquid flashing counting bottle and the stepper motor to drive lifting of lifting table, the lifting platform
The connected position-sensing switch of motor.
10. a kind of source system processed measured for carbon-14 according to claim 7, it is characterised in that：The source system processed
Also include the feeding device to be fed into the absorption plant, the feeding device is included to contain scintillation solution
3rd reagent bottle, to contain CO24th reagent bottle of absorbing liquid and one end and the 3rd reagent bottle and the 4th examination
Agent bottle is respectively connected with the auto injection pump that the other end is connected with liquid flashing counting bottle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710468189.0A CN107132095B (en) | 2017-06-20 | 2017-06-20 | Source manufacturing system for carbon-14 measurement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710468189.0A CN107132095B (en) | 2017-06-20 | 2017-06-20 | Source manufacturing system for carbon-14 measurement |
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| Publication Number | Publication Date |
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| CN107132095A true CN107132095A (en) | 2017-09-05 |
| CN107132095B CN107132095B (en) | 2020-03-06 |
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ID=59736235
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710468189.0A Active CN107132095B (en) | 2017-06-20 | 2017-06-20 | Source manufacturing system for carbon-14 measurement |
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| Country | Link |
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| CN (1) | CN107132095B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115326500A (en) * | 2022-07-14 | 2022-11-11 | 中核核电运行管理有限公司 | Liquid carbon-14 conversion absorbing device of nuclear power plant |
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| Publication number | Publication date |
|---|---|
| CN107132095B (en) | 2020-03-06 |
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