CN113640862A - Continuous tritium sampling device in ambient air - Google Patents
Continuous tritium sampling device in ambient air Download PDFInfo
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- CN113640862A CN113640862A CN202110831745.2A CN202110831745A CN113640862A CN 113640862 A CN113640862 A CN 113640862A CN 202110831745 A CN202110831745 A CN 202110831745A CN 113640862 A CN113640862 A CN 113640862A
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- 238000005070 sampling Methods 0.000 title claims abstract description 83
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 title claims abstract description 37
- 229910052722 tritium Inorganic materials 0.000 title claims abstract description 37
- 239000012080 ambient air Substances 0.000 title claims abstract description 18
- 230000003197 catalytic effect Effects 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-PWCQTSIFSA-N Tritiated water Chemical compound [3H]O[3H] XLYOFNOQVPJJNP-PWCQTSIFSA-N 0.000 claims abstract description 16
- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 13
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 238000005057 refrigeration Methods 0.000 claims abstract description 5
- 239000000919 ceramic Substances 0.000 claims description 36
- 239000003570 air Substances 0.000 claims description 27
- 239000003054 catalyst Substances 0.000 claims description 20
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- 239000000428 dust Substances 0.000 claims description 9
- 238000005485 electric heating Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000004065 semiconductor Substances 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 230000000903 blocking effect Effects 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 239000004809 Teflon Substances 0.000 claims description 3
- 229920006362 Teflon® Polymers 0.000 claims description 3
- 239000000443 aerosol Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000011491 glass wool Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000005192 partition Methods 0.000 claims description 3
- 238000009833 condensation Methods 0.000 abstract description 7
- 230000005494 condensation Effects 0.000 abstract description 7
- 238000010257 thawing Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 72
- 238000000034 method Methods 0.000 description 10
- 239000000523 sample Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- XLYOFNOQVPJJNP-MNYXATJNSA-N hydrogen tritium oxide Chemical compound [3H]O XLYOFNOQVPJJNP-MNYXATJNSA-N 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- -1 aqua regia Chemical class 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T7/00—Details of radiation-measuring instruments
- G01T7/02—Collecting means for receiving or storing samples to be investigated and possibly directly transporting the samples to the measuring arrangement; particularly for investigating radioactive fluids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2205—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with filters
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T7/00—Details of radiation-measuring instruments
- G01T7/02—Collecting means for receiving or storing samples to be investigated and possibly directly transporting the samples to the measuring arrangement; particularly for investigating radioactive fluids
- G01T7/04—Collecting means for receiving or storing samples to be investigated and possibly directly transporting the samples to the measuring arrangement; particularly for investigating radioactive fluids by filtration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N2001/2282—Devices for withdrawing samples in the gaseous state with cooling means
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Biomedical Technology (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention belongs to the technical field of tritium sampling, and particularly relates to a continuous tritium sampling device in ambient air. The device comprises a first sampling pipeline and a second sampling pipeline which are connected in parallel, wherein the first sampling pipeline comprises a mass flow meter (2), a catalytic device (3) and a collector (4) provided with a collecting bottle (5) which are sequentially connected in series, the second sampling pipeline comprises the mass flow meter (2) and the collector (4) provided with the collecting bottle (5) which are sequentially connected in series, and gas enters from the upstream end of the first sampling pipeline and the upstream end of the second sampling pipeline, is collected in the collector (4) to complete the collection of tritiated water in the gas and is discharged from the downstream end; the catalytic device (3) is used for oxidizing tritium gas in the gas into tritiated water. The invention adopts a mode of connecting two stages of collectors in series, and the collecting efficiency can be improved to 99 percent; refrigeration and defrosting are switched to work, so that continuous and uninterrupted sampling of condensation is realized in the real sense.
Description
Technical Field
The invention belongs to the technical field of tritium sampling, and particularly relates to a continuous tritium sampling device in ambient air.
Background
Tritium in air around a nuclear facility comprises two forms, namely oxidation state tritium (HTO) and non-oxidation state tritium (HT), the past technology only focuses on HTO, and methods for removing HTO are mostly based on a bubbling method, but the bubbling method is low in efficiency and high in lower limit of detection, and common equipment comprises foreign MARC7000 and TASC, and also comprises devices designed by domestic radiation hospitals, nuclear energy hospitals and Shanghai physics application research institutes. At present, a condensation method is well used for collecting tritium in air, a semiconductor cold trap is adopted in the condensation method, water in the air is firstly condensed into frost which is accumulated on the wall of the cold trap, the frost is reheated and is collected into water, the volume of a semiconductor chamber is small, the semiconductor chamber is easy to block and cannot be used for continuous sampling, a plurality of devices and equipment are used for the method, the TS212 designed by Shanghai applied physics research institute and equipment designed by China radiation colleges are arranged at present, and the collection efficiency of the equipment can reach more than 95%.
Disclosure of Invention
Aiming at the problem that a tritium sampling device adopting a condensation method is easy to block a gas circuit, the invention aims to provide the tritium sampling device adopting the condensation method, which can realize continuous and uninterrupted sampling, has high collection efficiency, and can collect oxidation state tritium (HTO) and non-oxidation state tritium (HT) in air.
In order to achieve the purposes, the invention adopts the technical scheme that the device for continuously sampling tritium in ambient air comprises a first sampling pipeline and a second sampling pipeline which are connected in parallel, wherein the first sampling pipeline comprises a mass flow meter, a catalytic device and a collector provided with a collecting bottle which are sequentially connected in series; the catalytic device is used for oxidizing tritium gas in the gas into tritiated water.
Further, a high-efficiency filter is arranged on the pipeline at the upstream end of the first sampling pipeline and the second sampling pipeline and used for removing dust particles and aerosol in the gas.
Further, two collectors are respectively arranged on the first sampling pipeline and the second sampling pipeline in series, and each collector is connected with the collecting bottle.
Further, the collector internally comprises a first collecting cavity and a second collecting cavity which are connected in parallel, and the first collecting cavity and the second collecting cavity are consistent in structure; electromagnetic valves are arranged at the gas inlet ends of the first collecting cavity and the second collecting cavity and used for controlling the gas to enter the first collecting cavity or the second collecting cavity; the first collecting cavity and the second collecting cavity are respectively connected with the collecting bottle.
Further, in the present invention,
the collector condenses tritiated water vapor into tritiated water in a semiconductor refrigeration mode;
the first collecting cavity and the second collecting cavity are internally provided with clapboards to divide the first collecting cavity and the second collecting cavity into a first sub-collecting cavity and a second sub-collecting cavity, and the gas flows in from a gas inlet at the top of the first sub-collecting cavity, enters the bottom of the second sub-collecting cavity through the bottom of the first sub-collecting cavity and then flows out from a gas outlet at the top of the second sub-collecting cavity;
the upper cover and the lower cover of the collector are made of Teflon materials; the upper cover is positioned at the top of the first sub-collecting cavity and the second sub-collecting cavity; the lower cover is positioned at the bottom of the first sub-collecting cavity and the second sub-collecting cavity; the air inlet and the air outlet are arranged on the upper cover; a water outlet is arranged on the lower cover and used for discharging tritiated water into the collecting bottle;
the first collecting cavity and the second collecting cavity are made of aluminum alloy through oxidation, and the interiors of the cavities of the first sub-collecting cavity and the second sub-collecting cavity are provided with saw-toothed structures which are easy to be attached to the interiors of the cavities after the gas is condensed;
the upper cover adopts the horn mouth embedded easily gas flows in and with first collection chamber with the second collection chamber keeps the biggest contact surface, prevents that gas is in the air inlet frosts and forms the jam, easily gas with the cavity contact freezes into the frost.
Further, the external device of the catalytic device is an electric heating furnace, the inside of the container of the catalytic device is a spherical ceramic tube, the electric heating furnace wraps the ceramic tube, and the ceramic tube is 5cm in inner diameter and 20cm in height.
Further, in the present invention,
the ceramic tube is of a vertical structure, the gas enters from the bottom, a spiral stainless steel gas tube is coiled at the inner bottom of the ceramic tube, and upward gas holes are formed in the stainless steel gas tube every 1 cm;
catalyst is filled in 3 layers of the ceramic tube, and a reticular metal sheet is arranged between each layer of the ceramic tube for fixing the catalyst and improving the catalytic efficiency; the aperture of the reticular metal sheet is 2 mm;
high-temperature-resistant meshed metal sheets and glass wool are arranged at the air inlet and the air outlet inside the ceramic tube and are used for increasing the gas circulation inside the ceramic tube, filtering dust of a catalyst and preventing the dust from blocking a rear-end gas path and the collector; the aperture of the high-temperature resistant reticular metal sheet is 2 mm.
Further, the catalyst filled in the ceramic tube is a Pd alumina catalyst, and the heating temperature of the catalytic device is 100-180 ℃.
Further, a vacuum pump is provided on the lines at the downstream ends of the first and second sampling lines for flowing the gas from the upstream ends to the downstream ends of the first and second sampling lines.
The invention has the beneficial effects that:
1. the space of the first collecting cavity 8 and the second collecting cavity 9 of the collector 4 is large, the refrigerating temperature is reduced to-40 ℃, and the collecting efficiency can be improved to 99 percent by adopting a mode of connecting two stages of collectors in series.
2. The design mode of the internal bell mouth of the collector 4 can accelerate the gas flow, accelerate the adhesion cold junction of the sample on the inner surfaces of the first collecting cavity 8 and the second collecting cavity 9, and improve the collecting efficiency.
3. The collector 4 is internally provided with two chambers which are connected in parallel (a first collecting chamber 8 and a second collecting chamber 9), and the two chambers work independently, so that refrigeration and defrosting are switched to work, condensation continuous sampling in the true sense is realized, and the running time is more than 10 d. In operation, can obtain the water yield by environment humiture and sample volume, automatic control cavity sample time, when the cavity volume of collecting water reaches 70%, switch over into another cavity sample, avoid blockking up the gas circuit, and can reach continuous incessant sample.
4. The electric heating furnace is wrapped outside the catalytic device 3, the Pd alumina catalyst is filled in the spherical ceramic tube adopted by the inner container, the ceramic tube has the advantages of high strength, high temperature resistance and low possibility of being oxidized, and the spherical ceramic can reduce the internal resistance. The catalytic device 3 can reach over 98 percent of tritium gas (HT) catalytic efficiency at the set heating temperature of 200 ℃.
Drawings
FIG. 1 is a schematic structural diagram of a device for continuously sampling tritium in ambient air according to an embodiment of the present invention;
FIG. 2 is a schematic view of a collector 4 according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of the catalytic efficiency test principle described in the embodiments of the present invention;
FIG. 4 is a schematic diagram of a collector collection efficiency test according to an embodiment of the present invention;
fig. 5 is a schematic view of a first collecting chamber 8 and a second collecting chamber 9 according to an embodiment of the invention;
in the figure: 1-a high-efficiency filter, 2-a mass flow meter, 3-a catalytic device, 4-a collector, 5-a collecting bottle, 6-a vacuum pump, 7-an electromagnetic valve, 8-a first collecting cavity, 9-a second collecting cavity, 10-a gas bottle, 11-a gas collecting bag, 12-a temperature and humidity probe, 13-a partition plate, 14-a first sub-collecting cavity, 15-a second sub-collecting cavity, 16-an upper cover, 17-a lower cover, 18-a gas inlet, 19-a gas outlet, 20-a saw-toothed structure and 21-a water outlet.
Detailed Description
The invention is further described below with reference to the figures and examples.
The invention provides a continuous sampling device for tritium in ambient air, which comprises a vacuum pump 6, a high-efficiency filter 1, a mass flow meter 2, a catalytic device 3, a collector 4, a gas circuit, a control system and other components.
As shown in fig. 1, the continuous sampling device for tritium in ambient air provided by the invention comprises a first sampling pipeline and a second sampling pipeline which are connected in parallel, wherein a high-efficiency filter 1 is arranged on the pipeline at the upstream end of the first sampling pipeline and the pipeline at the upstream end of the second sampling pipeline, and is used for removing dust particles and aerosol in gas, and then the gas enters the first sampling pipeline and the second sampling pipeline respectively. The first sampling pipeline comprises a mass flow meter 2, a catalytic device 3 and a collector 4 provided with a collecting bottle 5 which are sequentially connected in series, the second sampling pipeline comprises a mass flow meter 2 and a collector 4 provided with a collecting bottle 5 which are sequentially connected in series, and after gas enters from the upstream ends of the first sampling pipeline and the second sampling pipeline, collection of tritiated water in the gas is completed in the collector 4, and then the tritiated water is discharged from the downstream end; the catalytic device 3 is used for oxidizing tritium gas in the gas into tritiated water.
Only tritiated water (HTO) in the gas entering the first sampling line is condensed in the inner chamber of the collector 4; the tritium gas (HT) is oxidized, and tritiated water (HTO) and the tritium gas (HT) are all condensed in an internal chamber of the collector 4 after entering the second sampling pipeline and passing through the catalytic device 3 and then passing through the two-stage collector 4. The frost formed by the collector 4 is changed into liquid through heating and flows into the collecting bottle 5, the liquid in the collecting bottle 5 in the first sampling pipeline is used as a tritiated water (HTO) sample in the gas, the liquid in the collecting bottle 5 in the second sampling pipeline is used as a tritiated water (HTO) sample and a tritium gas (HT) sample in the gas, and the concentration of the tritiated water (HTO) and the tritium gas (HT) in the gas can be obtained through liquid flash measurement and analysis.
Two collectors 4 are respectively arranged on the first sampling pipeline and the second sampling pipeline in series, the upstream collector is used as a first-stage collector, the downstream collector is used as a second-stage collector, and each collector 4 is connected with a collecting bottle 5.
As shown in fig. 2, the collector 4 internally comprises a first collecting cavity 8 and a second collecting cavity 9 which are connected in parallel, and the first collecting cavity 8 and the second collecting cavity 9 are consistent in structure; the electromagnetic valve 7 is arranged at the air inlet end of the first collecting cavity 8 and the second collecting cavity 9, and the electromagnetic valve 7 is used for controlling the air inlet time of the cavities according to different temperatures and humidity, so that air is controlled to enter the first collecting cavity 8 or the second collecting cavity 9, the two cavities are switched with each other, the frosting amount in the cavities is controlled, and the permeability is maximized while the collecting efficiency is ensured; the first collecting chamber 8 and the second collecting chamber 9 are connected to the collecting bottle 5, respectively.
The collector 4 condenses tritiated water vapor into tritiated water in a semiconductor refrigeration mode;
as shown in fig. 5, a partition 13 is arranged inside the first collecting cavity 8 and the second collecting cavity 9 to divide the first collecting cavity 8 and the second collecting cavity 9 into a first sub-collecting cavity 14 and a second sub-collecting cavity 15, and the gas flows in from a gas inlet 18 at the top of the first sub-collecting cavity 14, enters the bottom of the second sub-collecting cavity 15 through the bottom of the first sub-collecting cavity 14, and then flows out from a gas outlet 19 at the top of the second sub-collecting cavity 15;
the collector 4 is provided with an upper cover 16 and a lower cover 17, the upper cover 16 is positioned at the top of the first sub-collecting cavity 14 and the second sub-collecting cavity 15; the lower cover 17 is positioned at the bottom of the first sub-collecting cavity 14 and the second sub-collecting cavity 15; an air inlet 18 and an air outlet 19 are provided on the upper cover 16; a water outlet 21 is arranged on the lower cover 17 and used for discharging tritiated water into the collecting bottle 5;
the upper cover 16 and the lower cover 17 of the collector 4 are made of teflon materials, have excellent heat-resistant and low-temperature-resistant characteristics, can work at a freezing temperature without embrittlement and can not melt at a high temperature. The surface of the coating is not stained with water and oil, can bear the action of all strong acids including aqua regia, strong oxidant, reducing agent and various organic solvents except molten alkali metal, fluorinated medium and sodium hydroxide with the temperature higher than 300 ℃, and can protect parts from any kind of chemical corrosion;
the first collecting cavity 8 and the second collecting cavity 9 are made of aluminum alloy through oxidation, the inner parts of the cavities of the first sub collecting cavity 14 and the second sub collecting cavity 15 are provided with saw-toothed structures 20, and the saw-toothed structures 20 are easy to be attached to the inner parts of the cavities after gas condensation;
the upper cover 16 is in a horn mouth embedded type, so that air can easily flow into the upper cover and can be kept in the maximum contact surface with the first collecting cavity 8 and the second collecting cavity 9, air is prevented from frosting and blocking at the air inlet 18, and air can easily contact with the cavities and can be frozen into frost.
The external device of the catalytic device 3 is an electric heating furnace, the internal container of the catalytic device 3 is a spherical ceramic tube, the electric heating furnace wraps the ceramic tube, and the ceramic tube has an inner diameter of 5cm and a height of 20 cm. The ceramic tube is high temperature resistant and not easy to be oxidized, the defect that the traditional metal tube inner surface is oxidized and dropped to be mixed with the catalyst to influence the performance of the catalyst is avoided, and the metal tube can be prevented from being oxidized and dropped to be contacted with the heating wire to cause the internal short circuit of the catalytic device under the condition of long-term high temperature.
The ceramic tube is of a vertical structure, gas enters from the bottom, a spiral stainless steel gas tube is arranged on the inner bottom plate of the ceramic tube, and upward gas holes are formed in the stainless steel gas tube every 1cm, so that the gas entering the ceramic tube is uniformly distributed, the contact area of the gas entering the ceramic tube and a catalyst is increased, and the catalytic efficiency is improved;
catalyst is filled in the partial 3 layers of the ceramic tube, a reticular metal sheet is arranged between each layer for fixing the catalyst, and meanwhile, the gas uniformly passes through each layer of catalyst, which is beneficial to improving the catalytic efficiency; the aperture of the reticular metal sheet is 2 mm;
high-temperature-resistant netted metal sheets and glass wool are arranged at the air inlet and the air outlet inside the ceramic tube and are used for increasing the gas circulation inside the ceramic tube, filtering the dust of the catalyst and preventing the dust from blocking a rear-end gas path and a collector 4; the aperture of the high-temperature resistant reticular metal sheet is 2 mm.
The catalyst filled in the ceramic tube is Pd alumina catalyst, and the heating temperature of the catalytic device 3 is 100-180 ℃.
A vacuum pump 6 is provided on the lines at the downstream ends of the first and second sampling lines for flowing gas from the upstream ends to the downstream ends of the first and second sampling lines.
The control system is used for controlling various components of the device, such as controlling and regulating flow, regulating the temperature of the catalytic furnace, regulating the temperature of a collector and the like.
Finally, the method for testing the catalytic efficiency and the collection efficiency of the continuous tritium sampling device in the ambient air provided by the invention is explained
and 4, after 3.0h, collecting gas samples in the gas cylinder 10 and the first gas sampling bag 11(1000L) by using a second gas sampling bag 11(5L) and a third gas sampling bag 11(5L) respectively, and measuring the hydrogen concentrations Cin and Cout in the gas samples respectively by using a gas chromatograph.
(1) Drying the collecting bottle 5, and weighing the collecting bottle with the mass m 1;
(2) according to a schematic diagram (shown in figure 4) of a collector collection efficiency test principle, a temperature and humidity probe 12 is placed at an outlet of a sampling pipeline of a collector 4;
(3) setting the flow rates of the first sampling pipeline and the second sampling pipeline to be 3.0L/min, setting the temperature of the catalytic device 3 to be 200 ℃, setting the temperature of the collector 4 to be-30 ℃ and setting the sampling time to be 168 h;
(4) after sampling, the mass m2 of the collection bottle 5 is weighed again, and the mass m3 of water in the tail gas is calculated according to the data of the temperature and humidity recorder and the mass flow meter 2.
the device according to the present invention is not limited to the embodiments described in the specific embodiments, and those skilled in the art can derive other embodiments according to the technical solutions of the present invention, and also belong to the technical innovation scope of the present invention.
Claims (9)
1. The utility model provides a tritium continuous sampling device in ambient air which characterized by: the device comprises a first sampling pipeline and a second sampling pipeline which are connected in parallel, wherein the first sampling pipeline comprises a mass flow meter (2), a catalytic device (3) and a collector (4) provided with a collecting bottle (5) which are sequentially connected in series, the second sampling pipeline comprises a mass flow meter (2) and a collector (4) provided with a collecting bottle (5) which are sequentially connected in series, and gas enters from the upstream end of the first sampling pipeline and the upstream end of the second sampling pipeline and then is collected in the collector (4) to be discharged from the downstream end; the catalytic device (3) is used for oxidizing tritium gas in the gas into tritiated water.
2. A continuous sampling device of tritium in ambient air as claimed in claim 1, wherein: and a high-efficiency filter (1) is arranged on the pipeline at the upstream end of the first sampling pipeline and the second sampling pipeline and is used for removing dust particles and aerosol in the gas.
3. A continuous sampling device of tritium in ambient air as claimed in claim 1, wherein: two collectors (4) are respectively arranged on the first sampling pipeline and the second sampling pipeline in series, and each collector (4) is connected with the collecting bottle (5).
4. A continuous sampling device of tritium in ambient air as claimed in claim 1, wherein: the collector (4) internally comprises a first collecting cavity (8) and a second collecting cavity (9) which are connected in parallel, and the first collecting cavity (8) and the second collecting cavity (9) are consistent in structure; an electromagnetic valve (7) is arranged at the gas inlet end of the first collecting cavity (8) and the second collecting cavity (9), and the electromagnetic valve (7) is used for controlling the gas to enter the first collecting cavity (8) or the second collecting cavity (9); the first collecting cavity (8) and the second collecting cavity (9) are respectively connected with the collecting bottle (5).
5. A continuous sampling device of tritium in ambient air as claimed in claim 4, wherein:
the collector (4) condenses tritiated water vapor into tritiated water in a semiconductor refrigeration mode;
a partition plate (13) is arranged inside the first collecting cavity (8) and the second collecting cavity (9) to divide the first collecting cavity (8) and the second collecting cavity (9) into a first sub-collecting cavity (14) and a second sub-collecting cavity (15), and the gas flows in from a gas inlet (18) at the top of the first sub-collecting cavity (14), enters the bottom of the second sub-collecting cavity (15) through the bottom of the first sub-collecting cavity (14) and then flows out from a gas outlet (19) at the top of the second sub-collecting cavity (15);
the upper cover (16) and the lower cover (17) of the collector (4) are made of Teflon materials; the upper cover (16) is positioned at the top of the first sub-collecting cavity (14) and the second sub-collecting cavity (15); the lower cover (17) is positioned at the bottom of the first sub-collecting cavity (14) and the second sub-collecting cavity (15); the air inlet (18) and the air outlet (19) are arranged on the upper cover (16); a drain port (21) is arranged on the lower cover (17) and used for draining tritiated water into the collecting bottle (5);
the first collecting cavity (8) and the second collecting cavity (9) are made of aluminum alloy through oxidation, a sawtooth-shaped structure (20) is arranged inside the cavity of the first sub-collecting cavity (14) and the cavity of the second sub-collecting cavity (15), and the sawtooth-shaped structure (20) is easy to be attached to the inside of the cavity after the gas is condensed;
the upper cover (16) adopts the horn mouth to be embedded easily gas flows into and with first collection chamber (8) with second collection chamber (9) keep the biggest contact surface, prevent that gas is in air inlet (18) frosting forms the jam, easily gas with the cavity contact freezes into the frost.
6. A continuous sampling device of tritium in ambient air as claimed in claim 1, wherein: the external device of the catalytic device (3) is an electric heating furnace, the internal container of the catalytic device (3) is a spherical ceramic tube, the electric heating furnace wraps the ceramic tube, and the inner diameter of the ceramic tube is 5cm and the height of the ceramic tube is 20 cm.
7. A continuous sampling device of tritium in ambient air as claimed in claim 6, wherein:
the ceramic tube is of a vertical structure, the gas enters from the bottom, a spiral stainless steel gas tube is coiled at the inner bottom of the ceramic tube, and upward gas holes are formed in the stainless steel gas tube every 1 cm;
catalyst is filled in 3 layers of the ceramic tube, and a reticular metal sheet is arranged between each layer of the ceramic tube for fixing the catalyst and improving the catalytic efficiency; the aperture of the reticular metal sheet is 2 mm;
high-temperature-resistant meshed metal sheets and glass wool are arranged at the air inlet and the air outlet inside the ceramic tube and are used for increasing the gas circulation inside the ceramic tube, filtering dust of a catalyst and preventing the dust from blocking a rear-end gas path and the collector (4); the aperture of the high-temperature resistant reticular metal sheet is 2 mm.
8. A continuous sampling device of tritium in ambient air as claimed in claim 7, wherein: the catalyst filled in the ceramic tube is a Pd alumina catalyst, and the heating temperature of the catalytic device (3) is 100-180 ℃.
9. A continuous sampling device of tritium in ambient air as claimed in claim 1, wherein: a vacuum pump (6) is provided on the lines at the downstream ends of the first and second sampling lines for flowing the gas from the upstream ends to the downstream ends of the first and second sampling lines.
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