CN203479599U - Sample preparation device for organic tritium measurement - Google Patents
Sample preparation device for organic tritium measurement Download PDFInfo
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- CN203479599U CN203479599U CN201320541185.8U CN201320541185U CN203479599U CN 203479599 U CN203479599 U CN 203479599U CN 201320541185 U CN201320541185 U CN 201320541185U CN 203479599 U CN203479599 U CN 203479599U
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Abstract
The utility model discloses a sample preparation device for organic tritium measurement. The device comprises a sample combustion area, a catalysis area and a collection area, wherein the collection area is a cold trap collection device; the sample combustion area is provided with an oxygen and nitrogen inlet; a catalyst is arranged in the catalysis area. The device is characterized in that the sample combustion area and the catalysis area mainly comprise a horizontally arranged double-temperature area tubular combustion furnace, wherein a second oxygen inlet is formed in one side of the catalysis area; the cold trap collection device is communicated with one end, away from the sample combustion area, in the catalysis area. According to the device, the combustion speed can be effectively controlled, the problems of deflagration and incomplete combustion are solved, and the measurement stability and reliability are improved; the oxygen concentration of the catalysis area can be controlled, so that the catalysis efficiency is improved.
Description
Technical field
The utility model relates to a kind of environment monitoring device, is specifically related to a kind of sample preparation device for the content of the organic tritium of environmental organism is measured.
Background technology
Tritium is the radioactive isotope of water, because the β decay of tritium only can be emitted an electronics for high-speed mobile, can not penetrate human body skin, therefore, only has a large amount of suction tritiums just can be harmful.But, tritium in HTO can be incorporated in animals and plants organic molecule and removes to form combination tritium (organically bound tritium, OBT), and the intestines and stomach of human body, respiratory tract and skin and mucosa can absorb HTO, drink after HTO, through 40～45 minutes, will absorb completely.The combination tritium entering in human body can cause direct internal radiation, thus the health of serious harm human body, research shows, the toxicity of HTO is 520 times of nucleic tritium.
Be engaged in the research of tritium and the unit of production and can in environment, discharge a small amount of tritium, to environment.For the degree that analysis environments biological sample is polluted by tritium, conventional method is at present, adopts oxidizing fire method that organic tritium is changed into tritiated water, collects, by the liquid scintillation counter measurement content of tritium wherein through cold-trap.For example, in " development of full tritium burning sample preparation device " literary composition of < < China's nuclear science echnology report > > 01 phase in 2008, a kind of full tritium burning sample preparation device is disclosed, by heating chamber, catalyst chamber, condenser pipe, cold-trap gathering-device forms, wherein, heating chamber is positioned at the below of catalyst chamber, there is oxygen and nitrogen inlet, sample burns in heating chamber, not clean-burning part is through catalyst chamber catalytic oxidation, form HTO, by cold-trap collect HTO for liquid scintillation counter detect.
This device can be realized the sample preparation of organic tritium and measure, but, in this apparatus structure, due to by realize the abundant burning of sample in heating chamber by oxygen and nitrogen, thereby enter in the gas of catalyst chamber, nitrogen content is higher, the carrying out that is unfavorable for catalytic oxidation, meanwhile, heating chamber is positioned at catalyst chamber below, catalyst chamber temperature is affected by heating chamber, is difficult to control.And in environmental and biological materials, the content of tritium is conventionally lower, therefore, the resolution of measurement is very large on the impact of measurement result.
Therefore, there is the measurement mechanism that must develop the organic tritium that improves structure, so that the measurement to environmental sample.
Summary of the invention
Goal of the invention of the present utility model is to provide the sample preparation device that a kind of organic tritium is measured, to realize the content of organic tritium in measurement environment biological sample in high sensitivity.
To achieve the above object of the invention, the technical solution adopted in the utility model is: the sample preparation device that a kind of organic tritium is measured, comprise sample combustion district, catalytic domain and collecting region, described collecting region is cold-trap gathering-device, in described catalytic domain, be provided with catalyzer, described sample combustion district is provided with oxygen and nitrogen inlet, described sample combustion district and catalytic domain mainly consist of two warm area tubular type combustion furnaces of a horizontal positioned, in described catalytic domain one side, be provided with the second oxygen intake, described cold-trap gathering-device is communicated with one end away from sample combustion district in catalytic domain.
In technique scheme, by being horizontally disposed with combustion furnace, sample combustion district and catalytic domain temperature can be controlled respectively, thereby suitable catalytic reaction temperature can be set as required, meanwhile, at catalytic domain, the second oxygen intake is set, is conducive to supplemental oxygen, the excessive problem that affects catalytic reaction of the concentration of carrier gas (nitrogen) the gas of avoiding coming from sample combustion district, improves catalytic reaction efficiency.Catalyzer be chosen as prior art, generally can adopt cupric oxide as catalyzer.
During use, first sample is dried, reaches constant weight, remove the free water in sample.Dry sample is put into sample combustion district, carry out oxidizing fire, the water vapor of generation is carried by carrier gas (nitrogen), after catalytic domain catalysis is further oxidized, through cold-trap, collects, and the water sample of collection is made the sample of liquid flashing counting and measured after distillation.
In actual measurement, for improving the accuracy of measuring, can be in sample oxidizing fire process, adopt elemental analyser to measure the content of protium in sample, the water yield obtaining according to collection is calculated the recovery of protium, by isotopic character, determines the recovery of tritium.
In technique scheme, the described pair of warm area tubular type combustion furnace Shang，Yu sample combustion district and catalytic domain are corresponding, are respectively equipped with independently temperature controller, are electrically connected to and are provided with control system with described temperature controller.
In described sample combustion district, be provided with for holding the example boat of sample.
Preferred technical scheme, described the second oxygen intake is arranged in catalytic domain near the one end in sample combustion district.
Because technique scheme is used, the utility model compared with prior art has following advantages:
1. the temperature of the utility model sample combustion district and catalytic domain can be controlled respectively, coordinates oxygen and nitrogen inlet, and effectively control combustion speed, has solved detonation and the inadequate problem of burning, has improved stability and the reliability measured.
2. the utility model arranges the second oxygen intake at catalytic domain, solved the problem that affects catalytic efficiency because carrier gas concentration is excessive, simultaneously, because the oxygen concentration of catalytic domain is controlled, the nitrogen air inflow in sample combustion district can regulate as required and needn't consider the catalysis problem in later stage, is more conducive to the control to burning.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model embodiment.
Fig. 2 is the schematic diagram of distilling apparatus.
Wherein: 1, sample combustion district; 2, catalytic domain; 3, collecting region; 4, example boat; 5, temperature controller; 6, oxygen and nitrogen inlet; 7, the second oxygen intake; 8, cold-trap gathering-device.
Embodiment
Below in conjunction with drawings and Examples, the utility model is further described:
Embodiment mono-: shown in Figure 1, the sample preparation device that a kind of organic tritium is measured, comprise sample combustion district 1, catalytic domain 2 and collecting region 3, described sample combustion district 1 and catalytic domain 2 mainly consist of two warm area tubular type combustion furnaces of a horizontal positioned, corresponding with sample combustion district 1 and catalytic domain 2, be respectively equipped with independently temperature controller 5, be electrically connected to and be provided with control system with described temperature controller 5; In sample combustion district 1 one sides, be provided with oxygen and nitrogen inlet 6, as required, two entrances can be set, an entrance also can be set, oxygen and nitrogen are being mixed in advance by ingress pipe before this, are provided with for holding the example boat 4 of sample in sample combustion district 1; In described catalytic domain 2, near the one end in sample combustion district 1, be provided with the second oxygen intake 7; Described collecting region is cold-trap gathering-device 8, and described cold-trap gathering-device 8 is communicated with one end away from sample combustion district in catalytic domain 2.
Particularly, described pair of warm area tubular type combustion furnace can comprise the quartz ampoule of a 50mm * 1100mm, and quartz ampoule inner right side is placed with the quartz boat of dress sample, and left side is placed with catalyzer, and catalyzer is cupric oxide; The right-hand end of quartz ampoule is provided with oxygen and nitrogen inlet, and the left distal end of quartz ampoule is inserted with a wireway, as the second oxygen intake, for importing oxygen.Around quartz ampoule, two cover well heater and temperature controllers are set respectively, for the temperature of independent Quality control combustion zone and catalytic domain.Cold-trap is connected with the left end of quartz ampoule, for collecting the water vapor of generation, thereby obtains water sample.
Further, shown in accompanying drawing 2, after the water sample of collecting is taken out, can be placed in cucurbit, add after several beaded glasses, on electric furnace, distill, slip out liquid and be collected in beaker, as treating test sample.
During sample preparation, adopt the mode of oven dry or freeze-drying to be dried to constant weight in fresh sample, dry sample is through pulverizing, take out a small amount of sample measurement protium content, get the about 40g sample of identical sample and put into oxidizing fire device, as Fig. 1, coupling arrangement, collect cold-trap and be placed in 5～10 ℃ of ice-water baths, slow adjusting gas flow meter flow, first combustion zone mixed gas flow is adjusted to 200ml/min(oxygen: nitrogen=50ml/min:150ml/min), then regulate catalytic domain oxygen flow to 100ml/min, after stability of flow, maintain ventilation 5 minutes, air in quartz ampoule is driven out of.
Catalytic domain rises to after 750 ℃ with speed faster, and combustion zone rises to 350 ℃ with 1 ℃/min, keeps this temperature 30min, then with 4 ℃/min, rises to 750 ℃, maintains 2 hours, finally stops heating up, and stops ventilation.Take out cold-trap, weigh and produce quality.
In the water sample of collecting, add sodium peroxide to regulate pH to neutral (6～8), then product water is poured in 50ml cucurbit, add two beaded glasses, add a small amount of potassium permanganate to solution to be purple, put up distilling apparatus, installation drawing is shown in accompanying drawing 2.Get 8ml distillate in 20ml counting vial, add 12ml scintillation solution to mix, put into dark place darkening and measure after 24 hours.
Claims (4)
1. the sample preparation device that organic tritium is measured, comprise sample combustion district, catalytic domain and collecting region, described collecting region is cold-trap gathering-device, described sample combustion district is provided with oxygen and nitrogen inlet, in described catalytic domain, be provided with catalyzer, it is characterized in that: described sample combustion district and catalytic domain mainly consist of two warm area tubular type combustion furnaces of a horizontal positioned, in described catalytic domain one side, be provided with the second oxygen intake, described cold-trap gathering-device is communicated with one end away from sample combustion district in catalytic domain.
2. the sample preparation device that organic tritium according to claim 1 is measured, is characterized in that: the described pair of warm area tubular type combustion furnace Shang，Yu sample combustion district and catalytic domain are corresponding, are respectively equipped with independently temperature controller, are electrically connected to and are provided with control system with described temperature controller.
3. the sample preparation device that organic tritium according to claim 1 is measured, is characterized in that: in described sample combustion district, be provided with for holding the example boat of sample.
4. the sample preparation device that organic tritium according to claim 1 is measured, is characterized in that: described the second oxygen intake is arranged in catalytic domain near the one end in sample combustion district.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320541185.8U CN203479599U (en) | 2013-09-02 | 2013-09-02 | Sample preparation device for organic tritium measurement |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320541185.8U CN203479599U (en) | 2013-09-02 | 2013-09-02 | Sample preparation device for organic tritium measurement |
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| CN203479599U true CN203479599U (en) | 2014-03-12 |
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| CN201320541185.8U Expired - Lifetime CN203479599U (en) | 2013-09-02 | 2013-09-02 | Sample preparation device for organic tritium measurement |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104678047A (en) * | 2015-03-18 | 2015-06-03 | 中国科学院上海应用物理研究所 | Organic tritium oxidation combustion tube and organic tritium oxidation combustion method |
| CN106586961A (en) * | 2016-12-13 | 2017-04-26 | 中国工程物理研究院材料研究所 | Tritiated water preparation apparatus and method |
-
2013
- 2013-09-02 CN CN201320541185.8U patent/CN203479599U/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104678047A (en) * | 2015-03-18 | 2015-06-03 | 中国科学院上海应用物理研究所 | Organic tritium oxidation combustion tube and organic tritium oxidation combustion method |
| CN106586961A (en) * | 2016-12-13 | 2017-04-26 | 中国工程物理研究院材料研究所 | Tritiated water preparation apparatus and method |
| CN106586961B (en) * | 2016-12-13 | 2018-09-07 | 中国工程物理研究院材料研究所 | Surabaya preparation facilities and method |
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Granted publication date: 20140312 |