CN212749262U

CN212749262U - Tritium and carbon-14 oxidation extraction element in environmental sample

Info

Publication number: CN212749262U
Application number: CN202020370029.XU
Authority: CN
Inventors: 毕卫国
Original assignee: Shandong Radiometric Biotechnology Co ltd
Current assignee: Shandong Radiometric Biotechnology Co ltd
Priority date: 2020-03-20
Filing date: 2020-03-20
Publication date: 2021-03-19
Anticipated expiration: 2030-03-20

Abstract

The utility model discloses an oxidation extraction device of tritium and carbon-14 in an environmental sample, which relates to the detection equipment technology, and comprises a rack, a tubular electric furnace, an atmosphere system, a tritium-carbon collection part and a temperature control system for controlling the tubular electric furnace, wherein the rack is provided with a movable catalytic area, an oxidation area and a preheating area; quartz pipelines penetrate through the catalytic zone, the oxidation zone and the preheating zone, an air inlet assembly and an air outlet assembly are respectively arranged at two ends of each quartz pipeline, a sample boat can be placed in the middle of each quartz pipeline in a replaceable manner, and a copper wire mesh body for a catalyst is arranged at one end, located at the air outlet assembly, of each quartz pipeline; the atmosphere system comprises an oxygen inlet pipeline in the same direction as the air inlet of the air inlet assembly and a control part for accurately adjusting the air flow; the tritium-carbon collecting part is communicated with the gas outlet end of the gas outlet assembly. The utility model discloses be convenient for observe, favourable cooling can realize the programmed control of combustion process, convenient efficient man-machine operation, the assurance of extraction efficiency.

Description

Tritium and carbon-14 oxidation extraction element in environmental sample

Technical Field

The utility model belongs to the technical field of check out test set, concretely relates to tritium and carbon-14's oxidation extraction element in environmental sample.

Background

Tritium is radioactive and undergoes beta decay with a half-life of 12.43 years. Since tritium's beta decay emits electrons moving at high speed and does not penetrate human body, a large amount of absorbed tritium is harmful to human body. Through the isotope exchange effect, the method has the advantages that,³h and H₂H in O is exchanged to form tritiated water HTO. Most of them³H is present as HTO. The pulmonary hazard of HTO taken in by breathing in the lungs has been shown by studies to be 20000 times more toxic than HT.

Carbon-14 has a half-life of about 5,730 + -40 years, with the decay mode being beta decay, with the carbon 14 atom being converted to the nitrogen-14 atom. In which the body accumulates nuclear radiation pollution by respiration¹⁴C, the direct intake of the polluted food is more harmful because the biological half-drain period is nearly 40 d.

Tritium and carbon are main nuclides discharged from nuclear power effluents, and nuclear facilities discharge a certain amount of tritium to the environment under certain conditions, so that certain pollution is caused to the environment. Tritium in biological samples consists of two parts, free water tritium (TFWT) and organically bound water tritium (OBT).¹⁴C participates in various biological cycles and is easily deposited in the food chain. The monitoring of tritium and carbon-14 in organisms is required to be carried out on the peripheral radiation environment monitoring of newly-built nuclear power plants. Environmental requirements require analysis of tritium-and carbon-14-containing contaminants with specific activities ranging from environmental levels to ILW (medium radioactivity) levels. A common method is to convert an organically bound tritium, carbon-14 sample to H2O (by oxidative combustion)³H) And CO₂(¹⁴C) And then to H₂O(³H) And CO₂(¹⁴C) Collection and analysis were performed.

SUMMERY OF THE UTILITY MODEL

The utility model aims at providing a be convenient for observe and cool down as early as possible after the experiment is accomplished, can realize the programmed control of combustion process, convenient efficient man-machine operation, the device of the assurance of extraction efficiency, and tritium and carbon-14's oxidation extraction element in the environmental sample who provides.

In order to achieve the above purpose, the utility model adopts the following technical scheme:

designing an oxidation extraction device of tritium and carbon-14 in an environmental sample, which comprises a rack, a tubular electric furnace, an atmosphere system, a tritium-carbon collection part and a temperature control system for controlling the tubular electric furnace, wherein a movable catalytic zone, an oxidation zone and a preheating zone are arranged on the rack along the length direction of the rack, and the catalytic zone, the oxidation zone and the preheating zone are respectively arranged in different tubular electric furnaces;

quartz pipelines penetrate through the catalytic zone, the oxidation zone and the preheating zone, an air inlet assembly and an air outlet assembly are respectively arranged at two ends of each quartz pipeline, a sample boat can be placed in the middle of each quartz pipeline in a replaceable manner, and a copper wire mesh body for a catalyst is arranged at one end, located on the air outlet assembly, of each quartz pipeline;

the atmosphere system comprises an oxygen inlet pipeline in the same direction as the air inlet of the air inlet assembly and a control part for accurately adjusting the gas flow;

the tritium-carbon collecting part is communicated with the gas outlet end of the gas outlet assembly.

Furthermore, the tubular electric furnace of the catalytic zone is positioned at the tail end of the quartz pipeline, and the tubular electric furnaces of the oxidation zone and the preheating zone are of an integrated structure.

Furthermore, the temperature control system is a programmable temperature control system and a human-computer interaction system used for compiling and automatically storing temperature rise programs of different samples, the programmable temperature control system is arranged in the tubular electric furnace and is provided with a communication interface communicated with the outside, an over-temperature protection device is further arranged in the programmable temperature control system, and the maximum threshold value of the over-temperature protection device is 1200 ℃.

Furthermore, the air inlet assembly comprises two air inlet gas paths of oxygen and nitrogen.

Furthermore, a venturi tube is arranged at one end, located at the air inlet assembly, of the quartz pipeline.

Furthermore, the oxygen inlet pipeline is a catalytic area air inlet pipe arranged in the catalytic area, the catalytic area air inlet pipe penetrates and is fixed on the air outlet assembly, and the air outlet end of the catalytic area air inlet pipe extends to the air inlet upstream of the copper wire mesh body.

Further, the control part is an air inlet flow meter which is arranged on the air inlet pipe of the catalytic area and is arranged in the rack.

Furthermore, the quartz pipeline is made of high-purity quartz materials, and the quartz pipeline is a heating pipe with the diameter of 50-120 mm.

Go toStep, tritium carbon collecting part includes the cryotrap, the cryotrap adopts integration intelligence accurate accuse temperature cryotrap system, the inside of cryotrap is equipped with first HTO receiving flask and second HTO receiving flask, and the outside of cryotrap is equipped with first HTO receiving flask¹⁴CO₂Collecting bottle, second¹⁴CO₂A collector bottle, the first HTO collector bottle, the second HTO collector bottle, the first HTO collector bottle¹⁴CO₂Collecting bottle, second¹⁴CO₂The collecting bottle is connected in series through the product air inlet pipe and connected to the air outlet end of the air outlet assembly, and the second¹⁴CO₂The collecting bottle is provided with a tail gas discharge end.

The utility model provides an oxidation extraction element of tritium and carbon-14 in environmental sample, beneficial effect lies in: the utility model discloses open-type structural design is adopted in the experiment, is convenient for observe, is convenient for place experimental sample boat, catalyst, simultaneously, is convenient for observe and cool down as early as possible after the experiment is accomplished, can realize the programmed control of combustion process, convenient efficient man-machine operation, the assurance of extraction efficiency.

Drawings

The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention, and together with the description serve to explain the invention and not to limit the invention. In the drawings:

fig. 1 is a schematic structural diagram of the present invention;

figure 2 is a schematic diagram of the structure of the tritiated carbon collection portion of the present invention.

Labeled as: 1. catalytic zone, 2, oxidation zone, 3, preheating zone, 4, quartz pipeline, 5, venturi tube, 6, copper wire mesh body, 7, sample boat, 8, air inlet assembly, 9, air outlet assembly, 10, catalytic zone air inlet pipe, 11, slide rail, 12, rack, 13, programmable temperature control system, 14, air inlet flowmeter, 15, first HTO collecting bottle, 16, second HTO collecting bottle, 17, first HTO collecting bottle¹⁴CO₂Collecting bottle, 18, second¹⁴CO₂The device comprises a collecting bottle 19, a low-temperature cold trap 20, a cold trap controller 21, a product air inlet pipe 22, a tail gas discharge end 23 and a supporting frame.

Detailed Description

The present invention will be further described with reference to the following specific examples. These examples are provided only for illustrating the present invention and are not intended to limit the scope of the present invention. In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted", "provided" and "connected" are to be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.

The structural features of the present invention will now be described in detail with reference to the accompanying drawings.

Referring to fig. 1-2, an oxidation extraction device for tritium and carbon-14 in an environmental sample comprises a rack 12, a tubular electric furnace, an atmosphere system, a tritium-carbon collection part and a temperature control system for controlling the tubular electric furnace, wherein a movable catalytic area 1, an oxidation area 2 and a preheating area 3 are arranged on the rack 12 along the length direction of the rack, the catalytic area 1, the oxidation area 2 and the preheating area 3 are respectively arranged in different tubular electric furnaces, a sliding rail 11 for moving the tubular electric furnace is arranged on the rack 12, the tubular electric furnace can slide along the sliding rail 11, rollers moving along the sliding rail 11 are arranged at the bottom of the tubular electric furnace, and the catalytic area 1, the oxidation area 2 and the preheating area 3 can all move on the sliding rail, so that observation and cooling as soon as possible are convenient after experiments are completed.

The catalytic zone 1, the oxidation zone 2 and the preheating zone 3 are provided with quartz pipelines 4 in a penetrating manner, two ends of each quartz pipeline 4 are provided with support frames 23, the tubular electric furnace of the catalytic zone 1 is positioned at the tail end of each quartz pipeline 4, the tubular electric furnaces of the oxidation zone 2 and the preheating zone 3 are of an integrated structure, each quartz pipeline 4 is made of high-purity quartz materials, the quartz pipelines 4 are heating pipes with diameters of 50-120 mm, and specifically, the quartz pipelines 4 can be heating pipes with diameters of 65 mm. The large pipe diameter can contain more samples, and improves the extraction amount and sample preparation effect of tritium and carbon-14.

And two ends of the quartz pipeline 4 are respectively provided with an air inlet assembly 8 and an air outlet assembly 9, and the air inlet assembly 8 comprises two air inlet paths of oxygen and nitrogen.

The sample boat 7 is placed in the middle of the quartz pipeline 4 in a replaceable mode, a copper wire mesh body 6 used for a catalyst is arranged at one end, located at the air outlet assembly 9, of the quartz pipeline 4, and a Venturi tube 5 is arranged at one end, located at the air inlet assembly 8, of the quartz pipeline 4. The venturi tube 5 is used for uniformly mixing oxygen and nitrogen, preventing gas from forming turbulence, and preventing backflow of generated products to ensure the oxidation effect.

The atmosphere system includes the control part with the same direction of 8 air admission oxygen inlet pipe and the accurate regulation of gas flow of air intake assembly, the oxygen inlet pipe is the catalytic zone intake pipe 10 that sets up in catalytic zone 1, catalytic zone intake pipe 10 runs through to be fixed on the assembly 9 of giving vent to anger, and the end of giving vent to anger of catalytic zone intake pipe 10 extends to the air intake upper reaches of copper wire netting body 6, and the tip is the crotch form towards catalytic zone 1, catalytic zone 1 is furnished with independent and the equidirectional oxygen suppliment design of admitting air, can strengthen catalytic effect like this, prevent again to blow to cause the gas refluence to the air intake after the gas that the exhaust is not smooth and the oxidation. The control part is an air intake flow meter 14, and the air intake flow meter 14 is installed on the catalytic zone air intake pipe 10 and is arranged in the stand 12.

The temperature control system is programmable temperature control system 13 for compile and the human-computer interaction system of automatic storage different sample intensification procedures, programmable temperature control system 13 sets up in tubular electric furnace, and dispose the communication interface with outside UNICOM, still be equipped with excess temperature protection device in the programmable temperature control system 13, the highest threshold value of excess temperature protection device is 1200 degrees centigrade, oxidation zone 2, the independent accuse temperature of catalysis zone 1, a sample experiment can set up the multistage heating procedure, this device can set up 30 sections, the parameter of setting can be stored, make things convenient for next experiment to call. The work of the three temperature zones can realize linkage. For different samples, such as plant samples, animal tissue samples and soil samples, the procedure of heating has great difference, and this device can be to the many sets of procedures of different samples, automatic storage after the edition, and the convenience is directly called next time. The device is provided with a communication interface to realize communication with the outside.

The tritium-carbon collecting part is communicated with the gas outlet end of the gas outlet assembly 9 and comprises a low-temperature cold trap 19, the low-temperature cold trap 19 adopts an integrated intelligent accurate temperature control cold trap system, a first HTO collecting bottle 15 and a second HTO collecting bottle 16 are arranged inside the low-temperature cold trap 19, and a first HTO collecting bottle 15 is arranged outside the low-temperature cold trap 19¹⁴CO₂Collecting bottle 17, second¹⁴CO₂ A collector bottle 18, a first HTO collector bottle 15, a second HTO collector bottle 16, a first HTO collector bottle¹⁴CO₂Collecting bottle 17, second¹⁴CO₂The collecting bottle 18 is connected in series and connected to the air outlet end of the air outlet assembly 9 through a product air inlet pipe 21, and the second¹⁴CO₂The collection bottle 18 is provided with an off-gas discharge end 22. An advanced integrated intelligent accurate temperature control cold trap system is adopted, the low temperature is stable for a long time, and the recovery effect of HTO is ensured.

The utility model discloses an oxidation extraction element of tritium and carbon-14 in the environmental sample, the utility model discloses the experiment adopts open-type structural design, and the observation of being convenient for is convenient for place experimental sample boat, catalyst, simultaneously, is convenient for observe and cool down as early as possible after the experiment is accomplished, can realize the programmed control of combustion process, convenient efficient man-machine operation, the assurance of extraction efficiency.

Specifically, the method of use is as follows:

1. the catalyst of the copper wire mesh body 6 is loaded into a quartz pipeline 4 of a catalytic zone 1 of a main engine of an organic tritium carbon oxide oxidation furnace shown in figure 1. The first HTO collection vial 15 and the second HTO collection vial 16 were weighed and placed in a cryotrap 19 according to fig. 2, and the trap controller 20 was adjusted to-15 ℃ for cooling. 250ml of 4mol/L sodium hydroxide solution is measured and respectively placed in the first place in figure 2¹⁴CO₂Collecting bottle 17 and second¹⁴CO₂Within the collection bottle 18. The gas collection portion of the organic tritium carbon extraction unit is connected as per FIG. 2.

2. Weighing about 50-100 g of biological sample in a sample boat 7, pushing the sample boat 7 into a combustion area of an oxidation area 2 in the figure 1, connecting a gas inlet and outlet end device of the instrument, connecting a gas inlet assembly 8 in the figure 1 with an oxygen cylinder and a nitrogen cylinder, connecting a gas outlet assembly 9 with a product gas inlet pipe 21 in the figure 2, and connecting a catalytic area gas inlet pipe 10 in the figure 1 with another oxygen cylinder.

3. Nitrogen gas was first introduced through the gas inlet assembly 8 of FIG. 1 at a flow rate of 150mL/min to drive off the air in the apparatus. After the flow rate stabilized, the oxygen flow rate through the oxidation zone 2 of the intake assembly 8 was adjusted to 50mL/min and the first bubble figure 2 was observed¹⁴CO₂Collecting bottle 17, second¹⁴CO₂The collection bottle 18 is normal and then the oxidation zone oxygen flow is adjusted to 100 mL/min. The gas flow rates listed in this example are approximate amounts, and may be adjusted to ensure the recovery rate and the oxidation effect according to the amount of the sample, the properties of the sample, and the like.

4. Open the main machine part power switch of the organic tritium carbon extraction device of the utility model, set the temperature of the catalytic zone 1 of figure 1 to 700 ℃. After the oxidation zone 2 and the preheating zone 3 in fig. 1 are added, the sample is oxidized in the quartz tube 4 in fig. 1 according to a temperature-raising program preset or set by the programmable control system 13 in fig. 1, and the incompletely oxidized intermediate product is sufficiently oxidized into carbon dioxide and water under the drive of the carrier gas by the catalyst of the copper wire mesh body 6 in the catalytic zone 1 in fig. 1. After the sample is completely oxidized, the power supply is cut off, the catalytic zone 1, the oxidation zone 2 and the preheating zone 3 of fig. 1 are stopped from heating, and the air intake of the air intake assembly 8 and the catalytic zone air intake pipe 10 of fig. 1 is stopped.

5. Closing the cold trap controller 20 of FIG. 2, collecting tritium-containing water vapor during combustion in the first HTO collection bottle 15 and the second HTO collection bottle 16 through the cold trap 19 of FIG. 2 for supply³H for analytical determination; carbon dioxide is passed through the first of FIG. 2 containing sodium hydroxide solution¹⁴CO₂Collecting bottle 17 and second¹⁴CO₂The collection bottle 18 is absorbed for analysis¹⁴And C, using.

Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. An oxidation extraction device for tritium and carbon-14 in an environmental sample comprises a rack (12), a tubular electric furnace, an atmosphere system, a tritium-carbon collection part and a temperature control system for controlling the tubular electric furnace, and is characterized in that a movable catalytic zone (1), an oxidation zone (2) and a preheating zone (3) are arranged on the rack (12) along the length direction of the rack, the catalytic zone (1), the oxidation zone (2) and the preheating zone (3) are respectively arranged in different tubular electric furnaces, and a slide rail (11) for moving the tubular electric furnace is arranged on the rack (12);

a quartz pipeline (4) penetrates through the catalytic zone (1), the oxidation zone (2) and the preheating zone (3), an air inlet assembly (8) and an air outlet assembly (9) are respectively arranged at two ends of the quartz pipeline (4), a sample boat (7) can be placed in the middle of the quartz pipeline (4) in a replaceable manner, and a copper wire mesh body (6) for a catalyst is arranged at one end, located on the air outlet assembly (9), of the quartz pipeline (4);

the atmosphere system comprises an oxygen inlet pipeline which has the same direction with the air inlet of the air inlet assembly (8) and a control part for accurately adjusting the gas flow;

the tritium-carbon collecting part is communicated with the gas outlet end of the gas outlet assembly (9).

2. The device for the oxidative extraction of tritium and carbon-14 in an environmental sample according to claim 1, characterized in that the tubular electric furnace of the catalytic zone (1) is located at the end of the quartz pipe (4), and the tubular electric furnaces of the oxidation zone (2) and the preheating zone (3) are of an integrated structure.

3. The device for extracting tritium and carbon-14 from an environmental sample according to claim 1, wherein the temperature control system is a programmable temperature control system (13) and a man-machine interaction system for programming and automatically storing temperature programs for different samples, the programmable temperature control system (13) is arranged in the tubular electric furnace and is provided with a communication interface communicated with the outside, an over-temperature protection device is further arranged in the programmable temperature control system (13), and the maximum threshold of the over-temperature protection device is 1200 ℃.

4. An apparatus for the oxidative extraction of tritium and carbon-14 from environmental samples, according to claim 1, characterized in that the gas inlet assembly (8) comprises two gas inlet paths for oxygen and nitrogen.

5. An apparatus for the oxidative extraction of tritium and carbon-14 from environmental samples, according to claim 1, characterized in that the quartz pipe (4) is provided with a venturi (5) at one end of the gas inlet assembly (8).

6. The device for extracting tritium and carbon-14 from an environmental sample by oxidation as claimed in claim 1, wherein the oxygen inlet pipeline is a catalytic region air inlet pipe (10) arranged in the catalytic region (1), the catalytic region air inlet pipe (10) is fixed on the air outlet assembly (9) in a penetrating manner, and the air outlet end of the catalytic region air inlet pipe (10) extends to the air inlet upstream of the copper wire mesh body (6).

7. An oxidation extraction device of tritium and carbon-14 in environmental sample according to claim 6, characterized in that the control part is a gas inlet flow meter (14), the gas inlet flow meter (14) is installed on the catalytic zone gas inlet pipe (10) and is arranged in the rack (12).

8. The device for the oxidative extraction of tritium and carbon-14 from an environmental sample according to claim 1, wherein the quartz pipe (4) is made of high-purity quartz, and the quartz pipe (4) is a heating pipe with a diameter of 50-120 mm.

9. The device for the oxidative extraction of tritium and carbon-14 in an environmental sample according to claim 1, wherein the tritium-carbon collection part comprises a low-temperature trap (19), the low-temperature trap (19) adopts an integrated intelligent precise temperature control cold trap system, a first HTO collection bottle (15) and a second HTO collection bottle (16) are arranged inside the low-temperature trap (19), and a first HTO collection bottle (15) is arranged outside the low-temperature trap (19)¹⁴CO₂A collecting bottle (17) and a second¹⁴CO₂A collection bottle (18), the first HTO collection bottle (15), the second HTO collection bottle (16), the first HTO collection bottle¹⁴CO₂A collecting bottle (17) and a second¹⁴CO₂The collecting bottle (18) is connected in series and connected to the air outlet end of the air outlet assembly (9) through a product air inlet pipe (21), and the second¹⁴CO₂The collecting bottle (18) is provided with a tail gas discharge end (22).