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CN117554461A - Calibration method and calibration device of hydrogen meter - Google Patents

Calibration method and calibration device of hydrogen meter Download PDF

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Publication number
CN117554461A
CN117554461A CN202311514967.7A CN202311514967A CN117554461A CN 117554461 A CN117554461 A CN 117554461A CN 202311514967 A CN202311514967 A CN 202311514967A CN 117554461 A CN117554461 A CN 117554461A
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hydrogen
alkali metal
liquid
concentration
liquid alkali
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宋德宽
段天英
余华金
张川
杨红义
吴水金
侯斌
杨建伟
刘林顶
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode

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Abstract

本申请的实施例涉及借助于测定材料的化学或物理性质来测试或分析材料,具体涉及一种氢计的标定方法及标定装置。标定方法包括:向液态碱金属回路中注入含氢气体,形成包含含氢化合物的含氢碱金属液体;确定液态碱金属回路中氢的浓度;利用高真空系统、质谱仪和离子泵实现对进入氢渗透结构的气体的组成成分和浓度的检测;根据液态碱金属回路中氢的浓度和质谱仪检测的气体组成成分,对离子泵检测的气体浓度进行标定。标定装置包括液态碱金属流动的液态碱金属回路、供应含氢气体的氢气供应部、控制氢计的控制部以及对氢计进行标定的处理部。本申请的实施例提供的氢计的标定方法及标定装置,能够使标定后的氢计的检测结果更加准确可靠。

Embodiments of the present application relate to testing or analyzing materials by measuring their chemical or physical properties, and specifically relate to a calibration method and calibration device of a hydrogen meter. The calibration method includes: injecting hydrogen-containing gas into the liquid alkali metal circuit to form a hydrogen-containing alkali metal liquid containing hydrogen-containing compounds; determining the concentration of hydrogen in the liquid alkali metal circuit; using a high vacuum system, mass spectrometer and ion pump to achieve incoming calibration Detection of the composition and concentration of gas in the hydrogen permeation structure; calibrating the gas concentration detected by the ion pump based on the concentration of hydrogen in the liquid alkali metal circuit and the gas composition detected by the mass spectrometer. The calibration device includes a liquid alkali metal circuit through which liquid alkali metal flows, a hydrogen supply part for supplying hydrogen-containing gas, a control part for controlling the hydrogen meter, and a processing part for calibrating the hydrogen meter. The calibration method and calibration device of the hydrogen meter provided by the embodiments of the present application can make the detection results of the calibrated hydrogen meter more accurate and reliable.

Description

氢计的标定方法及标定装置Calibration method and calibration device of hydrogen meter

技术领域Technical field

本申请的实施例涉及借助于测定材料的化学或物理性质来测试或分析材料,具体涉及一种氢计的标定方法及标定装置。Embodiments of the present application relate to testing or analyzing materials by measuring their chemical or physical properties, and specifically relate to a calibration method and calibration device of a hydrogen meter.

背景技术Background technique

扩散式氢计是根据氢通过镍的扩散渗透原理工作的。扩散式氢计以薄壁镍管作为传感器,传感器的一侧与蒸汽发生器或过热器的钠与氩气相连,另一侧与真空系统相接。当水/水蒸气泄漏时,钠水反应生成氢气和氢离子,钠和氩气中的氢浓度增加,氢便通过镍管扩散至真空系统,这样真空系统中的氢分压升高,与高真空系统相连的离子泵可以探测到氢分压的变化,从而得知泄漏及泄漏率的大小。Diffusion hydrogen meters work on the principle of diffusion and penetration of hydrogen through nickel. The diffusion hydrogen meter uses a thin-walled nickel tube as a sensor. One side of the sensor is connected to the sodium and argon gas of the steam generator or superheater, and the other side is connected to the vacuum system. When water/water vapor leaks, the sodium-water reaction generates hydrogen gas and hydrogen ions. The hydrogen concentration in the sodium and argon gas increases, and the hydrogen diffuses into the vacuum system through the nickel tube. In this way, the hydrogen partial pressure in the vacuum system increases, which is related to the high The ion pump connected to the vacuum system can detect changes in hydrogen partial pressure, thereby knowing the size of the leak and the leak rate.

快中子反应堆中用氢计检测液态金属钠或高温氩气中的氢浓度时,需要氢计在氢浓度发生变化时能准确地检测到氢浓度变化并产生响应的信号。因此,扩散型氢计设备在使用前或长期使用后需要对其进行标定,以保证监测数据的有效性。When using a hydrogen meter to detect the hydrogen concentration in liquid metal sodium or high-temperature argon in a fast neutron reactor, the hydrogen meter needs to be able to accurately detect changes in hydrogen concentration and generate a response signal when the hydrogen concentration changes. Therefore, diffusion hydrogen meter equipment needs to be calibrated before use or after long-term use to ensure the validity of monitoring data.

发明内容Contents of the invention

针对上述技术问题,本申请的实施例提供了一种氢计的标定方法及标定装置,以对氢计进行标定,从而提高氢计测量结果的准确性。In view of the above technical problems, embodiments of the present application provide a calibration method and calibration device of a hydrogen meter to calibrate the hydrogen meter, thereby improving the accuracy of the hydrogen meter measurement results.

第一方面,本申请的实施例提供了一种氢计的标定方法,其中,氢计包括测量腔、氢渗透结构、质谱仪以及含有离子泵的高真空系统,测量腔用于接收含氢碱金属液体,氢渗透结构位于测量腔内,高真空系统用于为氢渗透结构提供高真空环境以使含氢碱金属液体中的氢渗透进入氢渗透结构内;其中,标定方法包括:提供用于供液态碱金属流动的液态碱金属回路;向液态碱金属回路中注入含氢气体,以形成包含含氢化合物的含氢碱金属液体;确定液态碱金属回路中氢的浓度;利用高真空系统使含氢碱金属液体中的氢及其他气体渗透进入氢渗透结构内;利用质谱仪检测进入氢渗透结构的气体组成成分;利用离子泵检测进入氢渗透结构的气体浓度;根据液态碱金属回路中氢的浓度和质谱仪检测的气体组成成分,对离子泵检测的气体浓度进行标定。In a first aspect, embodiments of the present application provide a calibration method for a hydrogen meter, wherein the hydrogen meter includes a measurement chamber, a hydrogen permeability structure, a mass spectrometer, and a high vacuum system containing an ion pump, and the measurement chamber is used to receive a hydrogen-containing alkali. Metal liquid, hydrogen permeability structure is located in the measurement chamber, and the high vacuum system is used to provide a high vacuum environment for the hydrogen permeation structure to allow hydrogen in the hydrogen-containing alkali metal liquid to permeate into the hydrogen permeation structure; wherein, the calibration method includes: providing A liquid alkali metal circuit for the flow of liquid alkali metal; injecting hydrogen-containing gas into the liquid alkali metal circuit to form a hydrogen-containing alkali metal liquid containing hydrogen-containing compounds; determining the concentration of hydrogen in the liquid alkali metal circuit; using a high vacuum system to Hydrogen and other gases in the hydrogen-containing alkali metal liquid penetrate into the hydrogen permeation structure; use a mass spectrometer to detect the gas composition entering the hydrogen permeation structure; use an ion pump to detect the gas concentration entering the hydrogen permeation structure; according to the hydrogen in the liquid alkali metal circuit The concentration and the gas composition detected by the mass spectrometer are used to calibrate the gas concentration detected by the ion pump.

第二方面,本申请的实施例提供了一种氢计的标定装置,氢计包括测量腔、氢渗透结构、质谱仪以及含有离子泵的高真空系统,测量腔用于接收含氢碱金属液体,氢渗透结构位于测量腔内,高真空系统用于为氢渗透结构提供高真空环境以使含氢碱金属液体中的氢渗透进入氢渗透结构内。其中,标定装置包括:液态碱金属回路,用于供液态碱金属流动,液态碱金属回路具有标定接口,标定接口用于连接氢计的测量腔,以使液态碱金属能够进入氢计的测量腔;氢气供应部,用于向液态碱金属回路中供应含氢气体以形成包含含氢化合物的含氢碱金属液体;控制部,用于控制氢计的高真空系统开启,以使进入测量腔的液态碱金属中的氢及其他气体进入氢渗透结构,控制质谱仪检测进入氢渗透结构的气体组成成分,控制离子泵检测进入氢渗透结构的气体浓度;以及处理部,用于根据液态碱金属回路中氢的浓度以及质谱仪检测的气体组成成分对离子泵检测的气体浓度进行标定。In a second aspect, embodiments of the present application provide a calibration device for a hydrogen meter. The hydrogen meter includes a measurement chamber, a hydrogen permeability structure, a mass spectrometer, and a high vacuum system containing an ion pump. The measurement chamber is used to receive a hydrogen-containing alkali metal liquid. , the hydrogen permeation structure is located in the measurement chamber, and the high vacuum system is used to provide a high vacuum environment for the hydrogen permeation structure to allow hydrogen in the hydrogen-containing alkali metal liquid to permeate into the hydrogen permeation structure. Among them, the calibration device includes: a liquid alkali metal circuit for supplying the flow of liquid alkali metal. The liquid alkali metal circuit has a calibration interface. The calibration interface is used to connect the measurement cavity of the hydrogen meter so that the liquid alkali metal can enter the measurement cavity of the hydrogen meter. ; The hydrogen supply part is used to supply hydrogen-containing gas to the liquid alkali metal circuit to form a hydrogen-containing alkali metal liquid containing hydrogen-containing compounds; the control part is used to control the opening of the high vacuum system of the hydrogen meter so that the gas entering the measurement chamber Hydrogen and other gases in the liquid alkali metal enter the hydrogen permeation structure, control the mass spectrometer to detect the gas composition entering the hydrogen permeation structure, and control the ion pump to detect the gas concentration entering the hydrogen permeation structure; and a processing part for controlling the liquid alkali metal circuit The concentration of hydrogen in the medium and the gas composition detected by the mass spectrometer calibrate the gas concentration detected by the ion pump.

本申请的实施例提供的氢计的标定方法及标定装置,能够根据液态碱金属回路中氢的浓度以及质谱仪检测的气体组成成分对离子泵检测的气体浓度进行标定,从而使得标定后的氢计测量结果更为准确。The calibration method and calibration device of the hydrogen meter provided by the embodiments of the present application can calibrate the gas concentration detected by the ion pump according to the concentration of hydrogen in the liquid alkali metal circuit and the gas composition detected by the mass spectrometer, so that the calibrated hydrogen The meter measurement results are more accurate.

附图说明Description of the drawings

通过下文中参照附图对本申请的实施例所作的描述,本申请的其它目的和优点将显而易见,并可帮助对本申请有全面的理解。Through the following description of the embodiments of the present application with reference to the accompanying drawings, other objects and advantages of the present application will be apparent and may help to have a comprehensive understanding of the present application.

图1是本申请的实施例的氢计的结构示意图;Figure 1 is a schematic structural diagram of a hydrogen meter according to an embodiment of the present application;

图2是本申请的实施例的标定装置的示意性原理图;Figure 2 is a schematic schematic diagram of the calibration device according to the embodiment of the present application;

图3是本申请的实施例的氢计的标定方法的流程示意图。Figure 3 is a schematic flow chart of the calibration method of the hydrogen meter according to the embodiment of the present application.

附图标记说明:Explanation of reference symbols:

10、液态碱金属回路;101、标定接口;102、第一管路;1021、第一管路阀门;1022、第一管路电动阀门;1023、第一管路流量计;103、第二管路;1031、第二管路阀门;1032、第二管路阀门;1033、第二管路阀门;1034、第二管路流量计;104、第三管路;105、第四管路;1051、第四管路阀门;106、第五管路;1061、第五管路阀门;11、氢气供应部;111、氢气管路;1111、氢气接口;12、控制部;13、处理部;14、阻塞计;141、阻塞计阀门;142、阻塞计阀门;15、冷却部;151、冷却阀门;152、冷却阀门;16、缓冲罐;17、惰性气体供应部;171、气体管路;1711、阀门;172、气体管路;1721、阀门;1722、阀门;173、气体管路;1731、阀门;18、电磁泵;19、液态碱金属容器;20、真空部;201、真空阀门;21、冷却风机;22、空冷器;221、空冷阀门;25、测温件;31、仪表;10. Liquid alkali metal circuit; 101. Calibration interface; 102. First pipeline; 1021. First pipeline valve; 1022. First pipeline electric valve; 1023. First pipeline flow meter; 103. Second pipeline 1031. Second pipeline valve; 1032. Second pipeline valve; 1033. Second pipeline valve; 1034. Second pipeline flow meter; 104. Third pipeline; 105. Fourth pipeline; 1051 , the fourth pipeline valve; 106. the fifth pipeline; 1061. the fifth pipeline valve; 11. hydrogen supply department; 111. hydrogen pipeline; 1111. hydrogen interface; 12. control department; 13. processing department; 14 , obstruction meter; 141. obstruction meter valve; 142. obstruction meter valve; 15. cooling department; 151. cooling valve; 152. cooling valve; 16. buffer tank; 17. inert gas supply department; 171. gas pipeline; 1711 , valve; 172, gas pipeline; 1721, valve; 1722, valve; 173, gas pipeline; 1731, valve; 18, electromagnetic pump; 19, liquid alkali metal container; 20, vacuum department; 201, vacuum valve; 21 , cooling fan; 22. air cooler; 221. air cooling valve; 25. temperature measuring piece; 31. instrument;

8、氢计;81、电磁驱动设备;82、加热装置;83、测量腔;831、内套管;832、外套管;84、氢渗透结构;85、高真空系统;86、离子泵;87、质谱仪。8. Hydrogen meter; 81. Electromagnetic driving equipment; 82. Heating device; 83. Measuring chamber; 831. Inner casing; 832. Outer casing; 84. Hydrogen permeability structure; 85. High vacuum system; 86. Ion pump; 87 , mass spectrometer.

需要说明的是,附图并不一定按比例来绘制,而是仅以不影响读者理解的示意性方式示出。It should be noted that the drawings are not necessarily drawn to scale, but are only shown in a schematic manner that does not affect the reader's understanding.

具体实施方式Detailed ways

为使本申请的目的、技术方案和优点更加清楚,下面将结合本申请实施例的附图,对本申请的技术方案进行清楚、完整地描述。显然,所描述的实施例是本申请的一个实施例,而不是全部的实施例。基于所描述的本申请的实施例,本领域普通技术人员在无需创造性劳动的前提下所获得的所有其他实施例,都属于本申请保护的范围。In order to make the purpose, technical solutions and advantages of the present application clearer, the technical solutions of the present application will be clearly and completely described below in conjunction with the drawings of the embodiments of the present application. Obviously, the described embodiment is one embodiment of the present application, but not all embodiments. Based on the described embodiments of the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present application.

需要说明的是,除非另外定义,本申请使用的技术术语或者科学术语应当为本申请所属领域内具有一般技能的人士所理解的通常意义。若全文中涉及“第一”、“第二”等描述,则该“第一”、“第二”等描述仅用于区别类似的对象,而不能理解为指示或暗示其相对重要性、先后次序或者隐含指明所指示的技术特征的数量,应该理解为“第一”、“第二”等描述的数据在适当情况下可以互换。若全文中出现“和/或”,其含义为包括三个并列方案,以“A和/或B”为例,包括A方案,或B方案,或A和B同时满足的方案。此外,为了便于描述,在这里可以使用空间相对术语,如“上方”、“下方”、“顶部”、“底部”等,仅用来描述如图中所示的一个器件或特征与其他器件或特征的空间位置关系,应当理解为也包含除了图中所示的方位之外的在使用或操作中的不同方位。It should be noted that, unless otherwise defined, the technical terms or scientific terms used in this application should have the usual meanings understood by those with ordinary skills in the field to which this application belongs. If descriptions such as "first" and "second" are involved in the full text, the descriptions such as "first" and "second" are only used to distinguish similar objects and cannot be understood as indicating or implying their relative importance or sequence. The order or implicit indication of the number of technical features indicated should be understood to mean that the data described by "first", "second", etc. can be interchanged under appropriate circumstances. If "and/or" appears in the entire text, it means that it includes three parallel plans. Taking "A and/or B" as an example, it includes plan A, or plan B, or a plan that satisfies both A and B at the same time. In addition, for ease of description, spatially relative terms, such as "above", "below", "top", "bottom", etc., may be used herein, and are only used to describe the relationship between one device or feature as shown in the figures and other devices or features. The spatial positional relationship of features should be understood to also include different orientations in use or operation in addition to the orientation shown in the figures.

快中子反应堆中用氢计检测液态金属钠或高温氩气中的氢浓度时,需要氢计在氢浓度发生变化时能准确地检测到氢浓度变化并产生响应的信号。因此,扩散型氢计设备在使用前或长期使用后需要对其进行标定,以保证监测数据的有效性。When using a hydrogen meter to detect the hydrogen concentration in liquid metal sodium or high-temperature argon in a fast neutron reactor, the hydrogen meter needs to be able to accurately detect changes in hydrogen concentration and generate a response signal when the hydrogen concentration changes. Therefore, diffusion hydrogen meter equipment needs to be calibrated before use or after long-term use to ensure the validity of monitoring data.

针对上述技术问题,本申请的实施例提供了一种氢计的标定装置。如图1所示,其示出本申请的实施例中待标定的氢计8的结构示意图。该氢计8可以包括测量腔83、氢渗透结构84、质谱仪87以及含有离子泵的高真空系统85,测量腔83用于接收含氢碱金属液体,氢渗透结构84部分位于测量腔83内,高真空系统85用于为氢渗透结构84提供高真空环境以使含氢碱金属液体中的氢渗透进入氢渗透结构84内。To address the above technical problems, embodiments of the present application provide a calibration device for a hydrogen meter. As shown in Figure 1, it shows a schematic structural diagram of a hydrogen meter 8 to be calibrated in an embodiment of the present application. The hydrogen meter 8 may include a measurement chamber 83, a hydrogen permeation structure 84, a mass spectrometer 87 and a high vacuum system 85 containing an ion pump. The measurement chamber 83 is used to receive hydrogen-containing alkali metal liquid, and the hydrogen permeation structure 84 is partially located in the measurement chamber 83. , the high vacuum system 85 is used to provide a high vacuum environment for the hydrogen permeation structure 84 so that the hydrogen in the hydrogen-containing alkali metal liquid permeates into the hydrogen permeation structure 84 .

容易理解,对于氢渗透结构84而言,小分子透过率高,大分子透过率低,因此,液态金属和/或惰性气体中的绝大部分氢会进入氢渗透结构84内,少量氧氮等其他气体也会扩散进入氢渗透结构84内。质谱仪87能够检测进入氢渗透结构84的气体组成成分,如检测出氢渗透结构84内的气体中各种气体如氢、氧、氮等的含量。离子泵86能够检测氢渗透结构84的气体浓度。It is easy to understand that for the hydrogen permeable structure 84, the transmittance of small molecules is high and the transmittance of macromolecules is low. Therefore, most of the hydrogen in the liquid metal and/or inert gas will enter the hydrogen permeable structure 84, and a small amount of oxygen will enter the hydrogen permeable structure 84. Other gases such as nitrogen may also diffuse into the hydrogen permeable structure 84 . The mass spectrometer 87 can detect the components of the gas entering the hydrogen permeation structure 84, such as detecting the contents of various gases such as hydrogen, oxygen, nitrogen, etc. in the gas within the hydrogen permeation structure 84. Ion pump 86 is capable of detecting the gas concentration of hydrogen permeable structure 84 .

氢计8还可以包括内套管831和位于内套管831径向外侧的外套管832,氢渗透结构84位于内套管831内部,内套管831限定形成测量腔83。液态金属从内套管831和外套管832之间的环形间隙进入内套管831,流经氢渗透结构84后向外流出。The hydrogen meter 8 may also include an inner sleeve 831 and an outer sleeve 832 located radially outside the inner sleeve 831 . The hydrogen permeation structure 84 is located inside the inner sleeve 831 , and the inner sleeve 831 defines a measurement chamber 83 . The liquid metal enters the inner casing 831 from the annular gap between the inner casing 831 and the outer casing 832, flows through the hydrogen permeation structure 84, and then flows out.

氢计8还可以包括电磁驱动设备81,用于驱动液态金属流入测量腔83并从测量腔83中流出。氢计8还可以包括加热装置82,用于加热液态金属,以在不同温度下检测液态金属中的氢浓度。液态金属例如可以为液钠。在一些实施例中,氢计8还可以包括热电偶,用于检测氢渗透结构84温度。The hydrogen meter 8 may also include an electromagnetic driving device 81 for driving liquid metal to flow into and out of the measurement chamber 83 . The hydrogen meter 8 may also include a heating device 82 for heating the liquid metal to detect the hydrogen concentration in the liquid metal at different temperatures. The liquid metal may be liquid sodium, for example. In some embodiments, the hydrogen meter 8 may also include a thermocouple for detecting the temperature of the hydrogen permeation structure 84 .

如图2所示,其示出本申请的实施例提供的标定装置的示意性原理图,该装置可以包括:液态碱金属回路10,氢气供应部11,控制部12和处理部13。As shown in FIG. 2 , it shows a schematic principle diagram of a calibration device provided by an embodiment of the present application. The device may include: a liquid alkali metal circuit 10 , a hydrogen supply part 11 , a control part 12 and a processing part 13 .

液态碱金属回路10可以用于供液态碱金属流动,液态碱金属回路10具有标定接口101。标定接口101可以用于连接氢计8的测量腔83,以使液态碱金属能够进入氢计8的测量腔83。The liquid alkali metal circuit 10 can be used to supply liquid alkali metal to flow, and the liquid alkali metal circuit 10 has a calibration interface 101 . The calibration interface 101 can be used to connect the measurement chamber 83 of the hydrogen meter 8 so that liquid alkali metal can enter the measurement chamber 83 of the hydrogen meter 8 .

氢气供应部11可以用于向液态碱金属回路10中供应含氢气体以形成包含含氢化合物的含氢碱金属液体。The hydrogen supply part 11 may be used to supply hydrogen-containing gas into the liquid alkali metal circuit 10 to form a hydrogen-containing alkali metal liquid containing a hydrogen-containing compound.

控制部12可以与氢计8电性连接,控制部12可以用于控制氢气的高真空系统85开启,以使进入测量腔83的液态碱金属中的氢及其他气体进入氢渗透结构84,并控制质谱仪87检测进入氢渗透结构84的气体组成成分,以及控制离子泵86检测进入氢渗透结构84的气体浓度。The control part 12 can be electrically connected to the hydrogen meter 8, and the control part 12 can be used to control the opening of the high vacuum system 85 of hydrogen, so that the hydrogen and other gases in the liquid alkali metal entering the measurement chamber 83 enter the hydrogen permeation structure 84, and The mass spectrometer 87 is controlled to detect the gas composition entering the hydrogen permeation structure 84, and the ion pump 86 is controlled to detect the gas concentration entering the hydrogen permeation structure 84.

处理部13可以与氢计8电性连接,处理部13可以用于根据液态碱金属回路10中氢的浓度以及质谱仪87检测的气体组成成分对离子泵86检测的气体浓度进行标定。The processing part 13 may be electrically connected to the hydrogen meter 8 , and the processing part 13 may be used to calibrate the gas concentration detected by the ion pump 86 according to the concentration of hydrogen in the liquid alkali metal circuit 10 and the gas composition detected by the mass spectrometer 87 .

本申请的实施例提供的标定装置,能够根据液态碱金属回路10中氢的浓度以及质谱仪87检测的气体组成成分对离子泵86检测的气体浓度进行标定,从而使得标定后的氢计8对氢浓度的测量结果更为准确可靠。The calibration device provided by the embodiment of the present application can calibrate the gas concentration detected by the ion pump 86 according to the concentration of hydrogen in the liquid alkali metal circuit 10 and the gas composition detected by the mass spectrometer 87 , so that the calibrated hydrogen meter 8 can accurately The measurement results of hydrogen concentration are more accurate and reliable.

在一些实施例中,处理部13还用于:根据质谱仪87检测的气体组成成分确定进入氢渗透结构84的气体中氢气所占比例;根据氢气所占比例和液态碱金属回路10中氢的浓度,对离子泵86检测的气体浓度进行标定。In some embodiments, the processing part 13 is also used to: determine the proportion of hydrogen in the gas entering the hydrogen permeation structure 84 based on the gas composition detected by the mass spectrometer 87 ; based on the proportion of hydrogen and the concentration of hydrogen in the liquid alkali metal circuit 10 concentration, calibrating the gas concentration detected by the ion pump 86.

在本申请的实施例中,对氢计8进行标定,实际上是对离子泵86检测的气体浓度进行标定。容易理解,离子泵86输出的数据为电流值,该电流值包含了氢和其他杂质成分共同电离的结果。本申请的实施例通过根据液态碱金属回路10中氢的浓度以及进入氢渗透结构84的气体中氢气所占比例对离子泵86检测的气体浓度进行标定,能够将离子泵86输出的电流值中由氢电离引起的部分与液态碱金属中氢的浓度进行对应,从而排除杂质的影响,使得标定后的氢计8的检测结果更加准确可靠。In the embodiment of the present application, the calibration of the hydrogen meter 8 actually involves the calibration of the gas concentration detected by the ion pump 86 . It is easy to understand that the data output by the ion pump 86 is a current value, and the current value includes the result of joint ionization of hydrogen and other impurity components. Embodiments of the present application calibrate the gas concentration detected by the ion pump 86 according to the concentration of hydrogen in the liquid alkali metal circuit 10 and the proportion of hydrogen in the gas entering the hydrogen permeation structure 84, so that the current value output by the ion pump 86 can be The part caused by hydrogen ionization corresponds to the concentration of hydrogen in the liquid alkali metal, thereby eliminating the influence of impurities, making the detection results of the calibrated hydrogen meter 8 more accurate and reliable.

例如,液态碱金属回路10中氢的浓度为A ppm/ml,质谱仪87检测的气体组成成分中氢气为B ppm,氧气为C ppm,氮气为D ppm,经计算确定进入氢渗透结构84的气体中氢气所占比例为B/(B+C+D)。若离子泵86检测的电流值为EμA,则离子泵86检测的电流值中有E*B/(B+C+D)μA是由氢气电离得到的。对离子泵86检测的气体浓度进行标定的结果为:电流值为E*B/(B+C+D)μA对应液态碱金属容器19中氢的浓度为A ppm/ml。For example, the concentration of hydrogen in the liquid alkali metal circuit 10 is A ppm/ml, and the gas composition detected by the mass spectrometer 87 is B ppm for hydrogen, C ppm for oxygen, and D ppm for nitrogen. It is determined through calculation that the concentration of hydrogen entering the hydrogen permeation structure 84 The proportion of hydrogen in the gas is B/(B+C+D). If the current value detected by the ion pump 86 is EμA, then E*B/(B+C+D)μA among the current values detected by the ion pump 86 is obtained by hydrogen ionization. The result of calibrating the gas concentration detected by the ion pump 86 is: the current value is E*B/(B+C+D)μA and the corresponding hydrogen concentration in the liquid alkali metal container 19 is A ppm/ml.

参见图2,本申请的实施例提供的标定装置还可以包括冷却部15和阻塞计14。冷却部15可以用于对液态碱金属回路10中的含氢碱金属液体进行冷却,以使含氢碱金属液体中的部分含氢化合物在降温后结晶析出。阻塞计14可以用于获得含氢碱金属液体中的含氢化合物结晶析出的结晶温度。利用阻塞计获得含氢碱金属液体中的含氢化合物结晶析出的结晶温度,是本领域技术人员所熟知的,在此不予赘述。Referring to FIG. 2 , the calibration device provided by the embodiment of the present application may also include a cooling part 15 and an obstruction meter 14 . The cooling unit 15 may be used to cool the hydrogen-containing alkali metal liquid in the liquid alkali metal circuit 10 so that part of the hydrogen-containing compounds in the hydrogen-containing alkali metal liquid crystallizes and precipitates after cooling. The obstruction meter 14 can be used to obtain the crystallization temperature at which the hydrogen-containing compound in the hydrogen-containing alkali metal liquid crystallizes. The use of a blocking meter to obtain the crystallization temperature at which a hydrogen-containing compound in a hydrogen-containing alkali metal liquid is crystallized is well known to those skilled in the art and will not be described in detail here.

处理部13还可以与阻塞计14相连。处理部13可以用于根据含氢化合物结晶析出的结晶温度确定含氢碱金属液体中含氢化合物的饱和溶解度值,从而根据含氢化合物的饱和溶解度值确定在结晶温度下液态碱金属回路10中氢的浓度。The processing unit 13 may also be connected to the obstruction meter 14 . The processing part 13 may be used to determine the saturated solubility value of the hydrogen-containing compound in the hydrogen-containing alkali metal liquid according to the crystallization temperature at which the hydrogen-containing compound crystallizes, thereby determining the saturated solubility value of the hydrogen-containing compound in the liquid alkali metal circuit 10 at the crystallization temperature. hydrogen concentration.

含氢化合物结晶析出的结晶温度与含氢碱金属液体中含氢化合物的饱和溶解度值之间存在对应的关系,当结晶温度确定时,其对应的含氢化合物的饱和溶解度值即为确定值(即能够确定对应结晶温度下的碱金属中含氢化合物的浓度),再根据含氢化合物的饱和溶解度,计算出含氢化合物中氢的浓度,即为在结晶温度下液态碱金属回路10中氢的浓度。There is a corresponding relationship between the crystallization temperature of the hydrogen-containing compound crystallized out and the saturated solubility value of the hydrogen-containing compound in the hydrogen-containing alkali metal liquid. When the crystallization temperature is determined, the corresponding saturated solubility value of the hydrogen-containing compound is the determined value ( That is, the concentration of the hydrogen-containing compound in the alkali metal at the corresponding crystallization temperature can be determined), and then according to the saturated solubility of the hydrogen-containing compound, the concentration of hydrogen in the hydrogen-containing compound can be calculated, which is the hydrogen in the liquid alkali metal circuit 10 at the crystallization temperature concentration.

在相关技术中,通过氢气供应部向液态碱金属回路10中供应含氢气体的含量来计算液态碱金属回路10中的氢的浓度。本申请的发明人发现,氢在注入液态碱金属回路10后,在液态碱金属中不会均匀溶解,从而导致计算的液态碱金属回路10中的氢的浓度误差较大,从而导致对氢计8的标定不准确。In the related art, the hydrogen concentration in the liquid alkali metal circuit 10 is calculated by supplying the hydrogen-containing gas content into the liquid alkali metal circuit 10 through a hydrogen supply unit. The inventor of the present application found that after hydrogen is injected into the liquid alkali metal circuit 10, it will not be uniformly dissolved in the liquid alkali metal, resulting in a large error in the calculated concentration of hydrogen in the liquid alkali metal circuit 10, resulting in a miscalculation of the hydrogen meter. The calibration of 8 is not accurate.

本申请实施例的标定装置,通过利用冷却部15对液态碱金属回路10中的含氢碱金属液体进行冷却,使含氢碱金属液体中的部分含氢化合物在降温后结晶析出,再利用阻塞计14获得含氢碱金属液体中的含氢化合物结晶析出的结晶温度,从而能够较为准确地获得液态碱金属回路10中氢的浓度,进而更准确地对氢计8进行标定。The calibration device of the embodiment of the present application uses the cooling part 15 to cool the hydrogen-containing alkali metal liquid in the liquid alkali metal circuit 10, so that part of the hydrogen-containing compounds in the hydrogen-containing alkali metal liquid crystallizes and precipitates after cooling, and then uses the obstruction The meter 14 obtains the crystallization temperature of the hydrogen-containing compound in the hydrogen-containing alkali metal liquid, so that the concentration of hydrogen in the liquid alkali metal circuit 10 can be obtained more accurately, and the hydrogen meter 8 can be calibrated more accurately.

在一些实施例中,冷却部15可以为钠回路中常用的冷阱。冷却部15可以设置于液态碱金属回路10上。阻塞计14可以设置于液态碱金属回路10上。In some embodiments, cooling section 15 may be a cold trap commonly used in sodium circuits. The cooling unit 15 may be provided on the liquid alkali metal circuit 10 . The obstruction meter 14 may be provided on the liquid alkali metal circuit 10 .

液态碱金属回路10中的管路可以包覆有加热件,用于对管路进行加热,使液态碱金属回路10内液态金属的温度可以基本保持不变,例如与液态碱金属在实际工作中的温度范围(如中子反应堆电站蒸发器出口温度)大致相同,例如300℃-350℃左右。当液态碱金属流经冷却部15后,冷却部15将含氢碱金属液体冷却至使含氢碱金属液体能够结晶的温度以下(如冷却至t1℃),从而准确地获得液态碱金属回路中氢的浓度。当液态碱金属从阻塞计14出来后,温度可以被阻塞计14和/或管路外包覆的加热件再次加热至初始温度。当液态碱金属流经氢计8的测量腔83后,测量腔83内的液态碱金属被氢计8的加热装置82加热至氢计8的检测温度范围(该温度范围例如可为450℃-500℃),利用质谱仪87检测进入氢渗透结构的气体组成成分,且利用离子泵86检测进入氢渗透结构的气体浓度,再根据液态碱金属回路中氢的浓度和质谱仪87检测的气体组成成分,对离子泵86检测的气体浓度进行标定。The pipelines in the liquid alkali metal circuit 10 can be covered with heating elements for heating the pipelines so that the temperature of the liquid metal in the liquid alkali metal circuit 10 can remain basically unchanged. For example, in actual work with liquid alkali metal The temperature range (such as the evaporator outlet temperature of a neutron reactor power station) is roughly the same, such as around 300℃-350℃. After the liquid alkali metal flows through the cooling part 15, the cooling part 15 cools the hydrogen-containing alkali metal liquid to a temperature below which the hydrogen-containing alkali metal liquid can crystallize (such as cooling to t1°C), thereby accurately obtaining the liquid alkali metal in the circuit. hydrogen concentration. After the liquid alkali metal comes out of the obstruction meter 14, the temperature can be heated to the initial temperature again by the obstruction meter 14 and/or the heating element wrapped around the pipeline. When the liquid alkali metal flows through the measurement chamber 83 of the hydrogen meter 8, the liquid alkali metal in the measurement chamber 83 is heated by the heating device 82 of the hydrogen meter 8 to the detection temperature range of the hydrogen meter 8 (the temperature range can be, for example, 450°C- 500°C), using the mass spectrometer 87 to detect the gas composition entering the hydrogen permeable structure, and using the ion pump 86 to detect the gas concentration entering the hydrogen permeable structure, and then based on the concentration of hydrogen in the liquid alkali metal circuit and the gas composition detected by the mass spectrometer 87 The gas concentration detected by the ion pump 86 is calibrated.

在进行下一次标定时,可以使冷却部15将含氢碱金属液体冷却至t2℃,t2℃低于t1℃,以将含氢碱金属液体再次冷却至使含氢碱金属液体能够结晶的温度以下,以再次准确地获得液态碱金属回路中氢当前的浓度。之后,按照上述步骤利用离子泵86检测进入氢渗透结构的气体浓度,再根据液态碱金属回路中氢的浓度和质谱仪87检测的气体组成成分,对离子泵86检测的气体浓度进行标定。When performing the next calibration, the cooling part 15 can be used to cool the hydrogen-containing alkali metal liquid to t2°C, and t2°C is lower than t1°C, so as to cool the hydrogen-containing alkali metal liquid again to a temperature that enables the hydrogen-containing alkali metal liquid to crystallize. below, to obtain again exactly the current concentration of hydrogen in the liquid alkali metal circuit. After that, the ion pump 86 is used to detect the gas concentration entering the hydrogen permeation structure according to the above steps, and then the gas concentration detected by the ion pump 86 is calibrated according to the concentration of hydrogen in the liquid alkali metal circuit and the gas composition detected by the mass spectrometer 87 .

参见图2,本申请的实施例提供的标定装置还可以包括缓冲罐16和惰性气体供应部17。缓冲罐16可以设置在液态碱金属回路10上。惰性气体供应部17用于向缓冲罐16中供应惰性气体,以稳定液态碱金属回路10中的压力。缓冲罐16能够补充和吸收试验设施中钠介质因热胀冷缩产生的体积变化,使试验设施运行压力稳定。Referring to FIG. 2 , the calibration device provided by the embodiment of the present application may also include a buffer tank 16 and an inert gas supply part 17 . The buffer tank 16 may be provided on the liquid alkali metal circuit 10 . The inert gas supply part 17 is used to supply inert gas into the buffer tank 16 to stabilize the pressure in the liquid alkali metal circuit 10 . The buffer tank 16 can supplement and absorb the volume changes of the sodium medium in the test facility due to thermal expansion and contraction, so as to stabilize the operating pressure of the test facility.

在一些实施例中,惰性气体供应部17通过气体管路171与缓冲罐16相连。气体管路171上设有气体阀门1711,用于控制气体管路171与缓冲罐16之间的通断。惰性气体供应部17可以为氩气瓶。In some embodiments, the inert gas supply 17 is connected to the buffer tank 16 through a gas line 171 . The gas pipeline 171 is provided with a gas valve 1711 for controlling the connection between the gas pipeline 171 and the buffer tank 16 . The inert gas supply part 17 may be an argon gas bottle.

参见图2,在一些实施例中,标定装置还可以包括液态碱金属容器19。液态碱金属容器19可以用于存储液态碱金属,以及可以用于向液态碱金属回路10供应液态碱金属。Referring to Figure 2, in some embodiments, the calibration device may also include a liquid alkali metal container 19. The liquid alkali metal container 19 may be used to store liquid alkali metal and may be used to supply liquid alkali metal to the liquid alkali metal circuit 10 .

在一些实施例中,标定装置还可以包括加热件(图中未示出),液态碱金属容器19内可以设置有测温件25,测温件25可以检测液态碱金属容器19中的温度,以便对加热件进行控温,从而保证液态碱金属容器19中的液态碱金属不会凝固。In some embodiments, the calibration device may also include a heating element (not shown in the figure), and a temperature measuring element 25 can be provided in the liquid alkali metal container 19, and the temperature measuring element 25 can detect the temperature in the liquid alkali metal container 19, In order to control the temperature of the heating element, it is ensured that the liquid alkali metal in the liquid alkali metal container 19 will not solidify.

惰性气体供应部17还可以通过气体管路172与液态碱金属容器19相连,以向液态碱金属容器19中供应惰性气体。气体管路172与气体管路171并联后与惰性气体供应部17连接。The inert gas supply part 17 can also be connected to the liquid alkali metal container 19 through a gas pipeline 172 to supply inert gas into the liquid alkali metal container 19 . The gas pipeline 172 is connected in parallel with the gas pipeline 171 and is connected to the inert gas supply part 17 .

气体管路172与液态碱金属容器19相接的管段上可以设有阀门1722,用于控制气体管路172与液态碱金属容器19之间的通断。The pipe section connecting the gas pipeline 172 and the liquid alkali metal container 19 may be provided with a valve 1722 for controlling the connection between the gas pipeline 172 and the liquid alkali metal container 19 .

气体管路171与气体管路172之间可以设有气体管路173,气体管路173上设有阀门1731,用于控制气体管路173的通断。气体管路173的作用是在标定结束后,使缓冲罐16与液态碱金属容器19气腔联通,便于将液态碱金属转移至液态碱金属容器19中。当液态碱金属为钠时,液态碱金属容器19为可以储钠罐。A gas pipeline 173 may be provided between the gas pipeline 171 and the gas pipeline 172. The gas pipeline 173 is provided with a valve 1731 for controlling the on/off of the gas pipeline 173. The function of the gas pipeline 173 is to connect the buffer tank 16 with the gas chamber of the liquid alkali metal container 19 after the calibration is completed, so as to facilitate the transfer of liquid alkali metal into the liquid alkali metal container 19 . When the liquid alkali metal is sodium, the liquid alkali metal container 19 is a sodium storage tank.

气体管路172位于上还可设置阀门1721,阀门1721位于气体管路173与气体管路171之间。The gas pipeline 172 may also be provided with a valve 1721 , and the valve 1721 is located between the gas pipeline 173 and the gas pipeline 171 .

在一些实施例中,标定装置还可以包括电磁泵18。电磁泵18可以用于驱动液态碱金属回路10中的液态碱金属流动。In some embodiments, the calibration device may also include an electromagnetic pump 18 . The electromagnetic pump 18 can be used to drive the flow of liquid alkali metal in the liquid alkali metal circuit 10 .

在一些实施例中,标定装置还可以包括真空部20。真空部20可以用于在向液态碱金属回路10供应液态碱金属之前,对液态碱金属回路10进行抽真空。In some embodiments, the calibration device may further include a vacuum part 20 . The vacuum part 20 may be used to evacuate the liquid alkali metal circuit 10 before supplying the liquid alkali metal to the liquid alkali metal circuit 10 .

真空部20可以通过气体管路172与液态碱金属容器19相连。真空部20与气体管路172之间可以设有真空阀门201,用于控制真空部20与气体管路172之间的通断。The vacuum part 20 may be connected to the liquid alkali metal container 19 through a gas pipeline 172 . A vacuum valve 201 may be provided between the vacuum part 20 and the gas pipeline 172 for controlling the connection between the vacuum part 20 and the gas pipeline 172 .

液态碱金属回路10包括第一管路102、第二管路103、第三管路104、第四管路105以及第五管路106。第一管路102和第二管路103通过第五管路106连接,第二管路103和第四管路105连接,第四管路105和第三管路104通过缓冲罐16连接。第一管路102和第二管路103还分别与液态碱金属容器19相连,以由液态碱金属容器19向液态碱金属回路10中供应液态碱金属。The liquid alkali metal circuit 10 includes a first pipeline 102 , a second pipeline 103 , a third pipeline 104 , a fourth pipeline 105 and a fifth pipeline 106 . The first pipeline 102 and the second pipeline 103 are connected through the fifth pipeline 106 , the second pipeline 103 and the fourth pipeline 105 are connected, and the fourth pipeline 105 and the third pipeline 104 are connected through the buffer tank 16 . The first pipeline 102 and the second pipeline 103 are also connected to the liquid alkali metal container 19 respectively, so that the liquid alkali metal container 19 supplies liquid alkali metal to the liquid alkali metal circuit 10 .

第一管路102上设有第一管路阀门1021,第二管路103上设有第二管路阀门1031,第五管路106上设有第五管路阀门1061。当第五管路阀门1061关闭,第一管路阀门1021和第二管路阀门1031打开时,第一管路102和第二管路103与液态碱金属容器19相连;当第五管路阀门1061打开,第一管路阀门1021和第二管路阀门1031关闭时,第一管路102和第二管路103与第五管路106相连。The first pipeline 102 is provided with a first pipeline valve 1021, the second pipeline 103 is provided with a second pipeline valve 1031, and the fifth pipeline 106 is provided with a fifth pipeline valve 1061. When the fifth pipeline valve 1061 is closed and the first pipeline valve 1021 and the second pipeline valve 1031 are opened, the first pipeline 102 and the second pipeline 103 are connected to the liquid alkali metal container 19; when the fifth pipeline valve 1061 is opened and the first pipeline valve 1021 and the second pipeline valve 1031 are closed, the first pipeline 102 and the second pipeline 103 are connected to the fifth pipeline 106 .

第一管路102上还可以设有第一管路电动阀门1022以及第一管路流量计1023。The first pipeline 102 may also be provided with a first pipeline electric valve 1022 and a first pipeline flow meter 1023.

参见图2,在一些实施例中,标定装置还可以包括空冷部,用于带走标定装置中多余热量。空冷器22通过空冷阀门221与第四管路105连接。第四管路105还设有第四管路阀门1051,第四管路阀门1051与空冷阀门221共同用于控制第四管路105中的液态金属是否流经空冷部。空冷部可以包括冷却风机21和空冷器22,用于带走液态碱金属回路10中多余的热量。回路运行过程中,电磁泵18会产生热量,需要空冷部将热量带走,否则回路温度将持续升高。通过设置空冷部和缓冲罐16,可以有效地控制回路温度、压力和流量,保障标定装置长期稳定运行。Referring to Figure 2, in some embodiments, the calibration device may also include an air cooling part for taking away excess heat from the calibration device. The air cooler 22 is connected to the fourth pipeline 105 through an air cooling valve 221. The fourth pipeline 105 is also provided with a fourth pipeline valve 1051. The fourth pipeline valve 1051 and the air-cooling valve 221 are used together to control whether the liquid metal in the fourth pipeline 105 flows through the air-cooling part. The air cooling section may include a cooling fan 21 and an air cooler 22 for taking away excess heat in the liquid alkali metal circuit 10 . During the operation of the circuit, the electromagnetic pump 18 will generate heat, which needs to be taken away by the air cooling unit, otherwise the circuit temperature will continue to rise. By setting up the air cooling section and the buffer tank 16, the loop temperature, pressure and flow can be effectively controlled to ensure long-term stable operation of the calibration device.

参见图2,在一些实施例中,标定接口101和电磁泵18设置于第三管路104上。电磁泵18的进出口处分别设有两个仪表31,用于测量电磁泵18的进出口处的压力。仪表31可以为压力表,也可以为差压变送器,主要用于监测电磁泵18进出口压力。由于电磁泵18的泵沟为系统的薄弱环节,监测电磁泵18进出口压力,能够保护电磁泵18和系统其他设备管道不会由于超压而被破坏;此外,根据电磁泵18的压差可以通过变频器调节电磁泵功率,对系统流量进行粗调节,便于运行时系统流量调节控制。Referring to Figure 2, in some embodiments, the calibration interface 101 and the electromagnetic pump 18 are disposed on the third pipeline 104. Two instruments 31 are respectively provided at the inlet and outlet of the electromagnetic pump 18 for measuring the pressure at the inlet and outlet of the electromagnetic pump 18 . The instrument 31 can be a pressure gauge or a differential pressure transmitter, and is mainly used to monitor the inlet and outlet pressure of the electromagnetic pump 18 . Since the pump groove of the electromagnetic pump 18 is the weak link of the system, monitoring the inlet and outlet pressure of the electromagnetic pump 18 can protect the electromagnetic pump 18 and other equipment pipelines in the system from being damaged due to overpressure; in addition, according to the pressure difference of the electromagnetic pump 18, The power of the electromagnetic pump is adjusted through the frequency converter, and the system flow is roughly adjusted to facilitate the system flow adjustment and control during operation.

阻塞计14和冷却部15可以设置于第二管路103上。The obstruction gauge 14 and the cooling part 15 may be disposed on the second pipeline 103 .

第二管路103还设有第二管路阀门1032、第二管路阀门1033以及第二管路流量计1034。其中,第二管路阀门1031接近液态碱金属容器19设置。第二管路阀门1032设置于第二管路阀门1031与第二管路阀门1033之间。阻塞计14通过阻塞管路与第二管路阀门1033所在的管段并联设置,阻塞管路位于阻塞计14的进出口两侧分别设有阻塞计阀门142和阻塞计阀门141。The second pipeline 103 is also provided with a second pipeline valve 1032, a second pipeline valve 1033 and a second pipeline flow meter 1034. Among them, the second pipeline valve 1031 is disposed close to the liquid alkali metal container 19 . The second pipeline valve 1032 is provided between the second pipeline valve 1031 and the second pipeline valve 1033 . The obstruction meter 14 is arranged in parallel with the pipe section where the second pipeline valve 1033 is located through the obstruction pipeline. The obstruction pipeline is provided with obstruction meter valve 142 and obstruction meter valve 141 on both sides of the inlet and outlet of the obstruction meter 14 respectively.

冷却部15通过冷却管路与第二管路阀门1032所在的管段并联设置,冷却管路位于冷却部15的进出口两侧分别设有冷却阀门152和冷却阀门151。The cooling section 15 is provided in parallel with the pipe section where the second pipeline valve 1032 is located through a cooling pipeline. The cooling pipeline is respectively provided with a cooling valve 152 and a cooling valve 151 on both sides of the inlet and outlet of the cooling section 15 .

在标定之前,电磁泵18驱动液态碱金属从液态碱金属容器19中流入液态碱金属回路10中。当需要对液态碱金属进行净化时,可以使第二管路103中的液态碱金属流经冷却部15,进而利用冷却部15对液态碱金属回路10和液态碱金属容器19中的含氢碱金属液体进行冷却,使含氢碱金属液体中的部分含氢化合物在降温后结晶析出,实现对液态碱金属的净化除杂。Before calibration, the electromagnetic pump 18 drives the liquid alkali metal to flow from the liquid alkali metal container 19 into the liquid alkali metal circuit 10 . When the liquid alkali metal needs to be purified, the liquid alkali metal in the second pipeline 103 can be made to flow through the cooling part 15, and then the cooling part 15 can be used to purify the hydrogen-containing alkali in the liquid alkali metal circuit 10 and the liquid alkali metal container 19. The metal liquid is cooled, so that part of the hydrogen-containing compounds in the hydrogen-containing alkali metal liquid crystallizes and precipitates after cooling, thereby purifying and removing impurities from the liquid alkali metal.

在标定过程中,电磁泵18驱动液态碱金属在液态碱金属回路10中循环流动。具体地,液态碱金属从第一管路102中流出后流入第二管路103中,并依次进入冷却部15和阻塞计14,之后进入第四管路105中,进入缓冲罐16缓冲后进入第三管路104,在流经电磁泵18后返回第一管路102。During the calibration process, the electromagnetic pump 18 drives the liquid alkali metal to circulate in the liquid alkali metal circuit 10 . Specifically, the liquid alkali metal flows out of the first pipeline 102 and then flows into the second pipeline 103, and sequentially enters the cooling part 15 and the obstruction meter 14, and then enters the fourth pipeline 105, and enters the buffer tank 16 for buffering. The third pipeline 104 returns to the first pipeline 102 after flowing through the electromagnetic pump 18 .

气体管路171可以在缓冲罐16的上部与缓冲罐16连通,第四管路105在缓冲罐16的下部与缓冲罐16连通,第三管路104在缓冲罐16的底部与缓冲罐16连通。The gas pipeline 171 can be connected with the buffer tank 16 at the upper part of the buffer tank 16, the fourth pipeline 105 can be connected with the buffer tank 16 at the lower part of the buffer tank 16, and the third pipeline 104 can be connected with the buffer tank 16 at the bottom of the buffer tank 16. .

在一些实施例中,氢气供应部11提供的含氢气体可以是氢气和氩气的混合气体。氢气供应部11可以通过氢气管路111与液态碱金属回路10连接。氢气管路111具有氢气接口1111,氢气接口1111在电磁泵18与缓冲罐16之间与第三管路104连接。当标定氢计8时,氢气供应部11中的含氢气体流经氢气管路111由氢气接口1111进入第三管路104,注入第三管路104的液态碱金属中,形成包含含氢化合物的含氢碱金属液体。在这样的实施例,相当于氢气在缓冲罐16的下游进入液态碱金属回路10中,从而,有利于避免进入第三管路104的氢气在未充分溶解于液态碱金属中之前,扩散进入缓冲罐16内。In some embodiments, the hydrogen-containing gas provided by the hydrogen supply part 11 may be a mixed gas of hydrogen and argon. The hydrogen supply part 11 can be connected to the liquid alkali metal circuit 10 through a hydrogen pipeline 111 . The hydrogen pipeline 111 has a hydrogen interface 1111 , and the hydrogen interface 1111 is connected to the third pipeline 104 between the electromagnetic pump 18 and the buffer tank 16 . When calibrating the hydrogen meter 8, the hydrogen-containing gas in the hydrogen supply part 11 flows through the hydrogen pipeline 111 and enters the third pipeline 104 through the hydrogen interface 1111, and is injected into the liquid alkali metal in the third pipeline 104 to form a hydrogen-containing compound. Hydrogen-containing alkali metal liquid. In such an embodiment, it is equivalent to hydrogen entering the liquid alkali metal circuit 10 downstream of the buffer tank 16, thereby helping to avoid the hydrogen entering the third pipeline 104 from diffusing into the buffer before being fully dissolved in the liquid alkali metal. Inside the tank 16.

本申请实施例还提供一种氢计的标定方法。The embodiment of the present application also provides a calibration method of a hydrogen meter.

如图3所示,其示出本申请的实施例的氢计的标定方法的流程示意图,氢计可以为上述提及的氢计8。标定方法可以包括下面的步骤S31至步骤S37。As shown in FIG. 3 , it shows a schematic flow chart of the calibration method of a hydrogen meter according to an embodiment of the present application. The hydrogen meter may be the hydrogen meter 8 mentioned above. The calibration method may include the following steps S31 to S37.

步骤S31:提供用于供液态碱金属流动的液态碱金属回路。Step S31: Provide a liquid alkali metal circuit for flowing the liquid alkali metal.

步骤S32:向液态碱金属回路中注入含氢气体,以形成包含含氢化合物的含氢碱金属液体。Step S32: Inject hydrogen-containing gas into the liquid alkali metal circuit to form a hydrogen-containing alkali metal liquid containing a hydrogen-containing compound.

步骤S33:确定液态碱金属回路中氢的浓度。Step S33: Determine the concentration of hydrogen in the liquid alkali metal circuit.

步骤S34:利用高真空系统85使含氢碱金属液体中的氢及其他气体渗透进入氢渗透结构84内。Step S34: Use the high vacuum system 85 to permeate hydrogen and other gases in the hydrogen-containing alkali metal liquid into the hydrogen permeation structure 84.

步骤S35:利用质谱仪87检测进入氢渗透结构的气体组成成分。Step S35: Use the mass spectrometer 87 to detect the gas composition entering the hydrogen permeation structure.

步骤S36:利用离子泵86检测进入氢渗透结构的气体浓度。Step S36: Use the ion pump 86 to detect the gas concentration entering the hydrogen permeation structure.

步骤S37:根据液态碱金属回路中氢的浓度和质谱仪87检测的气体组成成分,对离子泵86检测的气体浓度进行标定。Step S37: Calibrate the gas concentration detected by the ion pump 86 based on the concentration of hydrogen in the liquid alkali metal circuit and the gas composition detected by the mass spectrometer 87 .

本申请的实施例提供的标定方法,能够根据液态碱金属回路中氢的浓度以及质谱仪87检测的气体组成成分对离子泵86检测的气体浓度进行标定,从而使得标定后的氢计8对氢浓度的测量结果更为准确可靠。The calibration method provided by the embodiment of the present application can calibrate the gas concentration detected by the ion pump 86 according to the concentration of hydrogen in the liquid alkali metal circuit and the gas composition detected by the mass spectrometer 87 , so that the calibrated hydrogen meter 8 can accurately measure the hydrogen The concentration measurement results are more accurate and reliable.

在一些实施例中,步骤S31中的液态碱金属可以是液态钠。步骤S32中的含氢化合物可以是氢氧化钠。In some embodiments, the liquid alkali metal in step S31 may be liquid sodium. The hydrogen-containing compound in step S32 may be sodium hydroxide.

在一些实施例中,步骤S33确定液态碱金属回路中氢的浓度的步骤可以包括:对液态碱金属回路中的含氢碱金属液体进行冷却,以使含氢碱金属液体中的部分含氢化合物在降温后结晶析出;获得含氢碱金属液体中的含氢化合物结晶析出的结晶温度,根据结晶温度确定含氢碱金属液体中含氢化合物的饱和溶解度值,根据含氢化合物的饱和溶解度值确定在结晶温度下液态碱金属回路中氢的浓度。In some embodiments, step S33 of determining the concentration of hydrogen in the liquid alkali metal circuit may include: cooling the hydrogen-containing alkali metal liquid in the liquid alkali metal circuit so that part of the hydrogen-containing compounds in the hydrogen-containing alkali metal liquid Crystallization and precipitation after cooling; obtain the crystallization temperature at which the hydrogen-containing compound in the hydrogen-containing alkali metal liquid crystallizes and precipitates, determine the saturated solubility value of the hydrogen-containing compound in the hydrogen-containing alkali metal liquid according to the crystallization temperature, and determine it according to the saturated solubility value of the hydrogen-containing compound. The concentration of hydrogen in the liquid alkali metal circuit at the crystallization temperature.

含氢化合物结晶析出的结晶温度与含氢碱金属液体中含氢化合物的饱和溶解度值之间存在对应的关系,当结晶温度确定时,其对应的含氢化合物的饱和溶解度值即为确定值(即能够确定对应结晶温度下的碱金属中含氢化合物的浓度),再根据含氢化合物的饱和溶解度,计算出含氢化合物中氢的浓度,即为在结晶温度下液态碱金属回路中氢的浓度。There is a corresponding relationship between the crystallization temperature of the hydrogen-containing compound crystallized out and the saturated solubility value of the hydrogen-containing compound in the hydrogen-containing alkali metal liquid. When the crystallization temperature is determined, the corresponding saturated solubility value of the hydrogen-containing compound is the determined value ( That is, the concentration of the hydrogen-containing compound in the alkali metal at the corresponding crystallization temperature can be determined), and then based on the saturated solubility of the hydrogen-containing compound, the concentration of hydrogen in the hydrogen-containing compound can be calculated, which is the concentration of hydrogen in the liquid alkali metal circuit at the crystallization temperature. concentration.

在相关技术中,通过氢气供应部向液态碱金属回路中供应含氢气体的含量来计算液态碱金属回路中的氢的浓度。本申请的发明人发现,氢在注入液态碱金属回路后,在液态碱金属中不会均匀溶解,从而导致计算的碱金属回路中的氢的浓度误差较大,从而导致对氢计8的标定不准确。In the related art, the concentration of hydrogen in the liquid alkali metal circuit is calculated by supplying the hydrogen-containing gas content into the liquid alkali metal circuit through a hydrogen supply unit. The inventor of the present application found that after hydrogen is injected into the liquid alkali metal circuit, it will not be uniformly dissolved in the liquid alkali metal, resulting in a large error in the calculated concentration of hydrogen in the alkali metal circuit, which leads to the calibration of the hydrogen meter 8 Inaccurate.

本申请实施例的标定方法,通过对液态碱金属回路10中的含氢碱金属液体进行冷却,以使含氢碱金属液体中的部分含氢化合物在降温后结晶析出,再获得含氢碱金属液体中的含氢化合物结晶析出的结晶温度,从而能够较为准确地获得液态碱金属回路中氢的浓度,进而更准确地对氢计8进行标定。The calibration method of the embodiment of the present application cools the hydrogen-containing alkali metal liquid in the liquid alkali metal circuit 10 so that part of the hydrogen-containing compounds in the hydrogen-containing alkali metal liquid crystallizes and precipitates after cooling, and then the hydrogen-containing alkali metal is obtained. The crystallization temperature of the hydrogen-containing compound in the liquid crystallizes out, so that the concentration of hydrogen in the liquid alkali metal circuit can be obtained more accurately, and the hydrogen meter 8 can be calibrated more accurately.

本申请实施例本质上是利用含氢杂质在碱金属中饱和溶解度来对氢计8进行标定。具体地,本申请的实施例中通过向液态碱金属中注入含氢气体,形成包含含氢化合物的含氢碱金属液体,然后通过降温使含氢杂质析出,这样液态碱金属中的氢仅为饱和溶解的氢,从而可以排除氢析出或溶解不均匀的影响,从而能够较为准确地获得液态碱金属回路中氢的浓度。The embodiment of the present application essentially uses the saturated solubility of hydrogen-containing impurities in alkali metals to calibrate the hydrogen meter 8 . Specifically, in the embodiments of the present application, hydrogen-containing gas is injected into the liquid alkali metal to form a hydrogen-containing alkali metal liquid containing hydrogen-containing compounds, and then the hydrogen-containing impurities are precipitated by cooling, so that the hydrogen in the liquid alkali metal is only Saturating dissolved hydrogen can eliminate the influence of hydrogen precipitation or uneven dissolution, so that the concentration of hydrogen in the liquid alkali metal circuit can be obtained more accurately.

容易理解,饱和溶解度和温度、压力有关系,试验时,可以获得液态碱金属的温度和压力,确定其利用饱和溶解度。It is easy to understand that saturated solubility is related to temperature and pressure. During the test, the temperature and pressure of the liquid alkali metal can be obtained to determine its saturated solubility.

在一些实施例中,在确定在结晶温度下液态碱金属回路中氢的浓度之后,标定方法可以包括下面的步骤:在结晶温度下,利用质谱仪87检测进入氢渗透结构84的气体组成成分,利用离子泵86检测进入氢渗透结构84的气体浓度;根据在结晶温度下液态碱金属回路中氢的浓度和在结晶温度下质谱仪87检测的气体组成成分,对在结晶温度下离子泵86检测的气体浓度进行标定,以获得氢计8在结晶温度下的标定结果。In some embodiments, after determining the concentration of hydrogen in the liquid alkali metal circuit at the crystallization temperature, the calibration method may include the following steps: using a mass spectrometer 87 to detect the gas composition entering the hydrogen permeation structure 84 at the crystallization temperature, The ion pump 86 is used to detect the gas concentration entering the hydrogen permeability structure 84; based on the concentration of hydrogen in the liquid alkali metal circuit at the crystallization temperature and the gas composition detected by the mass spectrometer 87 at the crystallization temperature, the ion pump 86 detects the gas concentration at the crystallization temperature. The gas concentration is calibrated to obtain the calibration result of the hydrogen meter 8 at the crystallization temperature.

在一些实施例中,确定液态碱金属回路10中氢的浓度时,可以利用冷却部15对液态碱金属回路10中的含氢碱金属液体进行降温;可以利用阻塞计14获得含氢碱金属液体中的含氢化合物结晶析出的结晶温度。In some embodiments, when determining the concentration of hydrogen in the liquid alkali metal circuit 10, the cooling unit 15 can be used to cool down the hydrogen-containing alkali metal liquid in the liquid alkali metal circuit 10; the obstruction meter 14 can be used to obtain the hydrogen-containing alkali metal liquid. The crystallization temperature at which hydrogen-containing compounds crystallize out.

在一些实施例中,在根据含氢化合物的饱和溶解度值确定在结晶温度下液态碱金属回路中氢的浓度之后,标定方法还可以包括下面的步骤:以预设温度梯度对液态碱金属回路中的含氢碱金属液体进行降温,以获得含氢碱金属液体中含氢化合物在不同温度下对应的多个不同饱和溶解度值;根据多个不同饱和溶解度值确定液态碱金属回路中的氢在不同温度下的浓度;在含氢碱金属液体的不同温度下,分别利用质谱仪87检测进入氢渗透结构84的气体组成成分,利用离子泵86检测进入氢渗透结构84的气体浓度;根据液态碱金属回路中氢的浓度和质谱仪87检测的气体组成成分,对离子泵86检测的气体浓度进行标定,以获得氢计8在不同温度下的标定结果。In some embodiments, after determining the concentration of hydrogen in the liquid alkali metal circuit at the crystallization temperature based on the saturated solubility value of the hydrogen-containing compound, the calibration method may further include the following step: measuring the liquid alkali metal circuit with a preset temperature gradient. Cool down the hydrogen-containing alkali metal liquid to obtain multiple different saturated solubility values corresponding to the hydrogen-containing compounds in the hydrogen-containing alkali metal liquid at different temperatures; determine the hydrogen in the liquid alkali metal circuit at different temperatures based on multiple different saturated solubility values The concentration at the temperature; at different temperatures of the hydrogen-containing alkali metal liquid, use the mass spectrometer 87 to detect the gas composition entering the hydrogen permeation structure 84, and use the ion pump 86 to detect the gas concentration entering the hydrogen permeation structure 84; according to the liquid alkali metal The concentration of hydrogen in the loop and the gas composition detected by the mass spectrometer 87 are calibrated to the gas concentration detected by the ion pump 86 to obtain the calibration results of the hydrogen meter 8 at different temperatures.

在本申请的实施例中,预设温度梯度例如可以为0.5℃-5℃。例如,预设温度梯度例如可以为1℃或2℃。In the embodiment of the present application, the preset temperature gradient may be, for example, 0.5°C-5°C. For example, the preset temperature gradient may be 1°C or 2°C.

在当前温度t℃下对氢计进行标定之后,可以利用冷却部对液态碱金属回路中的液态碱金属进行冷却,使液态碱金属的温度下降1℃左右,此时,液态碱金属中的含氢化合物进一步结晶。利用阻塞计获得当前的结晶温度,并进一步获得当前的结晶温度对应的含氢化合物的化合溶解度。After calibrating the hydrogen meter at the current temperature t°C, the cooling part can be used to cool the liquid alkali metal in the liquid alkali metal circuit, so that the temperature of the liquid alkali metal drops by about 1°C. At this time, the content of the liquid alkali metal The hydrogen compound crystallizes further. Use an obstruction meter to obtain the current crystallization temperature, and further obtain the chemical solubility of the hydrogen-containing compound corresponding to the current crystallization temperature.

在本申请实施例中,可以仅在标定开始时,向液态碱金属回路中注入一次氢即可,在之后的标定过程中,通过使液态碱金属降温,使液态碱金属中含氢化合物的溶解度不断降低,直至达到饱和状态后开始结晶析出,此时,能够通过阻塞计过得结晶温度,对氢计8进行首次标定,之后,通过以一定的温度梯度对液态碱金属进行冷却,再每一次降温后,均可利用阻塞计获得相应的结晶温度,从而对氢计8在相应的结晶温度下进行标定。In the embodiment of the present application, hydrogen can be injected into the liquid alkali metal circuit once only at the beginning of the calibration. In the subsequent calibration process, the temperature of the liquid alkali metal is cooled to increase the solubility of the hydrogen-containing compound in the liquid alkali metal. Continue to decrease until it reaches a saturated state and then crystallization begins. At this time, the crystallization temperature can be obtained through a blocking meter, and the hydrogen meter 8 can be calibrated for the first time. After that, the liquid alkali metal is cooled with a certain temperature gradient, and then each time After cooling down, the obstruction meter can be used to obtain the corresponding crystallization temperature, so that the hydrogen meter 8 can be calibrated at the corresponding crystallization temperature.

容易理解,液态碱金属回路内液态金属的温度可以基本保持不变,例如与液态碱金属在实际工作中的温度范围(如中子反应堆电站蒸发器出口温度)大致相同。当利用冷却部将液态碱金属的温度降低至结晶的温度以下后,当阻塞计获得当前的结晶温度后,可再次将液态碱金属回路内液态金属的温度加热至初始温度,以使处于初始温度的液态碱金属流入氢计8的测量腔83。测量腔83内的液态碱金属被氢计8的加热装置82加热至氢计8的检测温度范围(该温度范围例如可为450℃-500℃),利用质谱仪87检测进入氢渗透结构的气体组成成分,且利用离子泵86检测进入氢渗透结构的气体浓度,再根据液态碱金属回路中氢的浓度和质谱仪87检测的气体组成成分,对离子泵86检测的气体浓度进行标定。It is easy to understand that the temperature of the liquid metal in the liquid alkali metal circuit can remain basically unchanged, for example, approximately the same as the temperature range of the liquid alkali metal in actual operation (such as the evaporator outlet temperature of a neutron reactor power station). After the cooling part is used to reduce the temperature of the liquid alkali metal to below the crystallization temperature, and after the obstruction meter obtains the current crystallization temperature, the temperature of the liquid metal in the liquid alkali metal circuit can be heated to the initial temperature again, so that it is at the initial temperature The liquid alkali metal flows into the measuring chamber 83 of the hydrogen meter 8 . The liquid alkali metal in the measurement chamber 83 is heated by the heating device 82 of the hydrogen meter 8 to the detection temperature range of the hydrogen meter 8 (the temperature range can be, for example, 450°C-500°C), and the mass spectrometer 87 is used to detect the gas entering the hydrogen permeation structure. The ion pump 86 is used to detect the gas concentration entering the hydrogen permeation structure, and then the gas concentration detected by the ion pump 86 is calibrated according to the concentration of hydrogen in the liquid alkali metal circuit and the gas composition detected by the mass spectrometer 87 .

容易理解,在利用氢计8进行测量时,测量腔83内的液态碱金属由于被加热而温度升高,但这基本不会影响液态碱金属回路内液态金属的温度。It is easy to understand that when the hydrogen meter 8 is used for measurement, the temperature of the liquid alkali metal in the measurement chamber 83 increases due to being heated, but this basically does not affect the temperature of the liquid metal in the liquid alkali metal circuit.

在进行下一次标定时,可以使冷却部15在上一次冷却的基础上将含氢碱金属液体进行再次冷却。例如,上一次冷却的温度为t1℃,则本次冷却的温度为t2℃(t2<t1),下一次冷却的温度为温度更低的t3℃(t3<t2)。During the next calibration, the cooling unit 15 can be used to cool the hydrogen-containing alkali metal liquid again based on the previous cooling. For example, if the temperature of the last cooling was t1°C, the temperature of this cooling is t2°C (t2<t1), and the temperature of the next cooling is t3°C (t3<t2), which is even lower.

在本申请实施例中,通过降低温度使含氢组分杂质降温析出,逐级降低液态碱金属中含氢组分杂质的含量。这种氢浓度由高到低的氢计标定方法可以使标定精度更高,使标定后的氢计的测量结果更准确。In the embodiment of the present application, by lowering the temperature, the hydrogen-containing component impurities are cooled and precipitated, and the content of the hydrogen-containing component impurities in the liquid alkali metal is gradually reduced. This method of calibrating the hydrogen meter from high to low hydrogen concentration can make the calibration more accurate and make the measurement results of the calibrated hydrogen meter more accurate.

在一些实施例中,根据液态碱金属回路中氢的浓度和质谱仪87检测的气体组成成分对离子泵86检测的气体浓度进行标定可以包括:根据质谱仪87检测的气体组成成分确定进入氢渗透结构84的气体中氢气所占比例;根据氢气所占比例和液态碱金属回路中氢的浓度,对离子泵86检测的气体浓度进行标定。In some embodiments, calibrating the gas concentration detected by the ion pump 86 according to the concentration of hydrogen in the liquid alkali metal circuit and the gas composition detected by the mass spectrometer 87 may include: determining the hydrogen permeability according to the gas composition detected by the mass spectrometer 87 The proportion of hydrogen in the gas of structure 84; according to the proportion of hydrogen and the concentration of hydrogen in the liquid alkali metal circuit, the gas concentration detected by the ion pump 86 is calibrated.

在一些实施例中,本申请实施例的标定方法中提供的液态碱金属回路可以为本申请任一的标定装置中的液态碱金属回路10。在一些实施例中,本申请实施例的标定方法可以利用本申请任一实施例的标定装置实现。In some embodiments, the liquid alkali metal circuit provided in the calibration method of the embodiment of the present application can be the liquid alkali metal circuit 10 in any calibration device of the present application. In some embodiments, the calibration method of the embodiment of the present application can be implemented using the calibration device of any embodiment of the present application.

下面结合图2和具体实施例详细说明本申请的标定方法。The calibration method of this application will be described in detail below with reference to Figure 2 and specific embodiments.

打开液态碱金属回路10的各个阀门,打开真空阀门201和阀门1722,利用真空泵20将液态碱金属回路10抽至真空环境;打开气体阀门1711和阀门1721,通过氩气瓶17向液态碱金属回路10中供应惰性气体,重复上述操作3-4次,以使液态碱金属回路10中的气体排净;启动加热件对液态碱金属回路10进行加热。在一些实施例中,液态碱金属回路10的设计温度可以为350℃,模拟快中子反应堆电站蒸发器出口温度。Open each valve of the liquid alkali metal circuit 10, open the vacuum valve 201 and the valve 1722, and use the vacuum pump 20 to pump the liquid alkali metal circuit 10 to a vacuum environment; open the gas valve 1711 and the valve 1721, and pump the liquid alkali metal circuit to the liquid alkali metal circuit through the argon cylinder 17. Supply inert gas in 10 and repeat the above operation 3-4 times to drain the gas in the liquid alkali metal circuit 10; start the heating element to heat the liquid alkali metal circuit 10. In some embodiments, the design temperature of the liquid alkali metal circuit 10 may be 350°C, simulating the evaporator outlet temperature of a fast neutron reactor power plant.

关闭气体阀门1711和真空阀门201,通过惰性气体供应部17向液态碱金属容器19中充入惰性气体,使液态碱金属容器19内部气压增大。The gas valve 1711 and the vacuum valve 201 are closed, and the inert gas is filled into the liquid alkali metal container 19 through the inert gas supply part 17 to increase the internal pressure of the liquid alkali metal container 19 .

打开第二管路阀门1031、第二管路阀门1032、第二管路阀门1033、第四管路阀门1051、第一管路阀门1021、第一管路电动阀门1022(关闭液态碱金属回路10的其他阀门),液态碱金属容器19中的液态碱金属流出至第二管路103中,液态碱金属沿第二管路103、第四管路105流入缓冲罐16中,当缓冲罐16中液态碱金属的液位到达缓冲罐16的2/3处时,停止增压;启动电磁泵18使液态碱金属沿第三管路104流至标定接口101处,使液态碱金属能够通过标定接口101流入待标定氢计8的测量腔83内,并流经第一管路102返回液态碱金属容器19。液态碱金属回路10的管径可以为DN300,和快中子反应堆电站蒸发器出口处管径相同;液态碱金属在回路中的流速可以为0.8m/s。Open the second pipeline valve 1031, the second pipeline valve 1032, the second pipeline valve 1033, the fourth pipeline valve 1051, the first pipeline valve 1021, and the first pipeline electric valve 1022 (close the liquid alkali metal circuit 10 other valves), the liquid alkali metal in the liquid alkali metal container 19 flows out to the second pipeline 103, and the liquid alkali metal flows into the buffer tank 16 along the second pipeline 103 and the fourth pipeline 105. When the buffer tank 16 When the liquid level of the liquid alkali metal reaches 2/3 of the buffer tank 16, stop pressurizing; start the electromagnetic pump 18 to make the liquid alkali metal flow to the calibration interface 101 along the third pipeline 104, so that the liquid alkali metal can pass through the calibration interface 101 flows into the measurement chamber 83 of the hydrogen meter 8 to be calibrated, and flows back to the liquid alkali metal container 19 through the first pipeline 102 . The pipe diameter of the liquid alkali metal loop 10 can be DN300, which is the same as the pipe diameter at the evaporator outlet of the fast neutron reactor power station; the flow rate of the liquid alkali metal in the loop can be 0.8m/s.

打开第五管路阀门1061,关闭第一管路阀门1021和第二管路阀门1031,使液态碱金属在液态碱金属回路10内循环流动。Open the fifth pipeline valve 1061, close the first pipeline valve 1021 and the second pipeline valve 1031, so that the liquid alkali metal circulates in the liquid alkali metal circuit 10.

通过氢气供应部11和氢气管路111向第三管路104中注入一定量的含氢气体。打开冷却阀门151和冷却阀门152,打开阻塞计阀门141和阻塞计阀门142,关闭第二管路阀门1032,第二管路阀门1033,启动冷阱15对第二管路103中的含氢碱金属液体进行降温,以使碱金属中的含氢化合物结晶析出;利用阻塞计14获得含氢碱金属液体中的含氢化合物结晶析出的结晶温度,以获得含氢碱金属液体中含氢化合物在当前温度对应的饱和溶解度值。根据当前温度对应的饱和溶解度值确定液态碱金属回路10中的氢在当前温度下的浓度。A certain amount of hydrogen-containing gas is injected into the third pipeline 104 through the hydrogen supply part 11 and the hydrogen pipeline 111 . Open the cooling valve 151 and the cooling valve 152, open the obstruction meter valve 141 and the obstruction meter valve 142, close the second pipeline valve 1032, the second pipeline valve 1033, start the cold trap 15 to treat the hydrogen-containing alkali in the second pipeline 103 The metal liquid is cooled so that the hydrogen-containing compound in the alkali metal crystallizes out; the obstruction meter 14 is used to obtain the crystallization temperature at which the hydrogen-containing compound in the hydrogen-containing alkali metal liquid crystallizes out, so as to obtain the temperature of the hydrogen-containing compound in the hydrogen-containing alkali metal liquid The saturated solubility value corresponding to the current temperature. The concentration of hydrogen in the liquid alkali metal circuit 10 at the current temperature is determined according to the saturated solubility value corresponding to the current temperature.

使氢计8正常稳定运行,进入测量状态,氢计8正常运行时,预设镍管温度可以为475℃,电磁驱动设备81的频率可以为20Hz,氢计设计压力可以为1.5MPa。Make the hydrogen meter 8 operate normally and stably and enter the measurement state. When the hydrogen meter 8 is operating normally, the preset nickel tube temperature can be 475°C, the frequency of the electromagnetic driving device 81 can be 20Hz, and the design pressure of the hydrogen meter can be 1.5MPa.

启动高真空系统85对氢渗透结构84进行抽真空,启动氢计加热装置82,使其氢渗透结构84的温度达到要求,从而使得测量腔83内部氢分子能够通过氢渗透结构84的周壁进入氢渗透结构84内部,进而通过真空管路进入高真空系统85内。通过高真空系统85内离子泵86测试离子泵86电流大小,以确定进入氢渗透结构84的气体浓度;通过高真空系统85内质谱仪87测试气体组成成分,根据质谱仪87检测的气体组成成分确定进入氢渗透结构84的气体中氢气所占比例。Start the high vacuum system 85 to evacuate the hydrogen permeation structure 84, and start the hydrogen meter heating device 82 to make the temperature of the hydrogen permeation structure 84 meet the requirements, so that the hydrogen molecules inside the measurement chamber 83 can enter the hydrogen through the peripheral wall of the hydrogen permeation structure 84. Penetrates inside the structure 84 and then enters the high vacuum system 85 through the vacuum pipeline. Test the current size of the ion pump 86 through the ion pump 86 in the high vacuum system 85 to determine the gas concentration entering the hydrogen permeation structure 84; test the gas composition through the mass spectrometer 87 in the high vacuum system 85, and according to the gas composition detected by the mass spectrometer 87 The proportion of hydrogen in the gas entering the hydrogen permeable structure 84 is determined.

根据液态碱金属回路10中氢的浓度和质谱仪87检测的气体组成成分,对离子泵86检测的气体浓度进行标定,以获得氢计8在当前温度下的标定结果。According to the concentration of hydrogen in the liquid alkali metal circuit 10 and the gas composition detected by the mass spectrometer 87 , the gas concentration detected by the ion pump 86 is calibrated to obtain the calibration result of the hydrogen meter 8 at the current temperature.

之后,利用冷阱15对第二管路103中的含氢碱金属液体再次进行降温,以使碱金属的温度比利用冷阱15第一次降温时的温度下降1℃左右;之后利用阻塞计14获得含氢碱金属液体中的含氢化合物结晶析出的结晶温度,以获得含氢碱金属液体中含氢化合物在当前温度对应的饱和溶解度值。重复上述过程,从而实现对氢计8在不同的氢浓度下进行标定。After that, the cold trap 15 is used to cool down the hydrogen-containing alkali metal liquid in the second pipeline 103 again, so that the temperature of the alkali metal drops by about 1°C compared with the temperature when the cold trap 15 is used to cool down for the first time; and then the obstruction meter is used. 14 Obtain the crystallization temperature at which the hydrogen-containing compound in the hydrogen-containing alkali metal liquid crystallizes out, so as to obtain the saturated solubility value corresponding to the current temperature of the hydrogen-containing compound in the hydrogen-containing alkali metal liquid. Repeat the above process to achieve calibration of the hydrogen meter 8 under different hydrogen concentrations.

对于本申请的实施例,还需要说明的是,在不冲突的情况下,本申请的实施例及实施例中的特征可以相互组合以得到新的实施例。Regarding the embodiments of the present application, it should also be noted that, if there is no conflict, the embodiments of the present application and the features in the embodiments can be combined with each other to obtain new embodiments.

以上,仅为本申请的具体实施方式,但本申请的保护范围并不局限于此,本申请的保护范围应以权利要求的保护范围为准。The above are only specific embodiments of the present application, but the protection scope of the present application is not limited thereto. The protection scope of the present application shall be subject to the protection scope of the claims.

Claims (10)

1. A method of calibrating a hydrogen meter comprising a measurement chamber for receiving a hydrogen-containing alkali metal liquid, a hydrogen permeation structure positioned within the measurement chamber, a mass spectrometer, and a high vacuum system comprising an ion pump for providing a high vacuum environment for the hydrogen permeation structure to permeate hydrogen in the hydrogen-containing alkali metal liquid into the hydrogen permeation structure, wherein the method comprises:
Providing a liquid alkali metal loop for flowing liquid alkali metal;
injecting a hydrogen-containing gas into the liquid alkali metal loop to form a hydrogen-containing alkali metal liquid comprising a hydrogen-containing compound;
determining the concentration of hydrogen in the liquid alkali metal loop;
penetrating hydrogen and other gases in the hydrogen-containing alkali metal liquid into the hydrogen-permeable structure using the high vacuum system;
detecting a gas constituent entering the hydrogen permeation structure using the mass spectrometer;
detecting a concentration of gas entering the hydrogen permeation structure using the ion pump;
and calibrating the gas concentration detected by the ion pump according to the concentration of hydrogen in the liquid alkali metal loop and the gas composition detected by the mass spectrometer.
2. The method of claim 1, wherein determining the concentration of hydrogen in the liquid alkali metal loop comprises:
cooling the hydrogen-containing alkali metal liquid in the liquid alkali metal loop to crystallize and separate out part of hydrogen-containing compounds in the hydrogen-containing alkali metal liquid after cooling;
obtaining a crystallization temperature at which the hydrogen-containing compound in the hydrogen-containing alkali metal liquid is crystallized and separated, determining a saturated solubility value of the hydrogen-containing compound in the hydrogen-containing alkali metal liquid according to the crystallization temperature, and determining the concentration of hydrogen in the liquid alkali metal loop at the crystallization temperature according to the saturated solubility value of the hydrogen-containing compound.
3. The method of claim 2, wherein the gas composition entering the hydrogen permeation structure is detected with the mass spectrometer and the concentration of the gas entering the hydrogen permeation structure is detected with the ion pump at the crystallization temperature;
calibrating the concentration of the gas detected by the ion pump at the crystallization temperature according to the concentration of hydrogen in the liquid alkali metal loop at the crystallization temperature and the gas composition detected by the mass spectrometer at the crystallization temperature to obtain a calibration result of the hydrogen meter at the crystallization temperature.
4. The method of claim 3, further comprising, after determining the concentration of hydrogen in the liquid alkali metal loop at the crystallization temperature from the saturated solubility value of the hydrogen-containing compound:
cooling the hydrogen-containing alkali metal liquid in the liquid alkali metal loop by a preset temperature gradient to obtain a plurality of different saturated solubility values of hydrogen-containing compounds in the hydrogen-containing alkali metal liquid at different temperatures;
determining the concentration of hydrogen in the liquid alkali metal loop at different temperatures from the plurality of different saturated solubility values;
Detecting the gas composition entering the hydrogen permeation structure by using the mass spectrometer at different temperatures of the hydrogen-containing alkali metal liquid, and detecting the concentration of the gas entering the hydrogen permeation structure by using the ion pump;
and calibrating the gas concentration detected by the ion pump according to the concentration of hydrogen in the liquid alkali metal loop and the gas composition detected by the mass spectrometer so as to obtain calibration results of the hydrogen meter at different temperatures.
5. The method of claim 2, wherein,
cooling the hydrogen-containing alkali metal liquid in the liquid alkali metal circuit with a cooling portion;
obtaining a crystallization temperature at which the hydrogen-containing compound in the hydrogen-containing alkali metal liquid is crystallized by using a blockage meter.
6. The method of claim 1, wherein the calibrating the ion pump detected gas concentration based on the concentration of hydrogen in the liquid alkali metal loop and the mass spectrometer detected gas composition comprises:
determining the proportion of hydrogen in the gas entering the hydrogen permeation structure according to the gas composition detected by the mass spectrometer;
and calibrating the gas concentration detected by the ion pump according to the proportion of the hydrogen and the concentration of the hydrogen in the liquid alkali metal loop.
7. A calibration apparatus for a hydrogen meter comprising a measurement chamber for receiving a hydrogen-containing alkali metal liquid, a hydrogen permeation structure positioned within the measurement chamber, a mass spectrometer, and a high vacuum system comprising an ion pump for providing a high vacuum environment for the hydrogen permeation structure to permeate hydrogen in the hydrogen-containing alkali metal liquid into the hydrogen permeation structure, wherein the calibration apparatus comprises:
a liquid alkali metal loop for flowing liquid alkali metal, the liquid alkali metal loop having a calibration interface for connecting to a measurement cavity of the hydrogen meter so that the liquid alkali metal can enter the measurement cavity of the hydrogen meter;
a hydrogen supply section for supplying a hydrogen-containing gas into the liquid alkali metal circuit to form a hydrogen-containing alkali metal liquid containing a hydrogen-containing compound;
a control part for controlling the high vacuum system of the hydrogen meter to be started so as to enable hydrogen and other gases in the liquid alkali metal entering the measuring cavity to enter the hydrogen permeation structure, controlling the mass spectrometer to detect the gas composition entering the hydrogen permeation structure, and controlling the ion pump to detect the concentration of the gas entering the hydrogen permeation structure; and
And the processing part is used for calibrating the gas concentration detected by the ion pump according to the concentration of hydrogen in the liquid alkali metal loop and the gas composition detected by the mass spectrometer.
8. The calibration device of claim 7, further comprising:
a cooling part for cooling the hydrogen-containing alkali metal liquid in the liquid alkali metal loop so as to crystallize and separate out part of hydrogen-containing compounds in the hydrogen-containing alkali metal liquid after cooling; and
a blocker for obtaining a crystallization temperature at which a hydrogen-containing compound in the hydrogen-containing alkali metal liquid is crystallized out;
the processing section is further configured to determine a saturated solubility value of a hydrogen-containing compound in the hydrogen-containing alkali metal liquid based on the crystallization temperature, and determine a concentration of hydrogen in the liquid alkali metal circuit at the crystallization temperature based on the saturated solubility value of the hydrogen-containing compound.
9. The calibration device of claim 7, wherein the processing section is further configured to:
determining the proportion of hydrogen in the gas entering the hydrogen permeation structure according to the gas composition detected by the mass spectrometer;
and calibrating the gas concentration detected by the ion pump according to the proportion of the hydrogen and the concentration of the hydrogen in the liquid alkali metal loop.
10. The calibration device of claim 7, further comprising:
the buffer tank is arranged on the liquid alkali metal loop;
an inert gas supply section for supplying an inert gas into the buffer tank to stabilize the pressure in the liquid alkali metal circuit; and/or the number of the groups of groups,
an electromagnetic pump for driving the flow of liquid alkali metal in the liquid alkali metal loop; and/or the number of the groups of groups,
a liquid alkali metal vessel for storing liquid alkali metal and supplying liquid alkali metal to the liquid alkali metal circuit; and/or the number of the groups of groups,
and the vacuum part is used for vacuumizing the liquid alkali metal loop before supplying the liquid alkali metal to the liquid alkali metal loop.
CN202311514967.7A 2023-11-14 2023-11-14 Calibration method and calibration device of hydrogen meter Pending CN117554461A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118934588A (en) * 2024-08-30 2024-11-12 中国原子能科学研究院 Test system and test method for alkali metal driven pumps

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118934588A (en) * 2024-08-30 2024-11-12 中国原子能科学研究院 Test system and test method for alkali metal driven pumps

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