CN107132095B - Source manufacturing system for carbon-14 measurement - Google Patents
Source manufacturing system for carbon-14 measurement Download PDFInfo
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- CN107132095B CN107132095B CN201710468189.0A CN201710468189A CN107132095B CN 107132095 B CN107132095 B CN 107132095B CN 201710468189 A CN201710468189 A CN 201710468189A CN 107132095 B CN107132095 B CN 107132095B
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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 the field of environmental detection, and particularly relates to a source preparation system for carbon-14 measurement, which comprises a source preparation system and a source preparation system, wherein the source preparation system is sequentially communicated in a closed manner and used for generating CO2Generating device for drying CO2Drying apparatus for measuring CO2Volume detector and method for absorbing CO2An absorption device forming a sample source, wherein the detector at least comprises a first channel connected with the air outlet end of the drying device and a second channel independent from the first channel, a switching device capable of switching between a first state and a second state is arranged between the detector and the absorption device, and when the switching device is in the first state, the absorption device absorbs CO2When the conversion device is in the second state, the absorption device stops absorbing CO2After the technical scheme is adopted, CO can be realized2The quantitative absorption, stable preparation of carbon-14 sample sources with different contents, automatic control and implementation in the whole process, elimination of the influence of human factors, high detection efficiency, convenient operation and high stability.
Description
Technical Field
The invention belongs to the field of environmental detection, and particularly relates to a source system for carbon-14 measurement, which is applied to the detection of carbon-14 in air, water and biological samples.
Background
14C is a natural radionuclide and one of the most predominant radionuclides discharged from nuclear facilities, has half-life of 5730 years, emits pure β rays and has maximum energy of 156 keV14The C energy is low, and the most suitable measuring method is the measurement by a liquid flash spectrometer. In view of this, it is conventional14The method C is to mix calcium carbonate precipitation with scintillation liquid to prepare a colloid sample source, and has the advantages of capability of quantitatively adding calcium carbonate powder, guarantee of consistency of a measurement system, simple operation, low detection efficiency and relatively short sample preservation time. In recent years, another source preparation method is proposed, in which CO is absorbed by organic base/inorganic base2The method has the advantages of high detection efficiency, long storage time, complex operation, and CO2The absorption is not stable, resulting in large fluctuations in detection limits and uncertainty.
Disclosure of Invention
The invention aims to make up for the defects of the existing measuring method, thereby providing a full-automatic source making system for carbon-14 measurement, which can realize CO through program control and implementation in the whole process2The quantitative absorption is convenient to operate and the stability is high.
In order to achieve the purpose, the invention adopts the technical scheme that: a system of sources for carbon-14 measurement comprises a source system and a source system, wherein the source system is sequentially communicated in a closed mode and used for generating CO2Generating device for drying CO2Drying apparatus for measuring CO2Volume detector and method for absorbing CO2An absorption device forming a sample source, the detector at least comprises a first channel connected with the air outlet end of the drying device and a second channel independent from the first channel, a switching device capable of switching between a first state and a second state is arranged between the detector and the absorption device, and when the switching device is in the first state and the second state, the switching device is connected with the drying deviceIn a first state, the air outlet end of the first channel, the absorption device and the air inlet end of the second channel are communicated in sequence; when the conversion device is in the second state, the conversion device directly communicates the air outlet end of the first channel with the air inlet end of the second channel.
Further, the source system further comprises a control device connected with the switching device in a signal mode and used for controlling the switching device to switch between the first state and the second state, and when the detector detects CO entering through the first channel2The amount of CO flowing out of the second channel2When the difference between the quantities is less than a preset value, the switching device is in the first state; when the detector detects the CO entering through the first channel2The amount of CO flowing out of the second channel2When the difference between the amounts reaches a preset value, the switching device switches to the second state.
Furthermore, the conversion device is a planar four-way valve, the absorption device is provided with an air inlet pipe and an air outlet pipe, two pipe orifices of the planar four-way valve are respectively connected with the air outlet end of the first channel and the air inlet end of the second channel, and the other two pipe orifices of the planar four-way valve are respectively connected with the air inlet pipe and the air outlet pipe of the absorption device.
Further, said CO2The generating device comprises a reaction vessel, and a device which is connected with the reaction vessel and is used for adding the CO absorbed into the reaction vessel2The system comprises a reaction container, a first reagent bottle of NaOH absorption liquid, a second reagent bottle which is connected with the reaction container and used for adding HCl solution into the reaction container, a first peristaltic pump is arranged between the first reagent bottle and the reaction container, a second peristaltic pump is arranged between the second reagent bottle and the reaction container, and the source preparation system further comprises a third peristaltic pump which is connected with the reaction container and used for discharging waste liquid after the reaction is finished.
Furthermore, the source manufacturing system also comprises an inert gas supply device connected with the reaction container, and a gas flow meter is arranged between the inert gas supply device and the reaction container.
Further, a pH sensor is further arranged in the reaction container, and a stirring device is installed at the bottom of the outer side of the reaction container.
Further, absorbing device includes liquid scintillation counting bottle, can dismantle the lid and locate liquid scintillation counting bottle top will the sealed sealing member of liquid scintillation counting bottle, be equipped with scintillation liquid and CO in the liquid scintillation counting bottle2Absorbing the liquid.
Furthermore, the absorption device also comprises a semiconductor refrigerator and a temperature sensor which are arranged on the outer wall of the liquid scintillation counting bottle.
Furthermore, the absorbing device is still including locating the electric lift device of liquid scintillation counting bottle outside bottom, electric lift device is including the step motor that is used for the elevating platform of bearing liquid scintillation counting bottle and is used for driving the elevating platform to go up and down, be equipped with in the elevating platform with the position switch that step motor links to each other.
Further, the source manufacturing system also comprises a feeding device used for feeding materials into the absorption device, and the feeding device comprises a third reagent bottle used for containing scintillation liquid and a CO bottle used for containing CO2The device comprises a fourth reagent bottle for absorbing liquid and an automatic sampling pump, wherein one end of the automatic sampling pump is connected with the third reagent bottle and the fourth reagent bottle respectively, and the other end of the automatic sampling pump is connected with the liquid flash counting bottle.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the invention will absorb CO2The rate of addition of the HCl solution is controlled by a pH sensor and an inert gas supply unit desorbs the CO2Carrying out the carrier tape and sequentially passing through a drying device and CO2First channel of detector, absorption device and CO2A second channel of the detector for measuring CO passing through the first channel and the second channel in real time2The amount of CO absorbed by the absorption device can be measured in real time2When the absorption amount of the absorption device reaches a set value, the control device switches the conversion device to connect the air outlet end of the first channel with the air inlet end of the second channel, the residual gas is directly discharged without passing through the absorption device,thereby realizing CO2The quantitative absorption of the carbon-14 can be realized, the carbon-14 sample sources with different contents can be stably prepared, and the detection efficiency is high. The invention has the advantages of automatic control and implementation in the whole process, prevention of influence of human factors, one-key operation, convenient operation and high stability.
Drawings
FIG. 1 is a schematic diagram of a source system for carbon-14 measurements according to the present invention.
Wherein, 1, a generating device; 101. a reaction vessel; 102. a first reagent bottle; 103. a second reagent bottle; 104. a stirring device; 105. a first peristaltic pump; 106. a second peristaltic pump; 107. a third peristaltic pump; 108. a pH sensor; 2. a drying device; 3. a detector; 301. a first channel; 302. a second channel; 4. an absorption device; 401. a liquid flash counting bottle; 402. a semiconductor refrigerator; 403. a temperature sensor; 404. an electric lifting device; 5. a planar four-way valve; 6. an inert gas supply device; 7. a gas flow meter; 8. a feeding device; 801. a third reagent bottle; 802. a fourth reagent bottle; 803. an automatic sample injection pump; 804. A planar three-way valve.
Detailed Description
The invention is further explained below with reference to the drawings and examples.
As shown in FIG. 1, a source system for carbon-14 measurement comprises a source system and a source system, which are sequentially communicated in a closed mode and are used for generating CO2Generating device 1 for drying CO2Drying apparatus 2 for measuring CO2Volume detector 3, and method for absorbing CO2An absorption device 4 forming a sample source, the detector 3 at least comprises a first channel 301 connected with the air outlet end of the drying device 2 and a second channel 302 independent from the first channel 301, and a switching device capable of switching between a first state and a second state is arranged between the detector 3 and the absorption device 4.
When the conversion device is in the first state, the gas outlet end of the first channel 301, the absorption device 4 and the gas inlet end of the second channel 302 are sequentially communicated, and at this time, the absorption device 4 absorbs CO2(ii) a When the switching device is in the second stateIn a state, the conversion device directly communicates the gas outlet end of the first channel 301 with the gas inlet end of the second channel 302, and CO is2No longer passes the absorption means 4.
The source system further comprises a control device (not shown) in signal connection with the switching device and controlling the switching device to switch between the first state and the second state. CO passing through the first channel 301 and the second channel 302 of the detector 32When the difference value of the quantities is less than the preset value, the conversion device is controlled by the control device to be in a first state, CO2This is passed through the first passage 301, the absorption means 4 and the second passage 302 in this order. Real-time determination of CO through a first channel 301 and a second channel 3022Amount of CO passing through the first channel 301 and the second channel 3022When the difference reaches a predetermined value, the switching device is controlled by the control device and switched to the second state, and the absorption device 4 stops absorbing CO2。
The conversion device in this embodiment is a planar four-way valve 5, the absorption device 4 is provided with an air inlet pipe and an air outlet pipe, two pipe orifices of the planar four-way valve 5 are respectively connected with the air outlet end of the first channel 301 and the air inlet end of the second channel 302, and the other two pipe orifices of the planar four-way valve 5 are respectively connected with the air inlet pipe and the air outlet pipe of the absorption device 4. The first channel 301 is used for measuring CO in the container2Total amount, second channel 302 for measuring unabsorbed CO2Amount of the compound (A).
The drying device 2 comprises a drying tube and allochroic silicagel arranged in the drying tube, wherein the allochroic silicagel is used for absorbing water vapor in passing gas.
CO2The generating device 1 comprises a reaction vessel 101, and is connected with the reaction vessel 101 and used for adding CO absorbed in the reaction vessel 1012A first reagent bottle 102 of the NaOH absorption solution, and a second reagent bottle 103 connected to the reaction vessel 101 and configured to add the HCl solution to the reaction vessel 101.
In order to accurately control the conveying rate and the conveying amount of the NaOH absorption liquid and the HCl solution, a first peristaltic pump 105 is arranged between the first reagent bottle 102 and the reaction container 101, and a second peristaltic pump 106 is arranged between the second reagent bottle 103 and the reaction container 101.
A pH sensor 108 is also disposed in the reaction vessel 101, and the pH value in the reaction vessel 101 measured by the pH sensor 108 in real time is used to control the rate and the total amount of HCl added to the reaction vessel 101 by the third peristaltic pump 107.
In addition, a third peristaltic pump 107 is provided in communication with the reaction vessel 101, the third peristaltic pump 107 being configured to discharge waste liquid from the reaction vessel 101 after the reaction is completed.
In order to mix the reactants uniformly and accelerate the reaction, a stirring device 104 is installed at the outer bottom of the reaction vessel 101. The stirring device 104 in this embodiment is a magnetic stirrer.
The source manufacturing system further comprises an inert gas supply device 6 connected with the reaction container 101, and a gas flow meter 7 is arranged between the inert gas supply device 6 and the reaction container 101. The inert gas used in this example was nitrogen.
Absorbing device includes liquid scintillation counting bottle, can dismantle the lid and locate liquid scintillation counting bottle top will the sealed sealing member of liquid scintillation counting bottle, be equipped with scintillation liquid and CO in the liquid scintillation counting bottle2Absorbing the liquid.
Absorbing device 4 includes liquid scintillation counter bottle 401 and can dismantle the lid and locate liquid scintillation counter bottle 401 top will the sealed sealing member of liquid scintillation counter bottle 401 is equipped with scintillation liquid and CO in the liquid scintillation counter bottle 4012Absorbing the liquid. CO in this example2The absorption liquid is Carbsorb absorption liquid.
The outer wall of liquid scintillation counter bottle 401 is provided with semiconductor refrigerator 402 and temperature sensor 403, and temperature sensor 403 is connected with semiconductor refrigerator 402 and controls the operation of semiconductor refrigerator 402 by measuring the temperature of the liquid in liquid scintillation counter bottle 401. In the embodiment, the temperature of the liquid in the liquid scintillation counting bottle 401 is controlled to be-10-0 ℃, so that volatilization of the scintillation liquid and Carbsob absorption liquid can be reduced, and CO is increased2The absorption efficiency.
Preferably, the lower end of the air inlet pipe of the absorption device 4 is arranged on the scintillation liquid and CO2Below the liquid level of the absorption liquid, will absorbThe lower end of the air outlet pipe of the device 4 is arranged on the scintillation liquid and the CO2The absorption liquid is above the liquid level, thereby further increasing CO2The absorption efficiency.
The bottom of the outer side of the liquid flash counting bottle 401 is also provided with an electric lifting device 404. The electric lifting device 404 comprises a lifting platform for supporting the liquid scintillation counting bottle 401 and a stepping motor for driving the lifting platform to lift, and a positioning switch connected with the stepping motor is arranged in the lifting platform, so that the liquid scintillation counting bottle 401 is ensured to reach a designated position and be connected with a sealing piece, and the bottle mouth of the liquid scintillation counting bottle 401 is sealed at the moment.
The source system further comprises a feeding device 8 for feeding the absorbing device 4. The feeding device 8 comprises a third reagent bottle 801 for containing scintillation liquid and CO2A fourth reagent bottle 802 for absorbing the liquid, and an automatic sample feeding pump 803, one end of which is connected with the third reagent bottle 801 and the fourth reagent bottle 802 respectively, and the other end of which is connected with the absorption device 4. In this embodiment, the third reagent bottle 801, the fourth reagent bottle 802, and the absorption device 4 are connected to the automatic sample pump 803 through a planar three-way valve 804.
The stirring device 104, the first peristaltic pump 105, the second peristaltic pump 106, the third peristaltic pump 107, the pH sensor 108, the detector 3, the semiconductor refrigerator 402, the temperature sensor 403, the electric lifting device 404, the planar four-way valve 5, the inert gas supply device 6, the automatic sample feeding pump 803 and the planar three-way valve 804 in the embodiment are all electrically connected with the control device, so that the whole process is controlled and implemented by a program, the influence of human factors is avoided, the operation is convenient, and the stability is high.
The following describes a detailed process for preparing a sample source for carbon-14 measurement using the source preparation system of this example. It should be noted that the following steps are only specific examples of the preparation of the sample source for carbon-14 measurement, and should not be taken as limiting the function, structure or performance of the source system for carbon-14 measurement according to the present invention.
Step 1: the NaOH absorption liquid obtained by sample preparation is added into the first reagent bottle 102, the HCl solution with the concentration of 2mol/L is added into the second reagent bottle 103, the scintillation liquid is added into the third reagent bottle 801, the Carbsorb absorption liquid is added into the fourth reagent bottle 802, and the liquid scintillation counter bottle 401 is placed on the electric lifting platform.
Step 2: starting a control program, lifting the liquid flash counting bottle 401 to be connected with a sealing piece through an electric lifting platform to seal the bottle mouth, opening an inert gas supply device 6, introducing nitrogen into the system through a gas flowmeter 7, controlling the gas flow to be 10mL/min, purging for more than 5 minutes, and removing air in the system.
And step 3: adding NaOH absorption liquid into a reaction container 101 through a first peristaltic pump 105, starting an electromagnetic stirrer, and controlling the rotating speed to be 600 r/min; start-up of CO2The detector 3 starts to walk a base line; controlling a semiconductor refrigerator 402 to reduce the temperature in the liquid flash counting bottle 401 to-10 ℃; the automatic sample feeding pump 803 is controlled to respectively draw 11.00mL of scintillation fluid from the third reagent bottle 801 and 9.00mL of Carbsorb absorption liquid from the fourth reagent bottle 802 into the scintillation counter bottle 401.
And 4, step 4: when the temperature sensor 403 shows-10 ℃, HCl solution is added to the reaction vessel 101 via the second peristaltic pump 106 until the pH sensor 108 reads 7.0.
And 5: CO while the second peristaltic pump 106 is activated2The detector 3 starts measuring and recording data, while the four-way planar valve 5 is in the first state, i.e. gas from CO2The first channel 301 of the detector 3 flows in, enters the liquid flash counting bottle 401 through the plane four-way valve 5, and then enters CO through the plane four-way valve 52The second channel 302 of the probe 3 flows out.
Step 6: to be treated with CO2The absorption amount reaches the target amount, the planar four-way valve 5 is switched to the second state, namely, the gas directly enters the CO without passing through the liquid flash counting bottle 4012The second channel 302 of the probe 3 flows out.
And 7: when the pH sensor 108 indicates that the pH value is positive, the third peristaltic pump 107 is closed, the two-channel CO is stopped after the pH value is kept for 10 minutes2And acquiring data by the detector 3.
And 8: and opening the second peristaltic pump 106, discharging the waste liquid, taking down the liquid scintillation counting bottle 401 through the electric lifting platform, and covering the bottle cap to be measured.
And step 9: semiconductor chiller 402 is turned off and the process ends. The inert gas supply 6 is turned off.
After the technical scheme is adopted, the invention desorbs CO through the inert gas supply device 62Carrying out the carrier tape and sequentially passing through a drying device 2 and CO2First channel 301 of detector 3, absorption device 4 and CO2The second channel 302 of the detector 3 measures in real time the CO passing through the first channel 301 and the second channel 3022The amount of CO absorbed by the absorption device 4 can be measured in real time2And when the absorption amount of the absorption device 4 reaches a set value, the control device switches the conversion device to the second state, so that the gas outlet end of the first channel 301 is connected with the gas inlet end of the second channel 302, and residual gas is directly discharged without passing through the absorption device 4, thereby realizing CO2The quantitative absorption of the carbon-14 can be realized, the carbon-14 sample sources with different contents can be stably prepared, and the detection efficiency is high. The invention has the advantages of automatic control and implementation in the whole process, prevention of influence of human factors, one-key operation, convenient operation and high stability.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (9)
1. A source system for carbon-14 measurements, characterized by: comprises a plurality of closed and communicated units which are used for generating CO2Generating device for drying CO2Drying apparatus for measuring CO2Volume detector and method for absorbing CO2The absorption device is used for forming a sample source, the detector is at least provided with a first channel connected with the air outlet end of the drying device and a second channel independent from the first channel, a switching device capable of switching between a first state and a second state is arranged between the detector and the absorption device, and when the switching device is in the first state, the air outlet end of the first channel, the absorption device and the air inlet end of the second channel are sequentially communicated; when in useWhen the conversion device is in a second state, the conversion device directly communicates the air outlet end of the first channel with the air inlet end of the second channel;
the source system also comprises a control device which is connected with the switching device by signals and controls the switching device to switch between the first state and the second state, when the detector detects the CO entering through the first channel2The amount of CO flowing out of the second channel2When the difference between the quantities is less than a preset value, the switching device is in the first state; when the detector detects the CO entering through the first channel2The amount of CO flowing out of the second channel2When the difference between the amounts reaches a preset value, the switching device switches to the second state.
2. The source system for carbon-14 measurements as recited in claim 1, wherein: the conversion device is a planar four-way valve, the absorption device is provided with an air inlet pipe and an air outlet pipe, two pipe orifices of the planar four-way valve are respectively connected with the air outlet end of the first channel and the air inlet end of the second channel, and the other two pipe orifices of the planar four-way valve are respectively connected with the air inlet pipe and the air outlet pipe of the absorption device.
3. The source system for carbon-14 measurements as recited in claim 1, wherein: the CO is2The generating device comprises a reaction vessel, and a device which is connected with the reaction vessel and is used for adding the CO absorbed into the reaction vessel2The system comprises a reaction container, a first reagent bottle of NaOH absorption liquid, a second reagent bottle which is connected with the reaction container and used for adding HCl solution into the reaction container, a first peristaltic pump is arranged between the first reagent bottle and the reaction container, a second peristaltic pump is arranged between the second reagent bottle and the reaction container, and the source preparation system further comprises a third peristaltic pump which is connected with the reaction container and used for discharging waste liquid after the reaction is finished.
4. The source system for carbon-14 measurements according to claim 3, wherein: the source manufacturing system also comprises an inert gas supply device connected with the reaction container, and a gas flowmeter is arranged between the inert gas supply device and the reaction container.
5. The source system for carbon-14 measurements according to claim 3, wherein: and a pH sensor is also arranged in the reaction container, and a stirring device is arranged at the bottom of the outer side of the reaction container.
6. The source system for carbon-14 measurements as recited in claim 1, wherein: absorbing device includes liquid scintillation counting bottle, can dismantle the lid and locate liquid scintillation counting bottle top will the sealed sealing member of liquid scintillation counting bottle, be equipped with scintillation liquid and CO in the liquid scintillation counting bottle2Absorbing the liquid.
7. The source system for carbon-14 measurements according to claim 6, wherein: the absorption device also comprises a semiconductor refrigerator and a temperature sensor which are arranged on the outer wall of the liquid flash counting bottle.
8. The system of claim 6 or 7, wherein: the absorption device is characterized by further comprising an electric lifting device arranged at the bottom of the outer side of the liquid flash counting bottle, the electric lifting device comprises a lifting platform used for bearing the liquid flash counting bottle and a stepping motor used for driving the lifting platform to lift, and a positioning switch connected with the stepping motor is arranged in the lifting platform.
9. The source system for carbon-14 measurements according to claim 6, wherein: the source system also comprises a feeding device used for feeding materials into the absorption device, wherein the feeding device comprises a third reagent bottle used for containing scintillation liquid and a third reagent bottle used for containing CO2A fourth reagent bottle for absorbing the liquid, and a reagent bottle having one end connected with the first reagent bottleThe three reagent bottles and the fourth reagent bottle are respectively connected with an automatic sample injection pump, and the other end of the automatic sample injection pump is connected with the liquid flash counting bottle.
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| 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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