CN116465682A - Method and device for extracting and collecting free water tritium from biological sample tissue - Google Patents
Method and device for extracting and collecting free water tritium from biological sample tissue Download PDFInfo
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- CN116465682A CN116465682A CN202310171437.0A CN202310171437A CN116465682A CN 116465682 A CN116465682 A CN 116465682A CN 202310171437 A CN202310171437 A CN 202310171437A CN 116465682 A CN116465682 A CN 116465682A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 146
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 title claims abstract description 103
- 229910052722 tritium Inorganic materials 0.000 title claims abstract description 103
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- 238000001291 vacuum drying Methods 0.000 claims abstract description 54
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- 238000007710 freezing Methods 0.000 claims description 5
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Classifications
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
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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
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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
- G01N1/40—Concentrating samples
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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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
- G01N2001/1418—Depression, aspiration
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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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
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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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4033—Concentrating samples by thermal techniques; Phase changes sample concentrated on a cold spot, e.g. condensation or distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a method and a device for extracting and collecting free water tritium from biological sample tissues, wherein heating and suction are simultaneously applied to the biological samples through a vacuum drying oven to obtain TFWT steam, the TFWT steam is converted into liquid tritium water for collection after being cooled at a low temperature, the sample quantity required by TFWT detection and analysis can be obtained rapidly and efficiently, the operation is simple and convenient, no chemical reagent is introduced into the biological samples in the whole extraction process, on one hand, the physical health and safety of test personnel are protected, and on the other hand, the test cost is saved; the corresponding device is sequentially connected with the vacuum drying box, the low-temperature cooling assembly, the suction filtration connector and the vacuum pump, TFWT steam extracted from the biological sample by the vacuum drying box is condensed into liquid tritium water by the low-temperature cooling assembly to flow out of the suction filtration connector, and then the liquid tritium water is collected by the tritium water collecting box connected to the bottom end of the suction filtration connector, so that the device is convenient, safe and efficient to use.
Description
Technical Field
The invention belongs to the technical field of radiation environment monitoring and investigation, and particularly relates to a method and a device for extracting and collecting free water tritium from biological sample tissues.
Background
Tritium is a natural radionuclide widely existing in the environment, and is also an important artificial radionuclide in the field of nuclear industry, and the tritium participates in the global hydrogen circulation and all biological metabolic processes and irradiates organisms with radiation. Tritium in the environment exists primarily in the form of gaseous tritium, tritium water, or organic tritium in the atmosphere, in water bodies, and in organisms, wherein the organisms exist primarily in the form of organized free water tritium (TFWT) and Organically Bound Tritium (OBT). The detection analysis of The Free Water Tritium (TFWT) and the organically combined tritium (OBT) of the tissue in the organism is definitely regulated in relevant specifications such as radiation environment monitoring technical Specification (HJ 61-2021), radiation environment background investigation technical Specification before the operation of the nuclear power plant (HJ 969-2018) and the like in the process of radiation environment quality monitoring, radiation background investigation monitoring before the operation of the nuclear power plant, radiation environment monitoring during the operation of the nuclear power plant and the like. The detection and analysis method is implemented by referring to the analysis method of tritium in water (HJ 1126-2020), and the standard only provides for detection and analysis of the tritium content in a water sample containing tritium or in a liquid effluent, but the method of extracting and collecting Tissue Free Water Tritium (TFWT) in a living body and converting the tissue free water tritium into tritium water which can be detected by the analysis method of tritium in water (HJ 1126-2020) is not clearly defined.
At present, TFWT in organisms is usually separated by freeze dehydration, vacuum freeze drying, azeotropic distillation and other methods at home and abroad, wherein the former two methods can obtain higher recovery rate (more than 90 percent) of TFWT by continuous operation of a professional freeze dryer for 2-3 days, and biological samples are required to be frozen and decomposed before the operation of the instrument so as to meet the requirements of sample split charging and freeze drying. The azeotropic distillation method is to break up biological sample, then put the broken biological sample into organic solvent, carry out TFWT in organism by heating and distilling organic solvent, and realize TFWT separation by fractional distillation. Organic solvents with a low azeotropic point and a high water content of the azeotropic point, such as benzene, toluene, xylene, cyclohexane, etc., are generally selected by azeotropic distillation, and the method can complete the extraction and separation of the biological TFWT in several hours, but has a low recovery rate (generally less than 70%). Because the organic solvent is volatile and has chemical toxicity, the organic solvent inevitably has certain harm to the health of the testers. In addition, the method can generate a certain amount of organic waste liquid, and the separated tritium water can contain a small amount of organic solution so as to influence the analysis and measurement results of the sample.
Therefore, there is a need to develop a method and a corresponding device for extracting and collecting free water tritium from biological sample tissues, which are rapid, efficient, convenient and safe.
Disclosure of Invention
The invention aims to provide a method and a device for extracting and collecting free water tritium from biological sample tissues, which are rapid, efficient, convenient and safe.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a method for extracting and collecting free water tritium from biological sample tissues, which comprises the following steps:
s10, placing a biological sample in a vacuum drying oven, and generating TWFT vapor through heating and suction of the vacuum drying oven;
s20, the TWFT vapor is converted into liquid tritium water through low-temperature cooling;
s30, collecting the liquid tritium water.
Further, in the step S10, the biological sample is a washed fresh sample, and the biological sample is not subjected to one or more of pretreatment of being divided and crushed into fine pieces or particles, being frozen at a low temperature, and being freeze-dried in vacuum.
Further, in step S20, the TWFT water vapor is condensed by a condenser tube, and is converted into liquid tritium water, and the condenser tube is a serpentine condenser tube, a straight condenser tube or a spherical condenser tube.
Further, the following steps are included between the step S20 and the step S30:
s21, filtering the liquid tritium water obtained by condensation in the step S20.
The invention also discloses a device for extracting and collecting the free water tritium from the biological sample tissue, which can realize the method, and comprises a vacuum drying box, a low-temperature cooling assembly, a suction filter connector and a vacuum pump which are sequentially connected, wherein the suction filter connector is hollow to form a cavity, the suction filter connector is provided with a water inlet, a water outlet and an air outlet, the water inlet, the water outlet and the air outlet are all communicated with the cavity, the water inlet is connected with the low-temperature cooling assembly, the water outlet is connected with a tritium water collector, and the air outlet is connected with the vacuum pump.
Further, the vacuum drying box is provided with a vacuum valve and a release valve; the cryogenically cooled assembly includes a condenser tube having an inlet and an outlet, the inlet being connected to the vacuum valve.
Further, the suction filter connector is a water vapor filter, and a filter element is also accommodated in the cavity.
Further, the vacuum pump further comprises a dryer, one end of the dryer is connected with the exhaust port, and the other end of the dryer is connected with the vacuum pump.
Further, the cryocooling assembly further comprises a cryocooling liquid circulating pump, the cryocooling liquid circulating pump is provided with a cooling liquid inlet and a cooling liquid outlet, the condensing tube comprises an inner tube and an outer tube, the inner tube is sleeved in the outer tube, the outer tube is provided with a liquid inlet and a liquid outlet, the liquid inlet is communicated with the cooling liquid outlet, and the liquid outlet is communicated with the cooling liquid inlet.
Further, the condenser tube is a serpentine condenser tube, the serpentine condenser tube is obliquely arranged, and the use temperature of the low-temperature cooling liquid circulating pump is set to be 2-6 ℃.
Compared with the prior art, the invention has the beneficial effects that at least the following steps are included:
1. according to the method for extracting and collecting the free tritium from the biological sample, disclosed by the invention, heating and suction are simultaneously applied to the biological sample through the vacuum drying box, so that TFWT steam is obtained, the TFWT steam is converted into liquid tritium water for collection after being cooled at a low temperature, the sample quantity required by TFWT detection and analysis can be obtained quickly and efficiently, the operation is simple and convenient, no chemical reagent is introduced into the biological sample in the whole extraction process, on one hand, the health and safety of test personnel are protected, and on the other hand, the test cost is saved;
2. according to the biological sample tissue free water tritium extraction and collection device, the vacuum drying box, the low-temperature cooling component, the suction filter connector and the vacuum pump are sequentially connected, the environment of constant temperature heating and negative pressure provided by the vacuum drying box is utilized to directly heat and suck the biological sample, evaporation of TFWF in the biological sample is accelerated, TFWT steam is condensed into liquid tritium water through the low-temperature cooling component, and the liquid tritium water flows out of the suction filter connector and is collected by the tritium water collection box connected to the bottom end of the suction filter connector, so that tissue free water tritium in the biological sample is extracted rapidly and efficiently, and the use is more convenient and safer;
3. in the biological sample tissue free water tritium extraction and collection device provided by the invention, the vacuum drying box has high inclusion degree on biological samples, the cleaned biological samples are only required to be laid in the tray and put in the sample chamber of the vacuum drying box, the biological samples are not required to be divided and crushed into fine particles or grains, the vacuum drying box with proper volume can be selected according to the actual sample condition, or the vacuum drying box with larger volume is selected, so that the extraction requirements of TFWT (thin film wt) in different biological samples can be met at one time, namely, enough biological TFWT water tritium can be extracted for subsequent test analysis only by carrying out one time of test, the use is convenient and efficient, the sample processing time is saved, and the practicability is good;
4. according to the invention, the cooling assembly comprises the condensing pipe and the low-temperature cooling liquid circulating pump, the cooling liquid is circularly conveyed into the outer pipe of the condensing pipe through the low-temperature cooling liquid circulating pump to condense tritium-containing steam in the inner pipe, the low-temperature cooling liquid circulating pump is convenient for controlling the actual cooling temperature, and the TFWT steam can be effectively condensed without being frozen into ice to influence the flow property of a pipeline, so that the use safety of the device is further improved;
5. in the invention, the suction filter connector can be preferably a water vapor filter, namely, a filter element is also accommodated in the inner cavity of the suction filter connector, the water vapor filter not only can filter tritium water flowing out of the condenser pipe, but also has the functions of liquefying vapor and fog, and discharges filtered air, so that the collection efficiency of the TFWT can be further improved, a dryer can be connected to the side wall interface of the filter connector, the replacement frequency of a drying agent in the dryer is reduced, and the vacuum pump is protected from being corroded by water vapor;
6. in the device for extracting and collecting the free water tritium of the biological sample tissue, the side wall interface of the suction filter connector can be further connected with a dryer, so that the air exhausted by the suction filter connector is further dried, and the corrosion to a vacuum pump is reduced.
Drawings
Fig. 1: the invention provides a technical roadmap of a method for extracting and collecting free water tritium from biological sample tissues;
fig. 2: the embodiment of the invention provides a schematic diagram of a free water tritium extraction and collection device for biological sample tissues. In fig. 2: 10. a vacuum drying box 101, a vacuum valve 102 and a gas release valve;
201. a condensing pipe 2011, an inner pipe 202 and a low-temperature cooling liquid circulating pump;
30. a suction filter connector 301, a water inlet 302, a water outlet 303 and an exhaust port;
40. a tritium water collector;
50. a vacuum pump;
60. a connecting pipe;
70. dryer, 701, drier.
Detailed Description
In the prior art, the technical problems that the pretreatment of the biological sample is complex, the device is not convenient, safe and efficient enough for extracting and collecting free water tritium of the biological sample tissue, and further improvement is needed exist.
The invention is therefore to be considered in all respects as illustrative and not restrictive, and the invention will be described in detail with reference to the accompanying drawings and examples.
The invention provides a method for extracting and collecting free water tritium from biological sample tissues, which is shown by referring to FIG. 1 and comprises the following steps:
s10, placing a biological sample in a vacuum drying oven, and generating TWFT vapor through heating and suction of the vacuum drying oven;
specifically, in step S10, the biological sample may be a washed fresh sample, and there is no need to perform one or more pretreatment of dividing and crushing into fine pieces or particles, low-temperature freezing, vacuum freeze drying, etc.; the invention mainly adopts the vacuum drying box to heat and suck the biological sample for the first time, does not need to freeze the biological sample at low temperature or freeze-dry in vacuum in advance, and can not be greatly limited by the memory of the container like an analysis tube or a glass bottle adopted in the prior art, and the invention can completely meet the requirements of rapid and efficient extraction and collection of free water tritium of biological sample tissue by directly processing the fresh sample of the biological sample through the cooperation of subsequent steps.
In step S10, for a biological sample with a large volume, such as a biological sample with a long branch or leaf, the biological sample may be first roughly divided into sections, for example, when the lettuce sample TWFT is extracted, the washed lettuce leaves may be roughly divided into sections of 3-10 cm, so as to be placed in the sample chamber in the vacuum drying box.
In step S10, the heating temperature of the vacuum drying oven for the biological sample is 100-120 ℃, preferably 105 ℃, and the error range is +/-1 ℃. The pumping temperature is higher than 120 deg.c, which may pump out some organic substances, affecting the accuracy of the TFWT.
S20, the TWFT vapor is converted into liquid tritium water through low-temperature cooling;
specifically, in step S20, the TWFT vapor may be cooled at a low temperature by a cold trap (for example, the technical solution disclosed in CN 210442151U) in the prior art, but liquid nitrogen is used as the cold trap, which not only has higher use cost, but also has a risk that the vapor freezes into an ice column to block the air duct, thereby causing the air duct or the connecting device to be flushed out under high pressure. Therefore, the invention selects the condensing tube for condensation, the condensing tube is a serpentine condensing tube or a straight condensing tube or a spherical condensing tube, and is matched with the low-temperature cooling liquid circulating pump, the circulating pump is convenient for controlling the actual cooling temperature, and the circulation of the pipeline is not affected by freezing into ice while the effective condensation of TFWT steam is ensured. During operation, the temperature of the low-temperature cooling liquid circulating pump can be set to be 2-6 ℃, for example, 2 ℃,4 ℃ and 6 ℃, so that TFWT steam can be effectively condensed without being frozen into ice to influence the flow property of a pipeline.
S30, collecting the liquid tritium water.
Specifically, before the liquid tritium water obtained by condensation in the step S20 is collected, the liquid tritium water can be further filtered, so that the collection efficiency of water vapor is further improved.
The invention also provides a device for extracting and collecting the free water tritium from the biological sample tissue, which can correspondingly realize the method for extracting and collecting the free water tritium from the biological sample tissue, and referring to fig. 2, the extracting and collecting device comprises a vacuum drying box 10, a low-temperature cooling assembly, a suction filter connector 30 and a vacuum pump 50 which are sequentially connected, wherein the suction filter connector 30 is hollow to form a cavity, the suction filter connector 30 is provided with a water inlet 301, a water outlet 302 and an air outlet 303, the water inlet 301, the water outlet 302 and the air outlet 303 are all communicated with the cavity, the water inlet 301 is connected with the low-temperature cooling assembly, the water outlet 302 is connected with a tritium water collector 40, and the air outlet 303 is connected with the vacuum pump 50.
In a specific embodiment, the vacuum drying oven 10 is provided with a vacuum valve 101 and a bleeder valve 102, the cryogenically cooled assembly comprises a condenser tube 201, the condenser tube 201 has an inlet and an outlet, and the inlet is connected with the vacuum valve 101; the suction filter connector 30 comprises a connector body, the hollow arrangement of the connector body forms the cavity (not labeled in the figure), the top end, the bottom end and the side wall of the connector body are all provided with interfaces, the interface at the top end is a water inlet 301, the interface at the bottom end is a water outlet 302, the interface at the side wall is an air outlet 303, the water inlet 301 is connected with the outlet of the condenser tube 201 and is used for receiving tritium water condensed out of the condenser tube 201, and the tritium water flows into the cavity through the water inlet 301 and flows out of the water outlet 302. The tritium water collector 40 is connected with the water outlet 302 of the suction filter connector 30 and is used for collecting tritium water obtained after condensation, and the collector can be a common container and is made of glass or quartz; the vacuum pump 50 is connected to the interface (i.e., the exhaust port 303) of the side wall of the connector body, so that the vacuum pump 50 is sequentially connected to the suction filter connector 30, the condenser pipe 201, and the vacuum drying oven 10, so as to perform vacuum treatment on the vacuum drying oven 10, the condenser pipe 201, and the suction filter connector 30.
Referring to fig. 1, the technical principle adopted by the invention is that TFWT steam is obtained by simultaneously acting on a biological sample in a heating and sucking mode to accelerate the evaporation of TFWT in the biological sample, and the TFWT steam is converted into liquid tritium water for collection after being cooled at a low temperature. Aiming at the quality and density differences of different biological samples, the invention adopts the design concept of a vacuum drying box to increase the sample capacity, and simultaneously provides a working environment with constant temperature heating and negative pressure for the biological samples through the vacuum drying box so as to improve the TFWT evaporation rate in the biological samples, promote the rapid drying of the biological samples, and simultaneously avoid the external gas from entering the drying box to further influence the composition and content of tritium water.
In the present invention, the vacuum drying oven 10 can be a commercially available product, which is a traditional and mature drying device, and is often applied to the industries of pharmacy, chemical industry, food, etc., and has not been found in the related report of applying the vacuum drying oven to the extraction and collection field of tissue free water tritium in biological samples. The commercially available vacuum drying oven 10 is generally provided with a box body, a plurality of sample chambers for placing samples are arranged in the box body, the sample chambers can be separated by a plurality of partition boards, the box body is also provided with a vacuum valve 101 and a deflation valve 102, the vacuum valve 101 and the deflation valve 102 are communicated with the sample chambers, so that the vacuum treatment can be performed on the sample chambers through the vacuum valve 101, the vacuum treatment is performed on the sample chambers after the vacuum treatment through the deflation valve 102 and the external ventilation, and the vacuum meter is further arranged on the surface of the box body, so that the vacuum degree in the sample chambers can be reacted in real time. As an example, the vacuum drying oven 10 of the present invention may be a constant temperature electric heating vacuum drying oven, such as an intelligent temperature control vacuum drying oven (DZF series) manufactured by Shanghai-constant scientific instrument, and more specifically, the specific parameters of the vacuum drying oven may be: the working environment temperature of the vacuum drying box is 5-40 ℃, the temperature control range in the sample chamber is between Room Temperature (RT) +10-200 ℃, the temperature fluctuation degree is 1 ℃, and the maximum vacuum degree in the sample chamber can reach 133pa.
The water content of the biological samples of different types is generally about 60-90%, and the amount of tritium water required in the radiation detection process is about 50g, and the inventor finds that the biomass required for TFWT extraction and collection is better between 250g and 350g in the actual test process. Wherein, the higher the water content of the biological sample, the less biomass is required, and vice versa. Based on the differences in the amount of biological sample and the density of biological species, in a preferred embodiment, the vacuum oven 10 employs a liner size (mm) of: 320 The method has the advantages that (length) multiplied by 320 (width) multiplied by 300 (height) can meet the requirement of accommodating a sufficient amount of biological samples (different biological types meet the capacity requirement) at one time, heating and sucking TFWT in the body of the biological samples, multiple test extractions are not needed, and the test period duration is reduced. When the device provided by the invention is used for extracting and collecting free water tritium from biological sample tissues, the cleaned biological samples are only required to be laid on the tray and then placed in the sample chamber of the drying box, so that the human resources and the treatment time are further saved.
Referring to fig. 2, in the present invention, the cryocooling assembly further includes a cryocooling fluid circulation pump 202, the cryocooling fluid circulation pump 202 is provided with a cooling fluid inlet and a cooling fluid outlet, the condensation tube 201 includes an inner tube 2011 and an outer tube (not labeled in the drawing), the inner tube 2011 is sleeved in the outer tube, the outer tube is provided with a fluid inlet and a fluid outlet (the condensation tube generally follows the principle of fluid inlet at the lower port and fluid outlet at the upper port), the fluid inlet is communicated with the cooling fluid outlet, and the fluid outlet is communicated with the cooling fluid inlet. The condenser 201 may be a serpentine condenser or a straight condenser or a bulb condenser, which are commonly used in the market.
In the invention, the main function of the low-temperature cooling component is to cool TFWT steam pumped out by a vacuum drying oven into liquid tritium water. In a specific embodiment, the volume of the cooling fluid in the low-temperature cooling fluid circulation pump 202 may be 4L, the temperature range is-10-normal temperature, and the flow rate is 15L/min. The low-temperature antifreezing cooling liquid can be a cooling liquid consisting of 30% of ethanol and 70% of deionized water by volume, and the condensation point of the cooling liquid is about-10 ℃, so that the functional effect of cooling liquid circulation cooling can be satisfied. The extraction and collection device in the prior art adopts liquid nitrogen as a cold trap, so that the use cost is high, and the risk that the air duct is blocked by the water vapor freezing ice column to cause the air duct or the connecting device to be flushed by high pressure exists. The invention adopts the low-temperature cooling liquid circulating pump as a cooling device, is convenient for controlling the actual cooling temperature, and can ensure that TFWT steam is effectively condensed and can not be frozen into ice to influence the flow property of a pipeline. In operation, the temperature of the cryocoolant circulation pump 202 may be set at 2-6deg.C, e.g., 2deg.C, 4deg.C, 6deg.C, to ensure that TFWT vapor effectively condenses while not freezing to ice to affect the flow through the tubing. As an example, the cryo-coolant circulation pump 202 may be a model LC-LTC-5/10 cryo-coolant circulation pump manufactured by the company of instrument technology, inc.
In a preferred embodiment, the effect of condensing TFWT vapor into tritium water is further ensured by selecting a serpentine condenser tube and extending the length of the serpentine condenser tube and its layout in combination with the use of the cryogenic coolant circulation pump 202. A serpentine condenser pipe with the effective length of 600mm, the caliber of 24mm and the outer diameter of 40mm is selected, and the residence time of condensed tritium water in the condenser pipe is prolonged by obliquely arranging the condenser pipe 201, so that the circulation resistance of TFWT steam is increased, and the condensing effect of the TFWT steam is further improved. The angle of the condenser tube 201 to the horizontal may be about 45.
In the present invention, the suction filter connector 30 may be a tee joint made of glass material, and may be further modified into a water vapor filter, where the inner cavity accommodates a filter element. The tritium water of the TFWT after cooling, which is led out after condensation by the (inner tube 2011 of the) condensation tube, also contains a small amount of water vapor and air components, and the tail end of the condensation tube is connected with a water vapor filter, so that the collection efficiency of the TFWT can be further improved. The water vapor filter not only can filter tritium water flowing out of the condenser pipe 201, but also has the functions of liquefying vapor and fog, and discharges filtered air. The moisture filter may be disposed in an inclined or upright arrangement so that the filtered tritium water may flow under gravity from the drain opening 302 to the tritium water collector 40.
In a preferred embodiment, the selected vapor filter is of a vertical inlet and horizontal outlet design with a drain port (i.e., drain port 302) at the bottom. The water vapor filter is vertically arranged, filtered and collected TFWT tritium water can directly flow from the water outlet 302 to the tritium water collector 40, and filtered air is pumped out through the air outlet 303. The vent 303 may be further designed to be positioned near the top end. As an example, the Filter connector may be a CEMS-Filter with a model GL-2T manufactured by su zhou Jing-huan Filter technology, and has a length of about 20cm and a diameter of about 6cm, the Filter connector housing is made of thickened high-quality transparent glass material, the highest withstand temperature reaches 180 ℃, the corrosion resistance is strong, the pore diameter of the matched Filter core can reach 0.1 μm, the Filter precision is high, the water vapor and mist in the gas can be effectively separated, and the Filter effect of the TFWT is ensured.
In the invention, the vacuum pump 50 is sequentially connected with the suction filter connector 30, the condenser pipe 201 and the vacuum drying oven 10 through the connecting pipeline 60 (such as a connecting hose), so that a negative pressure environment can be provided for the interior of the pipeline, the circulation of TFWT steam, air, moisture and the like is promoted, and the collection rate of the TFWT is accelerated. In one embodiment, the vacuum pump 50 may be a rotary vane vacuum pump, and specific parameters of the vacuum filtration pump may be: the dimensions (length. Times. Width. Times. Height) were 300X 120X 235mm, the pumping rate was 120L/min, the limiting pressure was about 950kpa, the vacuum in the tube was reduced to 50mbar, and the operation was continued for 24 hours.
Based on the above structure and design, the present invention may further include a dryer 70. One end of the dryer 70 is connected to the exhaust port 303 of the connector body, and the other end is connected to the vacuum pump 50. Referring to fig. 2, the dryer 70 may be a straight tube with two ends communicating with each other, and a desiccant 701 is accommodated in the tube. The dryer 70 is preferably arranged upright, and the air discharged from the suction filter connector 30 (the air outlet 303) is fed from the bottom of the straight pipe and discharged from the top. The main function of the dryer 70 is to further dry the air exiting the suction connector 30 to reduce the corrosion of the vacuum pump 50 by the moisture in the air. In one embodiment, the drying tube 50 is formed of a straight tube having a length of about 20cm and a diameter of about 5cm and having two ends communicating with each other, the tube wall is formed of transparent glass, and SiO is contained in the tube 2 And (5) drying agent. In use, the color change (SiO) of the desiccant in the tube can be observed 2 The desiccant is normally blue in color and turns pink after being wet) to replace the desiccant. The wet and color-changed drying agent can be reused after being dried, and is convenient and practical.
The working flow of the extraction and collection device provided by the invention can comprise the following steps:
(1) Pre-cooling of the cryogenically cooled assembly: the circulation of the cooling liquid and the refrigerating button of the low-temperature cooling liquid circulation pump 202 are opened, and pre-refrigerating is carried out for 20 minutes, so that the temperature of the cooling liquid is reduced to about 4 ℃ (the acceptable error range is +/-2 ℃);
(2) Heating the biological sample: cleaning biological samples, spreading the biological samples in a tray, placing the biological samples in a sample chamber of a vacuum drying oven 10, closing a chamber door and a release valve 102 of the vacuum drying oven 10, opening a vacuum valve 101 and a heating switch, and setting the temperature of the sample chamber of the vacuum drying oven to be 105 ℃; vacuumizing the vacuum drying oven 10 through the vacuum pump 50, closing the vacuum valve 101 of the vacuum drying oven 10 when the vacuum degree in the vacuum drying oven 10 is 85kpa, and then closing the switch of the vacuum pump 50; the biological sample begins to be heated in the vacuum drying oven 10, releasing TFWT water vapor;
(3) Suction filtration TFWT vapor
Due to the evaporation of TFWT steam in the biological sample in the vacuum drying oven 10, the vacuum degree in the vacuum drying oven 10 is continuously reduced, when the vacuum degree in the vacuum drying oven 10 is reduced to 50kpa, the vacuum pump 50 and the vacuum valve 101 of the vacuum drying oven 10 are sequentially opened, the TFWT steam starts to be extracted, the steam is pumped into the condenser pipe 201 through the connecting pipe to be condensed into liquid tritium water, then flows in through the water inlet 301 of the suction filter connector 30, flows out into the tritium water collector 40 through the water outlet 302 and is collected into the tritium water to be detected and analyzed later;
(4) Closing device
After a sufficient amount of tritium water is collected, a heating switch of the vacuum drying oven 10 is turned off, the vacuum pump 50 is utilized to continuously vacuumize for about 1 hour, then the vacuum valve 101 of the vacuum drying oven 10 is turned off, the air release valve 102 is turned on, then the low-temperature cooling liquid circulating pump 202 and the vacuum pump 50 are sequentially turned off, finally the tritium water collector is taken out, and the tritium water is poured out.
The biological sample tissue free water tritium extraction and collection device provided by the invention (according to the layout shown in fig. 2, a serpentine condenser tube is adopted to be obliquely arranged, a water vapor filter and a dryer are added and are vertically arranged) is used for carrying out TFWT collection and extraction tests on different types of organisms according to the method, and test results show that various organisms are laid in a sample chamber of a vacuum drying box in a tray after pretreatment, heating and pumping are carried out for 2 hours in the device, and after heating is stopped, pumping is continued for 1 hour, sufficient tritium water can be collected (specific test data are shown in Table 1), so that the requirement of subsequent detection and analysis on the sample amount is met, and the device is proved to have the extraction efficiency of the biological TFWT which is obviously higher than the modes of freeze dehydration, vacuum freeze drying, azeotropic distillation and the like which are widely popular at present, and the condensation and collection efficiency of the TFWT is superior to or is in the same level with other treatment modes.
TABLE 1 TFWT extraction and collection test results provided by the present invention
The biological tissue free tritium (TFWT) extraction and collection device provided by the invention is safe, convenient and efficient, and the use and popularization of the device can effectively improve the detection/monitoring working efficiency of the biological tissue free tritium in radiation environment monitoring.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the above embodiments specifically illustrate the present invention, it should be understood by those skilled in the art that modifications and equivalents may be made to the specific embodiments of the present invention without departing from the spirit and scope of the present invention, and any modifications and equivalents are intended to be covered by the scope of the claims of the present invention.
Claims (10)
1. A method for extracting and collecting free water tritium from biological sample tissue is characterized by comprising the following steps: the method comprises the following steps:
s10, placing a biological sample in a vacuum drying oven, and generating TWFT vapor through heating and suction of the vacuum drying oven;
s20, the TWFT vapor is converted into liquid tritium water through low-temperature cooling;
s30, collecting the liquid tritium water.
2. The method for extracting and collecting free water tritium from biological sample tissue according to claim 1, wherein the method comprises the following steps:
in step S10, the biological sample is a washed fresh sample, and is not subjected to one or more of pretreatment of crushing into fine particles or flakes, low-temperature freezing, and vacuum freeze drying.
3. The method for extracting and collecting free water tritium from biological sample tissue according to claim 1, wherein the method comprises the following steps: in step S20, the TWFT water vapor is condensed by a condenser tube, and is converted into liquid tritium water, where the condenser tube is a serpentine condenser tube, a straight condenser tube, or a spherical condenser tube.
4. The method for extracting and collecting free water tritium from biological sample tissue according to claim 1, wherein the method comprises the following steps: the steps between the step S20 and the step S30 further include the following steps:
s21, filtering the liquid tritium water obtained by condensation in the step S20.
5. A biological sample tissue free water tritium draws collection device which characterized in that: including vacuum drying cabinet, cryocooling subassembly, suction connector and the vacuum pump of connecting in order, the suction connector cavity sets up and forms a cavity, water inlet, outlet and gas vent have been seted up to the suction connector, water inlet, outlet and gas vent all with the cavity intercommunication, the water inlet with cryocooling subassembly is connected, a tritium water collector is connected to the outlet, the gas vent with the vacuum pump is connected.
6. The biological sample tissue free water tritium extraction and collection device of claim 5, wherein: the vacuum drying box is provided with a vacuum valve and a gas release valve; the cryogenically cooled assembly includes a condenser tube having an inlet and an outlet, the inlet being connected to the vacuum valve.
7. The biological sample tissue free water tritium extraction and collection device of claim 5, wherein: the suction filter connector is a water vapor filter, and a filter element is also accommodated in the cavity.
8. The biological sample tissue free water tritium extraction and collection device of claim 5 or 7, wherein: the vacuum pump is characterized by further comprising a dryer, wherein one end of the dryer is connected with the exhaust port, and the other end of the dryer is connected with the vacuum pump.
9. The biological sample tissue free water tritium extraction and collection device of claim 6, wherein: the low-temperature cooling assembly further comprises a low-temperature cooling liquid circulating pump, the low-temperature cooling liquid circulating pump is provided with a cooling liquid inlet and a cooling liquid outlet, the condensing tube comprises an inner tube and an outer tube, the inner tube is sleeved in the outer tube, the outer tube is provided with a liquid inlet and a liquid outlet, the liquid inlet is communicated with the cooling liquid outlet, and the liquid outlet is communicated with the cooling liquid inlet.
10. The biological sample tissue free water tritium extraction and collection device of claim 9, wherein: the condenser pipe is a serpentine condenser pipe, the serpentine condenser pipe is obliquely arranged, and the use temperature of the low-temperature cooling liquid circulating pump is set to be 2-6 ℃.
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