CN106855473A - A kind of method for preparing the fluid sample of carbon 14 in live graphite - Google Patents
A kind of method for preparing the fluid sample of carbon 14 in live graphite Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 55
- 238000000034 method Methods 0.000 title claims description 54
- 229910002804 graphite Inorganic materials 0.000 title claims description 53
- 239000010439 graphite Substances 0.000 title claims description 53
- OKTJSMMVPCPJKN-NJFSPNSNSA-N Carbon-14 Chemical compound [14C] OKTJSMMVPCPJKN-NJFSPNSNSA-N 0.000 title claims description 45
- 239000012530 fluid Substances 0.000 title 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 88
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 81
- 239000007788 liquid Substances 0.000 claims description 52
- 229910000831 Steel Inorganic materials 0.000 claims description 51
- 239000010959 steel Substances 0.000 claims description 51
- 239000001569 carbon dioxide Substances 0.000 claims description 44
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 44
- 230000002285 radioactive effect Effects 0.000 claims description 44
- 239000007789 gas Substances 0.000 claims description 43
- 238000001179 sorption measurement Methods 0.000 claims description 41
- 238000010521 absorption reaction Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 30
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 claims description 29
- 229910052722 tritium Inorganic materials 0.000 claims description 29
- 238000007789 sealing Methods 0.000 claims description 24
- 238000005192 partition Methods 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000567 combustion gas Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 238000002485 combustion reaction Methods 0.000 description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- XLYOFNOQVPJJNP-PWCQTSIFSA-N Tritiated water Chemical compound [3H]O[3H] XLYOFNOQVPJJNP-PWCQTSIFSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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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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Abstract
本发明公开了一种制备放射性石墨中碳‑14液体样品的方法,该方法包括:提供一密封的反应容器,该反应容器内具有一含氚水蒸气吸附装置,从而将该反应容器的内部空间分割成第一空间和第二空间;所述第一空间内设置有放射性石墨样品,所述第二空间内设置有二氧化碳吸收液;向所述密封的反应容器内充入助燃气,使所述反应容器内的气压强达到1MPa‑4MPa;使所述放射性石墨样品在助燃气中进行燃烧,在所述第一空间形成含氚水蒸气和二氧化碳气体;保持一段时间,使所述含氚水蒸气和二氧化碳气体通过所述吸附装置向所述第二空间扩散,所述含氚水蒸气被所述吸附装置吸收,且所述二氧化碳气体被所述吸收液吸收;对所述密封的反应容器进行排气。
The invention discloses a method for preparing a carbon-14 liquid sample in radioactive graphite. The method comprises: providing a sealed reaction vessel with a tritium-containing water vapor adsorption device in the reaction vessel, so that the inner space of the reaction vessel is Divided into a first space and a second space; the first space is provided with a radioactive graphite sample, and the second space is provided with a carbon dioxide absorbing liquid; the sealed reaction vessel is filled with combustion-supporting gas to make the The air pressure in the reaction vessel reaches 1MPa-4MPa; the radioactive graphite sample is burned in the combustion-supporting gas to form tritium-containing water vapor and carbon dioxide gas in the first space; keep for a period of time to make the tritium-containing water vapor and carbon dioxide gas diffuse to the second space through the adsorption device, the tritium-containing water vapor is absorbed by the adsorption device, and the carbon dioxide gas is absorbed by the absorption liquid; the sealed reaction vessel is exhausted gas.
Description
技术领域technical field
本发明涉及核工业技术领域,尤其涉及一种制备放射性石墨中碳-14液体样品的方法。The invention relates to the technical field of nuclear industry, in particular to a method for preparing a carbon-14 liquid sample in radioactive graphite.
背景技术Background technique
核工业中会使用大量的石墨材料,石墨受到中子辐照后会带有放射性。为处理放射性石墨,必须建立石墨中所含放射性的分析方法,特别是要准确的测定其中碳-14的含量。碳-14分析的难点在于将固体石墨材料中的碳-14制备成液体样品,便于后续使用精密的放射性分析仪器对碳-14进行分析。A large amount of graphite materials are used in the nuclear industry, and graphite becomes radioactive after being irradiated by neutrons. In order to deal with radioactive graphite, it is necessary to establish an analytical method for the radioactivity contained in graphite, especially to accurately determine the content of carbon-14 in it. The difficulty in the analysis of carbon-14 is to prepare the carbon-14 in the solid graphite material into a liquid sample, which is convenient for subsequent analysis of carbon-14 with sophisticated radioactive analysis instruments.
目前广泛采用的是“燃烧-吸收法”制备碳-14的液体样品。即,将含有碳-14的石墨在空气或氧气等助燃气中点燃,使碳转化为二氧化碳,再采用吸收液吸收二氧化碳。由于放射性石墨中还含有另一种放射性核素——氚。在燃烧过程中会形成含氚的水蒸气,也会被吸收液吸收,因此,对后续碳-14的放射性测量产生严重干扰。所以在吸收液之前,都要有一个去除水含氚的水蒸气的过程。例如,邱永梅等在反应堆退役石墨中14C分析制样实验系统研制(原子能科学技术,2010,Vol.44(suppl.):119-123)一文中报道了续碳-14的制备方法和实验装置。其制备碳-14样品方法可以概括为:将石墨在氧气气氛下加热燃烧,气体通过冷凝管和硅胶干燥器来除去含氚水,通过收集器中的吸收液制备碳-14液体样品。然而,该方法和装置具有如下缺点:(1)设备复杂、部件多、体积大、集成度差;(2)难以实现标准化、多数是临时搭建的实验装置,不利于规模化生产和推广使用;(3)控制困难:气体流速太小时不利于石墨完全燃烧、气体流速太大时不利于二氧化碳气体完全被吸收液吸收;(4)放射性废物多:整个管路都会被碳-14、氚沾污;(5)设备存在危险性:石墨粉末比表面积大,与氧气混合易发生爆炸。At present, the "combustion-absorption method" is widely used to prepare liquid samples of carbon-14. That is, the graphite containing carbon-14 is ignited in air or oxygen and other combustion gases to convert the carbon into carbon dioxide, and then absorb the carbon dioxide with the absorbing liquid. Because radioactive graphite also contains another radionuclide - tritium. Tritium-containing water vapor will be formed during the combustion process and will also be absorbed by the absorbing liquid. Therefore, it will seriously interfere with the subsequent carbon-14 radioactivity measurement. Therefore, before absorbing the liquid, there must be a process of removing the water vapor containing tritium in the water. For example, Qiu Yongmei et al. reported the preparation method and experimental device of carbon-14 in the article Development of Experimental System for 14 C Analysis and Sample Preparation in Reactor Decommissioned Graphite (Atomic Energy Science and Technology, 2010, Vol.44(suppl.): 119-123) . The method for preparing carbon-14 samples can be summarized as follows: graphite is heated and burned in an oxygen atmosphere, the gas passes through a condensation tube and a silica gel drier to remove tritium-containing water, and a carbon-14 liquid sample is prepared through the absorption liquid in the collector. However, the method and device have the following disadvantages: (1) complex equipment, many parts, large volume, and poor integration; (2) it is difficult to achieve standardization, and most of them are temporary experimental devices, which are not conducive to large-scale production and popularization; (3) Difficult to control: too small a gas flow rate is not conducive to the complete combustion of graphite, and too high a gas flow rate is not conducive to the complete absorption of carbon dioxide gas by the absorption liquid; (4) There are many radioactive wastes: the entire pipeline will be contaminated by carbon-14 and tritium (5) There is danger in the equipment: graphite powder has a large specific surface area, and it is easy to explode when mixed with oxygen.
为了部分解决上述方法的缺点,特别是出于操作安全的考虑,目前也存在一种使用耐高压样品燃烧装置(氧弹)来制备碳-14样品的技术。这类技术与之前所述样品制备方法的显著区别在于:引入了一种特殊的样品燃烧装置(氧弹)。具体地,该方法为:在一个密闭耐高压样品燃烧装置中使石墨与氧气燃烧生成二氧化碳和含氚水蒸气;然后将燃烧装置的阀门打开,将燃烧生成二氧化碳和含氚水蒸气引导至类似于邱永梅等提供的除水蒸气和吸收二氧化碳的装置中。然而,该方法和装置仍然具有如下缺点:(1)除样品燃烧装置外,需要另外配备除含氚水蒸气和吸收二氧化碳的装置:设备复杂、集成度差、大多需要临时搭建除水和吸收二氧化碳的装置、不利于装置推广使用。如果没有配套装置,则无法去除氚的干扰,难以用于C-14的准确分析;(2)样品燃烧装置的放气操作必须手动控制、工作强度大:样品燃烧装置放气的操作,需要根据内部残留压力来调解一个放气阀,保持放气速度缓慢稳定。目前这个操作只能通过人工手动控制螺旋放气阀来完成,工作人员需要连续数小时持续调解,工作强度很大;(3)手动放气操作造成吸收不稳定,实验误差大:样品燃烧装置放出的气体也要求缓慢通入氚水吸附材料和氢氧化钠溶液,通过速度对氚水和二氧化碳的吸收效果有直接影响。特别是,当通过速度过快会造成吸收率下降,影响测定的碳-14含量。但通过人工控制螺旋放气阀的方式来调节放气速度,放气速度波动大、吸收不稳定、实验误差大、结果重复性差。In order to partially solve the shortcomings of the above methods, especially for the consideration of operational safety, there is also a technology of using a high-pressure sample combustion device (oxygen bomb) to prepare carbon-14 samples. A significant difference between this type of technique and the previously described sample preparation methods is the introduction of a special sample combustion device (oxygen bomb). Specifically, the method is as follows: burning graphite and oxygen in a closed high-pressure sample combustion device to generate carbon dioxide and tritiated water vapor; then opening the valve of the combustion device to guide the combustion to generate carbon dioxide and tritiated water vapor In the device for removing water vapor and absorbing carbon dioxide provided by Qiu Yongmei et al. However, this method and device still have the following disadvantages: (1) In addition to the sample combustion device, additional devices for removing tritium-containing water vapor and absorbing carbon dioxide are required: the equipment is complex, poorly integrated, and most of them require temporary construction to remove water and absorb carbon dioxide device, which is not conducive to the popularization and use of the device. If there is no supporting device, the interference of tritium cannot be removed, and it is difficult to be used for the accurate analysis of C-14; (2) the gas release operation of the sample combustion device must be manually controlled, and the work intensity is high: the gas release operation of the sample combustion device needs to be performed according to Internal residual pressure is used to mediate a deflation valve to keep the deflation rate slow and steady. At present, this operation can only be completed by manually controlling the spiral air release valve, and the staff needs to continue to mediate for several hours, and the work intensity is very high; (3) The manual air release operation causes the absorption to be unstable, and the experimental error is large: the sample combustion device releases The gas also needs to pass slowly into the tritium water adsorption material and sodium hydroxide solution, and the passing speed has a direct impact on the absorption effect of tritium water and carbon dioxide. In particular, when the passing speed is too fast, the absorption rate will decrease, which will affect the measured carbon-14 content. However, by manually controlling the spiral deflation valve to adjust the deflation rate, the deflation rate fluctuates greatly, the absorption is unstable, the experimental error is large, and the repeatability of the results is poor.
因此,提供一种简单有效的制备放射性石墨中碳-14的液体样品的方法成为目前需要解决的技术问题。Therefore, providing a simple and effective method for preparing liquid samples of carbon-14 in radioactive graphite has become a technical problem to be solved at present.
发明内容Contents of the invention
本发明提供一种简单有效的制备放射性石墨中碳-14液体样品的方法。The invention provides a simple and effective method for preparing a carbon-14 liquid sample in radioactive graphite.
一种制备放射性石墨中碳-14液体样品的方法,该方法包括:提供一密封的反应容器,该反应容器内具有一含氚水蒸气吸附装置,从而将该反应容器的内部空间分割成一第一空间和一第二空间;所述第一空间内设置有放射性石墨样品,所述第二空间内设置有二氧化碳吸收液;向所述密封的反应容器内充入助燃气,使所述反应容器内的气压强达到1-4MPa;使所述放射性石墨样品在助燃气中进行燃烧,在所述第一空间形成含氚水蒸气和二氧化碳气体;保持一段时间,使所述含氚水蒸气和二氧化碳气体通过所述吸附装置向所述第二空间扩散,所述含氚水蒸气被所述吸附装置吸收,且所述二氧化碳气体被所述吸收液吸收;以及对所述密封的反应容器进行排气。A method for preparing a carbon-14 liquid sample in radioactive graphite, the method comprising: providing a sealed reaction vessel with a tritium-containing water vapor adsorption device in the reaction vessel, thereby dividing the inner space of the reaction vessel into a first space and a second space; radioactive graphite samples are arranged in the first space, and carbon dioxide absorbing liquid is arranged in the second space; gas-supporting gas is filled into the sealed reaction vessel to make the reaction vessel The air pressure reaches 1-4MPa; the radioactive graphite sample is burned in the combustion-supporting gas to form tritium-containing water vapor and carbon dioxide gas in the first space; keep for a period of time to make the tritium-containing water vapor and carbon dioxide gas Diffusion from the adsorption device to the second space, the tritium-containing water vapor is absorbed by the adsorption device, and the carbon dioxide gas is absorbed by the absorption liquid; and exhausting the sealed reaction container.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述密封的反应容器包括:一承压钢瓶、一顶部端盖、一密封盖、两个电极和一点火丝;所述顶部端盖插入所述承压钢瓶的顶部开口之内,所述密封盖将所述顶部端盖固定在所述承压钢瓶上;所述两个电极间隔设置于所述顶部端盖上,且从外部延伸至所述承压钢瓶内部,所述两个电极延伸至所述承压钢瓶内部的一端通过该点火丝电连接;使所述放射性石墨样品在助燃气中进行燃烧的方法为向所述点火丝通电。The above method for preparing a carbon-14 liquid sample in radioactive graphite, wherein the sealed reaction vessel includes: a pressure-bearing steel cylinder, a top end cap, a sealing cap, two electrodes and a ignition wire; The end cap is inserted into the top opening of the pressure-bearing steel cylinder, and the sealing cap fixes the top end cap on the pressure-bearing steel cylinder; the two electrodes are arranged on the top end cap at intervals, and from The outside extends to the inside of the pressure-bearing steel cylinder, and one end of the two electrodes extending to the inside of the pressure-bearing steel cylinder is electrically connected through the ignition wire; the method for making the radioactive graphite sample burn in the combustion gas is to provide the The ignition wire is energized.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述吸附装置包括一第一透气隔板、一与该第一透气隔板间隔设置的第二透气隔板、一设置于所述第一透气隔板和第二透气隔板之间的水蒸气吸附材料以及一橡胶密封环。The above method for preparing a carbon-14 liquid sample in radioactive graphite, wherein the adsorption device includes a first gas-permeable partition, a second gas-permeable partition spaced apart from the first gas-permeable partition, and a second gas-permeable partition arranged on the The water vapor adsorption material and a rubber sealing ring between the first air-permeable partition and the second air-permeable partition.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述承压钢瓶的内壁为圆柱形,所述吸附装置为圆柱或圆台形,其侧面与所述承压钢瓶的内壁贴合,并依靠橡胶密封环实现侧壁密封。As in the above method for preparing a carbon-14 liquid sample in radioactive graphite, wherein the inner wall of the pressure-bearing steel cylinder is cylindrical, the adsorption device is cylindrical or truncated-conical, and its side is bonded to the inner wall of the pressure-bearing steel cylinder , and rely on rubber sealing ring to achieve side wall sealing.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述水蒸气吸附材料为吸水硅胶。As in the above method for preparing a carbon-14 liquid sample in radioactive graphite, wherein the water vapor adsorption material is water-absorbing silica gel.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述承压钢瓶的内壁上形成台阶或设置凸起,从而使所述吸附装置卡固在该台阶或凸起处。As in the above method for preparing a carbon-14 liquid sample in radioactive graphite, wherein a step or a protrusion is formed on the inner wall of the pressure-bearing steel cylinder, so that the adsorption device is clamped on the step or protrusion.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述两个电极和点火丝设置于所述第一空间;所述充排气阀设置于所述承压钢瓶上且直接与所述第二空间连通;所述密封的反应容器内充入助燃气的方法为通过该充排气阀充入纯氧气。The method for preparing a carbon-14 liquid sample in radioactive graphite as described above, wherein, the two electrodes and the ignition wire are arranged in the first space; the inflation and exhaust valve is arranged on the pressure-bearing steel cylinder and directly connected The second space is connected; the method of filling the sealed reaction vessel with supporting gas is to fill pure oxygen through the filling and exhaust valve.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述吸收液为氢氧化钠溶液。As in the above method for preparing a carbon-14 liquid sample in radioactive graphite, wherein the absorbing liquid is sodium hydroxide solution.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述吸收液中放置一磁力转子;所述使所述含氚水蒸气和二氧化碳气体通过所述吸附装置向所述第二空间扩散的步骤进一步包括:将反应容器放于一个磁力搅拌装置上,通过磁力带动磁力转子对所述吸收液进行搅拌。The method for preparing a carbon-14 liquid sample in radioactive graphite as described above, wherein a magnetic rotor is placed in the absorption liquid; the tritium-containing water vapor and carbon dioxide gas pass through the adsorption device to the second space The step of diffusing further includes: placing the reaction vessel on a magnetic stirring device, and driving the magnetic rotor through magnetic force to stir the absorbing liquid.
如上述的制备放射性石墨中碳-14液体样品的方法,其中,所述吸收液进行搅拌的时间为5-10分钟。As in the above-mentioned method for preparing a carbon-14 liquid sample in radioactive graphite, wherein the time for stirring the absorption liquid is 5-10 minutes.
相较于现有技术,本发明的方法使反应后气体中的二氧化碳扩散到达吸收碱液表面,避免了通过导管引导的手动控制放气过程的难度,不仅降低工作强度、大大提高了样品制备的效率,而且减少了人为的实验误差和不确定性,提高了样品制备过程的可靠性。Compared with the prior art, the method of the present invention allows the carbon dioxide in the reacted gas to diffuse to the surface of the lye to absorb, avoiding the difficulty of manually controlling the deflation process guided by the catheter, not only reducing the work intensity, but also greatly improving the efficiency of sample preparation. Efficiency, but also reduce human experimental errors and uncertainties, and improve the reliability of the sample preparation process.
本发明的其它特征和优点将在随后的说明书中阐述,并且,部分地从说明书中变得显而易见,或者通过实施本发明而了解。本发明的目的和其他优点可通过在所写的说明书、权利要求书、以及附图中所特别指出的结构来实现和获得。Additional features and advantages of the invention will be set forth in the description which follows, and in part will be apparent from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
下面通过附图和实施例,对本发明的技术方案做进一步的详细描述。The technical solutions of the present invention will be described in further detail below with reference to the accompanying drawings and embodiments.
附图说明Description of drawings
附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实施例一起用于解释本发明,并不构成对本发明的限制。在附图中:The accompanying drawings are used to provide a further understanding of the present invention, and constitute a part of the description, and are used together with the embodiments of the present invention to explain the present invention, and do not constitute a limitation to the present invention. In the attached picture:
图1为本发明实施例提供的制备放射性石墨中碳-14的液体样品的实验装置的结构示意图。Fig. 1 is a schematic structural diagram of an experimental device for preparing a liquid sample of carbon-14 in radioactive graphite provided by an embodiment of the present invention.
图2为本发明实施例提供的制备放射性石墨中碳-14的液体样品的方法流程图。Fig. 2 is a flowchart of a method for preparing a liquid sample of carbon-14 in radioactive graphite provided by an embodiment of the present invention.
附图标号说明Explanation of reference numbers
具体实施方式detailed description
以下结合附图对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。The preferred embodiments of the present invention will be described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described here are only used to illustrate and explain the present invention, and are not intended to limit the present invention.
请参见图1,本发明实施例提供的制备放射性石墨中碳-14的液体样品的实验装置10包括:一承压钢瓶101、一顶部端盖102、一密封盖103、两个电极104、一点火丝105、一样品坩埚106、一充排气阀107、一烧杯108、二氧化碳吸收碱液109以及一含氚水蒸气吸附装置110。Please refer to Fig. 1 , the experimental device 10 for preparing the liquid sample of carbon-14 in radioactive graphite provided by the embodiment of the present invention comprises: a pressure-bearing steel cylinder 101, a top end cap 102, a sealing cap 103, two electrodes 104, a point Fire wire 105 , a sample crucible 106 , a filling and exhausting valve 107 , a beaker 108 , a carbon dioxide absorbing lye 109 and a tritium-containing water vapor adsorption device 110 .
所述承压钢瓶101的形状和尺寸不限,可以根据需要设置。可以理解,所述承压钢瓶101也可以为采用其它金属材料制备的可以承受高压的容器。本实施例中,所述承压钢瓶101为圆柱形,其侧边和底部密封,顶部开口且的具有与所述密封盖103配合的螺纹。The shape and size of the pressurized steel cylinder 101 are not limited, and can be set as required. It can be understood that the pressure-bearing steel cylinder 101 can also be a container made of other metal materials that can withstand high pressure. In this embodiment, the pressure-bearing steel cylinder 101 is cylindrical, its sides and bottom are sealed, and its top is open and has threads that match the sealing cap 103 .
所述顶部端盖102用于与所述承压钢瓶101构成一个密封的且可以承受高压的反应腔室。使用时,所述顶部端盖102插入所述承压钢瓶101的顶部开口之内。The top end cap 102 is used to form a sealed reaction chamber with the pressurized steel cylinder 101 that can withstand high pressure. In use, the top end cap 102 is inserted into the top opening of the pressure-bearing steel cylinder 101 .
所述密封盖103用于将所述顶部端盖102固定在所述承压钢瓶101上。所述密封盖103的结构可以根据需要设置。本实施例中,所述密封盖103具有与所述承压钢瓶101的顶部配合的螺纹,且所述密封盖103与所述顶部端盖102为一体结构。使用时,所述密封盖103通过螺旋与所述承压钢瓶101固定连接,从而压住所述顶部端盖102,确保密封完好。The sealing cap 103 is used to fix the top end cap 102 on the pressure steel cylinder 101 . The structure of the sealing cover 103 can be set as required. In this embodiment, the sealing cap 103 has a screw thread matched with the top of the pressure-bearing steel cylinder 101 , and the sealing cap 103 and the top end cap 102 are integrally structured. When in use, the sealing cap 103 is fixedly connected with the pressure-bearing steel cylinder 101 by screwing, thereby pressing the top end cap 102 to ensure a good seal.
所述两个电极104间隔设置于所述顶部端盖102上,且从外部延伸至所述承压钢瓶101内部。所述两个电极104露在外部的一端用于与外部电源连接,延伸至所述承压钢瓶101内部的一端用于施加电压,从而实现点火。所述点火的方式不限,可以为电弧放电等。可以理解,所述两个电极104的设置位置不限于所述顶部端盖102上,也可以设置于所述承压钢瓶101上,只要从外部延伸至所述承压钢瓶101内部即可。本实施例中,所述两个电极104延伸至所述承压钢瓶101内部的一端通过一点火丝105电连接。在外部电源通电情况下,通过所述两个电极104和点火丝105构成一个回路,所述点火丝105会瞬间点火并自身熔断。所述点火丝105会引燃所述样品坩埚106中的石墨待测样品,使样品燃烧气化。可以理解,所述电极104和点火丝105为可选结构,本发明也可以通过其它点燃装置或点燃方式实现引燃,例如将整个反应容器加热。The two electrodes 104 are spaced apart on the top end cap 102 and extend from the outside to the inside of the pressure cylinder 101 . The exposed ends of the two electrodes 104 are used to connect to an external power source, and the ends extending to the inside of the pressure-bearing steel cylinder 101 are used to apply a voltage to achieve ignition. The ignition method is not limited, and may be arc discharge or the like. It can be understood that the location of the two electrodes 104 is not limited to the top end cap 102 , and can also be arranged on the pressure-bearing steel cylinder 101 , as long as they extend from the outside to the inside of the pressure-bearing steel cylinder 101 . In this embodiment, one end of the two electrodes 104 extending to the inside of the pressure cylinder 101 is electrically connected through an ignition wire 105 . When the external power supply is powered on, a circuit is formed by the two electrodes 104 and the ignition wire 105, and the ignition wire 105 will instantly ignite and fuse itself. The ignition wire 105 will ignite the graphite sample to be tested in the sample crucible 106 to make the sample burn and gasify. It can be understood that the electrode 104 and the ignition wire 105 are optional structures, and the present invention can also achieve ignition through other ignition devices or ignition methods, such as heating the entire reaction vessel.
所述样品坩埚106设置于所述承压钢瓶101内,用于承载石墨待测样品。所述样品坩埚106可以设置于所述承压钢瓶101内的一固定装置上。本实施例中,所述样品坩埚106固定于一电极104上,且所述电极104设置于所述顶部端盖102上,从而可以在打开所述顶部端盖102的同时将所述样品坩埚106从所述承压钢瓶101内取出,以便装在样品。可以理解,所述样品坩埚106不限于坩埚,只要是可以耐高温的样品承载装置即可。The sample crucible 106 is set in the pressure-bearing steel cylinder 101 and is used to carry the graphite sample to be tested. The sample crucible 106 can be set on a fixing device inside the pressure cylinder 101 . In this embodiment, the sample crucible 106 is fixed on an electrode 104, and the electrode 104 is arranged on the top end cover 102, so that the sample crucible 106 can be opened while the top end cover 102 is opened. Take it out from the pressure-bearing steel cylinder 101 so as to contain the sample. It can be understood that the sample crucible 106 is not limited to a crucible, as long as it is a sample carrying device that can withstand high temperature.
所述充排气阀107用于燃烧前向所述承压钢瓶101内充入氧气等助燃气,燃烧和吸收完成后排出所述承压钢瓶101内的废气。所述充排气阀107可以设置于所述承压钢瓶101上或所述顶部端盖102上。优选地,所述充排气阀107设置于所述承压钢瓶101上且位于所述样品坩埚106的背面,这样可以避免在充气过程中,气流将所述样品坩埚106内部的样品吹散。现有装置的充排气口通常设置于在所述顶部端盖102上,且正对装载样品的样品坩埚。当装置充入氧气时,进气气流可能将样品吹走。本实施例中,所述充排气阀107设置于所述承压钢瓶101靠近底部的侧壁上。The charging and exhausting valve 107 is used to fill the pressure-bearing steel cylinder 101 with combustion-supporting gas such as oxygen before combustion, and discharge the waste gas in the pressure-bearing steel cylinder 101 after the combustion and absorption are completed. The inflation and exhaust valve 107 may be arranged on the pressure-bearing steel cylinder 101 or on the top end cap 102 . Preferably, the filling and exhausting valve 107 is arranged on the pressure-bearing steel cylinder 101 and located at the back of the sample crucible 106 , so as to prevent the sample inside the sample crucible 106 from being blown away by air flow during the filling process. The filling and exhausting ports of the existing devices are usually arranged on the top end cover 102, facing the sample crucible loaded with samples. When the device is filled with oxygen, the incoming gas flow may blow the sample away. In this embodiment, the inflation and exhaust valve 107 is arranged on the side wall of the pressure-bearing steel cylinder 101 close to the bottom.
所述含吸附装置110设置于所述承压钢瓶101内,从而将所述承压钢瓶101的内部空间分割成一第一空间115和一第二空间116。所述样品坩埚106设置于所述第一空间115内。所述吸附装置110具有多个通孔,所述第一空间115和一第二空间116仅通过所述吸附装置110连通。所述第一空间115内反应生产的含氚水蒸气和二氧化碳气体可以通过所述吸附装置110向所述第二空间116扩散,且所述含氚水蒸气可以被所述吸附装置110中的水蒸气吸附材料吸收。所述吸附装置110包括一第一透气隔板111、一与该第一透气隔板111间隔设置的第二透气隔板113、一设置于所述第一透气隔板111和第二透气隔板113之间的水蒸气吸附材料112以及一橡胶密封环114。优选地,所述第二透气隔板113边缘固定于所述橡胶密封环114上,从而形成一容器,以便放置该水蒸气吸附材料112。本实施例中,所述吸附装置110为圆柱或圆台形,其侧面与所述承压钢瓶101的内壁贴合,并依靠橡胶密封环114实现侧壁密封。所述承压钢瓶101的内壁上可以形成台阶或设置凸起(图未示),从而使所述吸附装置110可以卡固在该台阶或凸起处。所述水蒸气吸附材料112可以为吸水硅胶等。所述吸水硅胶等材料自身堆积时存在大量空隙,与所述第一透气隔板111和第二透气隔板113共同构成了气体在所述第一空间115和一第二空间116之间自由流通的通道。The adsorption-containing device 110 is arranged in the pressure steel cylinder 101 to divide the inner space of the pressure cylinder 101 into a first space 115 and a second space 116 . The sample crucible 106 is disposed in the first space 115 . The adsorption device 110 has a plurality of through holes, and the first space 115 and a second space 116 communicate only through the adsorption device 110 . The tritium-containing water vapor and carbon dioxide gas produced by the reaction in the first space 115 can diffuse to the second space 116 through the adsorption device 110, and the tritium-containing water vapor can be absorbed by the water in the adsorption device 110. Vapor absorbent material absorbs. The adsorption device 110 includes a first air-permeable partition 111, a second air-permeable partition 113 spaced apart from the first air-permeable partition 111, a second air-permeable partition arranged between the first air-permeable partition 111 and the second air-permeable partition. 113 between the water vapor adsorption material 112 and a rubber sealing ring 114 . Preferably, the edge of the second air-permeable partition 113 is fixed on the rubber sealing ring 114 to form a container for placing the water vapor adsorption material 112 . In this embodiment, the adsorption device 110 is in the shape of a cylinder or a truncated cone, and its side is attached to the inner wall of the pressure-bearing steel cylinder 101 , and the side wall is sealed by the rubber sealing ring 114 . A step or a protrusion (not shown) may be formed on the inner wall of the pressure-bearing steel cylinder 101, so that the adsorption device 110 can be clamped on the step or protrusion. The water vapor adsorption material 112 may be water-absorbing silica gel or the like. There are a lot of gaps when the water-absorbing silica gel and other materials are piled up, and together with the first gas-permeable partition 111 and the second gas-permeable partition 113, the gas can freely circulate between the first space 115 and a second space 116 channel.
所述烧杯108设置于所述承压钢瓶101内部的第二空间116内,用于盛放所述吸收碱液109。所述吸收碱液109用于吸收二氧化碳。可以理解,所述烧杯108也可以为其它盛放吸收碱液109的容器。本实施例中,所述烧杯108设置于所述承压钢瓶101底部。所述吸收碱液109为氢氧化钠水溶液。The beaker 108 is arranged in the second space 116 inside the pressure-bearing steel cylinder 101 and is used for containing the absorption lye 109 . The absorption lye 109 is used to absorb carbon dioxide. It can be understood that the beaker 108 can also be other containers for absorbing the lye 109 . In this embodiment, the beaker 108 is arranged at the bottom of the pressure cylinder 101 . The absorption lye 109 is an aqueous sodium hydroxide solution.
进一步,所述烧杯108内还可以包括一磁力转子117。所述磁力转子117用于搅拌所述吸收碱液109,从而加快所述吸收碱液109对二氧化碳的吸收。可以理解,所述磁力转子117为可选结构。Further, the beaker 108 may also include a magnetic rotor 117 . The magnetic rotor 117 is used to stir the absorption lye 109, thereby accelerating the absorption of carbon dioxide by the absorption lye 109. It can be understood that the magnetic rotor 117 is an optional structure.
可以理解,所述烧杯108、样品坩埚106以及二氧化碳吸收碱液109通常并不与其它元件一起生产销售,仅在该实验装置10制备放射性石墨中碳-14的液体样品时放入即可,因此,所述烧杯108、样品坩埚106以及二氧化碳吸收碱液109可以不理解为该实验装置10的一部分。It can be understood that the beaker 108, the sample crucible 106 and the carbon dioxide absorbing lye 109 are generally not produced and sold together with other components, and are only put into the experimental device 10 when preparing a liquid sample of carbon-14 in radioactive graphite, so , the beaker 108 , the sample crucible 106 and the carbon dioxide absorbing lye 109 may not be understood as a part of the experimental device 10 .
请参见图2,本发明实施例进一步提供一种制备放射性石墨中碳-14的液体样品的方法。该方法包括以下步骤:Please refer to FIG. 2 , the embodiment of the present invention further provides a method for preparing a liquid sample of carbon-14 in radioactive graphite. The method includes the following steps:
S11,提供一密封的反应容器,该反应容器内具有一含氚水蒸气吸附装置110,从而将该反应容器的内部空间分割成一第一空间115和一第二空间116;所述第一空间115内设置有放射性石墨样品,所述第二空间116内设置有二氧化碳吸收碱液109;S11, providing a sealed reaction vessel, the reaction vessel has a tritium-containing water vapor adsorption device 110, thereby dividing the internal space of the reaction vessel into a first space 115 and a second space 116; the first space 115 A sample of radioactive graphite is arranged inside, and a carbon dioxide absorbing lye 109 is arranged inside the second space 116;
S12,向所述密封的反应容器内充入氧气等的助燃气,使所述反应容器内的气压强达到1-4MPa;S12, filling the sealed reaction vessel with a gas-supporting gas such as oxygen, so that the air pressure in the reaction vessel reaches 1-4 MPa;
S13,使所述放射性石墨样品在助燃气中进行燃烧,在所述第一空间115形成含氚水蒸气和二氧化碳气体;S13, burning the radioactive graphite sample in a combustion-supporting gas to form tritium-containing water vapor and carbon dioxide gas in the first space 115;
S14,保持一段时间,使所述含氚水蒸气和二氧化碳气体通过所述吸附装置110向所述第二空间116扩散,所述含氚水蒸气被所述吸附装置110吸收,且所述二氧化碳气体被所述吸收碱液109吸收;以及S14, maintain for a period of time, make the tritium-containing water vapor and carbon dioxide gas diffuse to the second space 116 through the adsorption device 110, the tritium-containing water vapor is absorbed by the adsorption device 110, and the carbon dioxide gas absorbed by the absorption lye 109; and
S15,对所述密封的反应容器进行排气。S15, exhausting the sealed reaction container.
可以理解,所述步骤S14中,随着吸收碱液109对二氧化碳的吸收,第一空间115和第二空间116中二氧化碳会自发扩散,一定时间后,使得吸收碱液109对承压钢瓶101中所有二氧化碳完全吸收。而现有技术中,将反应后气体从承压反应容器中排出,再通过导管引导含氚水蒸气被所述吸附装置和二氧化碳气体吸收碱液中。该方法需要手动调控流量,保持流量足够小,避免对吸附除氚效果、二氧化碳吸收效果产生影响。而且,随着反应容器内的气压逐渐下降,需要持续手动调节来保证流量稳定。所述步骤S14中,还可以进一步对所述吸收碱液109进行搅拌,从而加快所述吸收碱液109对二氧化碳的吸收。It can be understood that, in the step S14, as the absorption of lye 109 absorbs carbon dioxide, the carbon dioxide in the first space 115 and the second space 116 will diffuse spontaneously, and after a certain period of time, the absorption of lye 109 in the pressure steel cylinder 101 will All carbon dioxide is completely absorbed. In the prior art, the reacted gas is discharged from the pressurized reaction vessel, and then the tritium-containing water vapor is guided through a conduit to be absorbed into the lye by the adsorption device and carbon dioxide gas. This method needs to manually adjust the flow rate to keep the flow rate small enough to avoid affecting the effect of detritium adsorption and carbon dioxide absorption. Moreover, as the air pressure in the reaction vessel gradually drops, continuous manual adjustment is required to ensure a stable flow rate. In the step S14, the absorption lye 109 may be further stirred, so as to accelerate the absorption of carbon dioxide by the absorption lye 109 .
可以理解,本发明的实验装置10和方法,不仅可以制备放射性石墨中碳-14的液体样品,其可以用于任何反应后生成两种以上不同气体,且有的气体需要被除去,有的气体需要被收集的实验。It can be understood that the experimental device 10 and method of the present invention can not only prepare liquid samples of carbon-14 in radioactive graphite, but also can be used for any reaction to generate more than two different gases, and some gases need to be removed, and some gases need to be removed. Experiments that need to be collected.
以下为本发明制备放射性石墨中碳-14的液体样品方法的具体实施例。The following are specific examples of the method for preparing a liquid sample of carbon-14 in radioactive graphite according to the present invention.
实施例1Example 1
本实施例中,采用实验装置10制备放射性石墨中碳-14的液体样品的方法如下:In the present embodiment, the method for preparing a liquid sample of carbon-14 in radioactive graphite by using experimental device 10 is as follows:
(1)打开该实验装置10的密封盖103,取出顶部端盖102;(1) Open the sealing cover 103 of the experimental device 10, and take out the top end cover 102;
(2)在该顶部端盖102下方的内支架上放好样品坩埚106,品坩埚106内装入质量0.05-0.2g待测放射性石墨样品,并连接好点火丝105;(2) Place the sample crucible 106 on the inner support below the top end cover 102, load the quality 0.05-0.2g radioactive graphite sample to be measured in the sample crucible 106, and connect the ignition wire 105;
(3)将装有固定体积5.0-20.0ml氢氧化钠吸收碱液109的烧杯108放入该承压钢瓶101底部;(3) Put the beaker 108 equipped with a fixed volume of 5.0-20.0ml sodium hydroxide to absorb the lye 109 into the bottom of the pressure cylinder 101;
(4)根据需要在氚水蒸汽吸附装置110中装入适量硅胶水蒸气吸附材料112,封闭后放入该承压钢瓶101内部,保证该承压钢瓶101的内壁四周被该吸附装置110密封;(4) according to needs, in the tritium water vapor adsorption device 110, pack an appropriate amount of silica gel water vapor adsorption material 112, put into this pressure-bearing steel cylinder 101 inside after sealing, guarantee that the inner wall of this pressure-bearing steel cylinder 101 is sealed by this adsorption device 110 around;
(5)装回顶部端盖102,使电极104、点火丝105、样品坩埚106、和待燃烧样品装入该承压钢瓶101内;(5) Put back the top end cap 102, make the electrode 104, ignition wire 105, sample crucible 106, and the sample to be burned be packed in this pressure-bearing steel cylinder 101;
(6)封好该螺旋密封盖103;(6) seal the screw seal cover 103;
(7)从该充排气阀107充入适量的高压氧气,使该承压钢瓶101内部压强达到1MPa-4MPa;(7) Charge an appropriate amount of high-pressure oxygen from the filling and exhausting valve 107, so that the internal pressure of the pressurized steel cylinder 101 reaches 1MPa-4MPa;
(8)将整个实验装置10置于冷水水域中,检漏确保实验装置10密封;(8) The whole experimental device 10 is placed in cold water, and leak detection ensures that the experimental device 10 is sealed;
(9)连接电极104到外部电源,通过外部电源点火引燃点火丝105和石墨待燃烧样品;(9) Connect the electrode 104 to an external power supply, and ignite the ignition wire 105 and the graphite sample to be burned by igniting the external power supply;
(10)待样品燃烧完成并降温后,将实验装置10放于一个磁力搅拌装置上,通过磁力带动烧杯108中磁力转子117对吸收碱液109搅拌5-10分钟,促进该吸收碱液109对气体中二氧化碳的吸收;(10) After the sample combustion is completed and cooled, the experimental device 10 is placed on a magnetic stirring device, and the magnetic rotor 117 in the beaker 108 is driven by magnetic force to stir the absorption lye 109 for 5-10 minutes to promote the absorption of the lye 109 to the Absorption of carbon dioxide in gases;
(11)二氧化碳吸收完全后,通过该充排气阀107将该承压钢瓶101中的气体排出,不必考虑排出速度,可以快速完成放气过程;(11) After the carbon dioxide is absorbed completely, the gas in the pressurized steel cylinder 101 is discharged through the filling and exhausting valve 107, without considering the discharge speed, and the deflation process can be quickly completed;
(12)打开该密封盖103,取出烧杯108,烧杯108中的氢氧化钠吸收碱液109作为后续分析样品。(12) Open the sealing cover 103, take out the beaker 108, and the sodium hydroxide in the beaker 108 absorbs the lye 109 as a follow-up analysis sample.
为了检测本发明的实验装置10和制备方法中吸收碱液109对气体中二氧化碳的吸收情况,本实施例中,通过该充排气阀107将该承压钢瓶101中的气体排出的过程中,通过导管将排除的气体先缓慢通入另一烧杯内的第二氢氧化钠吸收碱液中,是该第二氢氧化钠吸收碱液进一步吸收气体残余的二氧化碳。结果发现,该第二氢氧化钠吸收碱液中吸收的二氧化碳几乎为零。由此可见,本发明的实验装置10和制备方法中吸收碱液109可以将该承压钢瓶101中的二氧化碳完全吸收。In order to detect the absorption of lye 109 in the experimental device 10 and the preparation method of the present invention to the absorption of carbon dioxide in the gas, in the present embodiment, in the process of discharging the gas in the pressurized steel cylinder 101 through the inflation and exhaust valve 107, Through the conduit, the exhausted gas is first slowly passed into the second sodium hydroxide absorption lye in another beaker, which is the second sodium hydroxide absorption lye to further absorb the carbon dioxide remaining in the gas. As a result, it was found that the carbon dioxide absorbed in the second sodium hydroxide absorption lye was almost zero. It can be seen that the absorption lye 109 in the experimental device 10 and the preparation method of the present invention can completely absorb the carbon dioxide in the pressurized steel cylinder 101 .
本发明具有以下优点:本发明的装置将含氚水蒸气吸收、二氧化碳吸收以及样品燃烧等功能都集成在承压钢瓶内部,操作简单;本发明的方法使反应后气体中的二氧化碳扩散到达吸收碱液表面,避免了通过导管引导的手动控制放气过程的难度,不仅降低工作强度、大大提高了样品制备的效率,而且减少了人为的实验误差和不确定性,提高了样品制备过程的可靠性。The invention has the following advantages: the device of the invention integrates functions such as tritium-containing water vapor absorption, carbon dioxide absorption, and sample combustion inside the pressure-bearing steel cylinder, and is easy to operate; the method of the invention makes the carbon dioxide in the reacted gas diffuse to reach the absorption base The surface of the liquid avoids the difficulty of manually controlling the deflation process guided by the catheter, which not only reduces the work intensity, greatly improves the efficiency of sample preparation, but also reduces artificial experimental errors and uncertainties, and improves the reliability of the sample preparation process .
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalent technologies, the present invention also intends to include these modifications and variations.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018099429A1 (en) * | 2016-12-01 | 2018-06-07 | 清华大学 | Experimental device for preparing liquid sample of carbon-14 in radioactive graphite |
WO2018099428A1 (en) * | 2016-12-01 | 2018-06-07 | 清华大学 | Method for preparing liquid sample of carbon-14 in radioactive graphite |
CN110672778A (en) * | 2019-10-31 | 2020-01-10 | 上海屹尧仪器科技发展有限公司 | Oxygen combustion reaction kettle capable of being ignited by microwave |
CN113295498A (en) * | 2021-06-09 | 2021-08-24 | 广州海洋地质调查局 | Organic sulfur's extraction element in kerogen |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1195570A (en) * | 1996-12-24 | 1998-10-14 | 液体空气乔治洛德方法利用和研究有限公司 | Thermally insulated reactor |
CN1330970A (en) * | 2000-06-29 | 2002-01-16 | 波克股份有限公司 | Purification of gas |
US20040178124A1 (en) * | 2003-03-11 | 2004-09-16 | Ke Liu | Hydrogen desulfurizer for hydrocarbon feeds with separated adsorption and catalyst material |
CN1864810A (en) * | 2005-05-20 | 2006-11-22 | 财团法人工业技术研究院 | Waste gas treatment equipment and method using scrubber and membrane bioreactor |
CN201454533U (en) * | 2009-06-11 | 2010-05-12 | 中国矿业大学 | A combustion synthesis device |
CN202204703U (en) * | 2011-08-31 | 2012-04-25 | 江苏省辐射环境监测管理站 | Tritium and carbon-14 collection device |
CN103118775A (en) * | 2010-07-16 | 2013-05-22 | 乔治洛德方法研究和开发液化空气有限公司 | Adsorber having inner coating |
CN103529162A (en) * | 2013-10-29 | 2014-01-22 | 四川农业大学 | Determination method for total organic carbon (TOC) of solid combustible matters |
CN104280354A (en) * | 2014-10-27 | 2015-01-14 | 合肥卓越分析仪器有限责任公司 | Method for detecting sulfur content of coal test sample |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4255870B2 (en) * | 2004-03-26 | 2009-04-15 | 三菱電機株式会社 | Tritium sampler |
CN103728653A (en) * | 2013-07-02 | 2014-04-16 | 中国工程物理研究院核物理与化学研究所 | Sample preparation system of carbon-14 in solid sample |
CN205353376U (en) * | 2015-01-27 | 2016-06-29 | 上海怡星机电设备有限公司 | Organic tritium carbon collecting system |
CN106706383A (en) * | 2016-12-01 | 2017-05-24 | 清华大学 | Experimental device for preparing carbon-14 liquid sample in radioactive graphite |
CN106855473A (en) * | 2016-12-01 | 2017-06-16 | 清华大学 | A kind of method for preparing the fluid sample of carbon 14 in live graphite |
-
2016
- 2016-12-01 CN CN201611090947.1A patent/CN106855473A/en active Pending
-
2017
- 2017-11-30 WO PCT/CN2017/113937 patent/WO2018099428A1/en active Application Filing
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1195570A (en) * | 1996-12-24 | 1998-10-14 | 液体空气乔治洛德方法利用和研究有限公司 | Thermally insulated reactor |
CN1330970A (en) * | 2000-06-29 | 2002-01-16 | 波克股份有限公司 | Purification of gas |
US20040178124A1 (en) * | 2003-03-11 | 2004-09-16 | Ke Liu | Hydrogen desulfurizer for hydrocarbon feeds with separated adsorption and catalyst material |
CN1864810A (en) * | 2005-05-20 | 2006-11-22 | 财团法人工业技术研究院 | Waste gas treatment equipment and method using scrubber and membrane bioreactor |
CN201454533U (en) * | 2009-06-11 | 2010-05-12 | 中国矿业大学 | A combustion synthesis device |
CN103118775A (en) * | 2010-07-16 | 2013-05-22 | 乔治洛德方法研究和开发液化空气有限公司 | Adsorber having inner coating |
CN202204703U (en) * | 2011-08-31 | 2012-04-25 | 江苏省辐射环境监测管理站 | Tritium and carbon-14 collection device |
CN103529162A (en) * | 2013-10-29 | 2014-01-22 | 四川农业大学 | Determination method for total organic carbon (TOC) of solid combustible matters |
CN104280354A (en) * | 2014-10-27 | 2015-01-14 | 合肥卓越分析仪器有限责任公司 | Method for detecting sulfur content of coal test sample |
Non-Patent Citations (1)
Title |
---|
邱永梅 等: "反应堆退役石墨中14C分析制样实验系统研制", 《原子能科学技术》 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018099429A1 (en) * | 2016-12-01 | 2018-06-07 | 清华大学 | Experimental device for preparing liquid sample of carbon-14 in radioactive graphite |
WO2018099428A1 (en) * | 2016-12-01 | 2018-06-07 | 清华大学 | Method for preparing liquid sample of carbon-14 in radioactive graphite |
CN110672778A (en) * | 2019-10-31 | 2020-01-10 | 上海屹尧仪器科技发展有限公司 | Oxygen combustion reaction kettle capable of being ignited by microwave |
CN110672778B (en) * | 2019-10-31 | 2022-03-01 | 上海屹尧仪器科技发展有限公司 | Oxygen combustion reaction kettle capable of being ignited by microwave |
CN113295498A (en) * | 2021-06-09 | 2021-08-24 | 广州海洋地质调查局 | Organic sulfur's extraction element in kerogen |
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