阅读说明：本技术 一种气体纯化装置、稀有气体同位素的测定设备及其方法 (Gas purification device, and rare gas isotope measuring equipment and method ) 是由 曹春辉 于 2021-08-20 设计创作，主要内容包括：本发明公开一种气体纯化装置、稀有气体同位素的测定设备及其方法,其中,一种气体纯化装置包括壳体和纯化机构,壳体具有反应腔,反应腔处于真空状态,且反应腔能够容置气体样品,纯化机构设置于壳体上,纯化机构具有空腔,纯化机构的空腔与反应腔连通,纯化机构用于对反应腔内的气体样品进行纯化处理,以得到纯化后的气体。相对于现有技术,纯化机构都是直接对反应腔内的气体样品进行纯化的,气体样品的整个纯化过程都是在反应腔内进行的,纯化时无需将气体样品进行多次分割,也无需将气体样品从一个纯化部件进入下一个纯化部件,从而有效避免气体样品在每个纯化部件之间转移的损失,从而大大降低了气体样品的损失率。(The invention discloses a gas purification device, and equipment and a method for measuring a rare gas isotope, wherein the gas purification device comprises a shell and a purification mechanism, the shell is provided with a reaction cavity, the reaction cavity is in a vacuum state and can contain a gas sample, the purification mechanism is arranged on the shell and is provided with a cavity, the cavity of the purification mechanism is communicated with the reaction cavity, and the purification mechanism is used for purifying the gas sample in the reaction cavity to obtain purified gas. Compared with the prior art, purification mechanism is direct to carry out the purification to the gas sample of reaction intracavity, and the whole purification process of gas sample is gone on in the reaction intracavity, need not to cut apart gas sample many times during the purification, also need not to get into next purification part with gas sample from a purification part to effectively avoid the loss that gas sample shifted between every purification part, thereby greatly reduced the loss rate of gas sample.)

1. A gas purification apparatus, comprising:

the device comprises a shell, a gas sample collecting device and a gas sample processing device, wherein the shell is provided with a reaction cavity which is in a vacuum state and can contain the gas sample; and

the purification mechanism is arranged on the shell and provided with a cavity, the cavity of the purification mechanism is communicated with the reaction cavity, and the purification mechanism is used for purifying the gas sample in the reaction cavity to obtain purified gas.

2. The gas purification apparatus of claim 1, wherein the purification mechanism comprises a water vapor removal assembly having a first housing chamber in communication with the reaction chamber, the water vapor removal assembly configured to remove water vapor from the gas sample within the reaction chamber.

3. The gas purification apparatus of claim 2, wherein the water vapor removal assembly comprises a cold finger and a coolant, the cold finger having the first receiving cavity, the cold finger being soaked in the coolant and causing the water vapor in the reaction cavity to cool and condense into ice.

4. The gas purification apparatus as claimed in claim 1, wherein the purification mechanism further comprises an active gas removal assembly disposed on the housing, the active gas removal assembly having a second receiving chamber, the second receiving chamber being in communication with the reaction chamber, the active gas removal assembly being configured to remove active gas from the reaction chamber.

5. The gas purification apparatus of claim 4, wherein the active gas removal assembly is a titanium sponge furnace.

6. The gas purification apparatus as claimed in claim 1, wherein the purification mechanism further comprises a hydrogen removal assembly disposed on the housing, the hydrogen removal assembly having a third receiving chamber in communication with the reaction chamber, the hydrogen removal assembly being configured to remove hydrogen from the reaction chamber.

7. The gas purification apparatus of claim 6, wherein the hydrogen removal component is a zirconium aluminum pump.

8. The gas purification apparatus as claimed in claim 1, wherein the purification mechanism further comprises an activated carbon trap disposed on the housing, the activated carbon trap having a fourth receiving chamber, the fourth receiving chamber being in communication with the reaction chamber, the activated carbon trap being configured to separate the rare gas in the reaction chamber.

9. A rare gas isotope measuring apparatus comprising the gas purifying device according to any one of claims 1 to 8 and a rare gas isotope spectrometer provided in the gas purifying device, the rare gas isotope spectrometer being configured to measure a rare gas in the gas purifying device.

10. A method for measuring a rare gas isotope, comprising:

delivering a gas sample into a reaction chamber of a housing;

opening a water vapor removal component to remove water vapor in the gas sample;

closing the water vapor removal assembly, opening the active gas removal assembly, and removing active gas in the gas sample treated by the water vapor removal assembly;

closing the active gas removal assembly, opening the hydrogen removal assembly, and removing hydrogen in the gas sample treated by the active gas removal assembly;

closing the hydrogen removal assembly, and separating rare gas in the gas sample treated by the active gas removal assembly;

and closing the active gas removal assembly, opening a rare gas isotope spectrometer, and carrying out isotope determination on the separated rare gas.

Technical Field

The invention relates to the technical field of rare gas isotopes, in particular to a gas purification device, a device and a method for determining rare gas isotopes.

Background

In the prior art, the rare gas analysis technology uses a linear purification system, the purification process is in a flow line type, each purification part is used as an independent section, and the communication of a gas sample in each purification part is controlled through valves at the front end and the rear end of each purification part. After the purification of the previous stage is completed, a part of the gas sample is taken to enter the next purification part for purification, the rest of the gas sample is pumped away by a vacuum pump, and each purification step causes a large amount of gas sample loss. Therefore, the high loss rate of the gas sample in the linear purification system becomes a technical problem to be solved urgently.

Disclosure of Invention

Therefore, it is necessary to provide a gas purification device, a rare gas isotope measurement apparatus, and a method thereof, so as to solve the technical problem of high gas sample loss rate of a linear purification system in the prior art.

The invention provides a gas purification device, comprising:

the device comprises a shell, a gas sample collecting device and a gas sample processing device, wherein the shell is provided with a reaction cavity which is in a vacuum state and can contain the gas sample; and

the purification mechanism is arranged on the shell and provided with a cavity, the cavity of the purification mechanism is communicated with the reaction cavity, and the purification mechanism is used for purifying the gas sample in the reaction cavity to obtain purified gas.

Further, the purification mechanism comprises a water vapor removal assembly, the water vapor removal assembly is provided with a first accommodating cavity, the first accommodating cavity is communicated with the reaction cavity, and the water vapor removal assembly is used for removing the water vapor of the gas sample in the reaction cavity.

Further, the water vapor removing assembly comprises a cold finger and a coolant, the cold finger is provided with the first accommodating cavity, the cold finger is soaked in the coolant, and the water vapor in the reaction cavity is cooled and condensed into ice.

Further, purification mechanism still includes active gas and gets rid of the subassembly, active gas get rid of the subassembly set up in on the casing, active gas gets rid of the subassembly and has second holding chamber, second holding chamber with reaction chamber intercommunication, active gas gets rid of the subassembly and is used for getting rid of the active gas in the reaction chamber.

Further, the active gas removal assembly is a titanium sponge furnace.

Further, the purification mechanism further comprises a hydrogen removal assembly, the hydrogen removal assembly is arranged on the shell and provided with a third accommodating cavity, the third accommodating cavity is communicated with the reaction cavity, and the hydrogen removal assembly is used for removing hydrogen in the reaction cavity.

Further, the hydrogen removal assembly is a zirconium aluminum pump.

Further, purification mechanism still includes the activated carbon trap, the activated carbon trap set up in on the casing, the activated carbon trap has the fourth holding chamber, the fourth holding chamber with the reaction chamber intercommunication, the activated carbon trap be used for with the rare gas separation in the reaction chamber.

In another embodiment, the present invention further provides a rare gas isotope measuring apparatus, which is characterized by comprising the above-mentioned gas purifying device and a rare gas isotope spectrometer, wherein the rare gas isotope spectrometer is disposed on the gas purifying device, and the rare gas isotope spectrometer is used for measuring the rare gas in the gas purifying device.

In another embodiment, the present invention also provides a method for measuring a rare gas isotope, comprising:

delivering a gas sample into a reaction chamber of a housing;

opening a water vapor removal component to remove water vapor in the gas sample;

closing the water vapor removal assembly, opening the active gas removal assembly, and removing active gas in the gas sample treated by the water vapor removal assembly;

closing the active gas removal assembly, opening the hydrogen removal assembly, and removing hydrogen in the gas sample treated by the active gas removal assembly;

closing the hydrogen removal assembly, and separating rare gas in the gas sample treated by the active gas removal assembly;

and closing the active gas removal assembly, opening a rare gas isotope spectrometer, and carrying out isotope determination on the separated rare gas.

The invention provides a gas purification device, wherein a shell is provided with a reaction cavity, the reaction cavity is in a vacuum state and is used for accommodating a cavity gas sample, purification mechanisms are arranged on the shell, and a cavity of each purification mechanism is communicated with the reaction cavity. Compared with the prior art, purification mechanism is direct to carry out the purification to the gas sample of reaction intracavity, and the whole purification process of gas sample is gone on in the reaction intracavity, need not to cut apart gas sample many times during the purification, also need not to get into next purification part with gas sample from a purification part to effectively avoid the loss that gas sample shifted between every purification part, thereby greatly reduced the loss rate of gas sample.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.

FIG. 1 is a schematic view of the structure of a gas purification apparatus and a rare gas isotope measuring apparatus in an embodiment of the subject matter of the present invention;

fig. 2 is a flow chart of a method for noble gas isotope determination in an embodiment of the inventive subject matter.

The main components are as follows:

100. a housing; 110. a reaction chamber; 200. a purification mechanism; 210. a water vapor removal assembly; 211. a first valve; 220. a reactive gas removal assembly; 221. a second valve; 230. a hydrogen removal assembly; 231. a third valve; 240. an activated carbon trap; 241. a fourth valve; 300. a vacuum gauge; 400. a vacuum pump set; 410. a fifth valve; 500. rare gas isotope spectrometers.

The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

It should be noted that all the directional indicators (such as up, down, left, right, front, and rear … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.

In addition, the descriptions related to "first", "second", etc. in the present invention are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, "and/or" in the whole text includes three schemes, taking a and/or B as an example, including a technical scheme, and a technical scheme that a and B meet simultaneously; in addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.

As shown in fig. 1, in some embodiments, a gas purifying apparatus includes a housing 100 and a purifying mechanism 200, the housing 100 has a reaction chamber 110, the reaction chamber 110 is in a vacuum state, and the reaction chamber 110 can contain a gas sample, the purifying mechanism 200 is disposed on the housing 100, the purifying mechanism 200 has a cavity, the cavity of the purifying mechanism 200 is communicated with the reaction chamber 110, and the purifying mechanism 200 is configured to purify the gas sample in the reaction chamber 110 to obtain a purified gas. Compared with the prior art, purification mechanism 200 is the gas sample that directly carries out the purification to in the reaction chamber 110, and the whole purification process of gas sample is gone on in reaction chamber 110, need not to cut apart gas sample many times during the purification, need not to get into next purification part with gas sample from a purification part to effectively avoid the loss of gas sample transfer between every purification part, thereby greatly reduced the loss rate of gas sample.

Specifically, the material of the housing 100 may be, but is not limited to, stainless steel. More specifically, the material of the housing 100 is 304 stainless steel. The stainless steel material has enough strength, high temperature resistance and chemical stability. The inner side wall of the shell 100 is polished, so that the inner side wall of the shell 100 is smoother, and the gas sample is prevented from being accommodated on the rough inner side wall surface to influence the purification effect of the gas sample. The shell 100 and the purification mechanism 200 can bear high temperature of 250 ℃ for baking and degassing, and the vacuum degree can reach the requirement of ultra-vacuum (better than 10)^-8Pa) that the gas sample can be stored in the reaction chamber 110 for at least 8 hours without leakage.

Further, the housing 100 is vacuum flanged to the purification mechanism 200.

In some embodiments, the purification mechanism 200 includes a water vapor removal assembly 210, the water vapor removal assembly 210 has a first housing chamber, the first housing chamber is communicated with the reaction chamber 110, and the water vapor removal assembly 210 is used for removing water vapor from the gas sample in the reaction chamber 110 to purify the gas sample. More specifically, the water vapor removal assembly 210 is disposed at the bottom of the housing 100. The water vapor removing assembly 210 is provided at the bottom of the case 100 to facilitate discharging condensed water to the outside. The water vapor removal assembly 210 is vacuum flanged to the housing 100. The gas purification apparatus includes a first valve 211, the first valve 211 is disposed between the first accommodating chamber and the reaction chamber 110, and the first valve 211 is used to control the communication or isolation between the first accommodating chamber and the reaction chamber 110. The first valve 211 is opened, the water vapor removing assembly 210 purifies the gas sample in the reaction chamber 110, the first valve 211 is closed, and the water vapor removing assembly 210 stops purifying the gas sample in the reaction chamber 110.

More specifically, the water vapor removing assembly 210 includes a cold finger having a first receiving chamber and a coolant, and the cold finger is soaked in the coolant and cools the water vapor in the reaction chamber to condense into ice. The cooling fluid may be, but is not limited to, liquid nitrogen. The cold finger is used for removing impurity gases such as water vapor and the like in a gas sample to achieve the purpose of purifying rare gas. Under the vacuum condition of the reaction chamber 110, the water vapor is condensed into ice by using the low-temperature environment of liquid nitrogen (the temperature of the cold finger is reduced to-196 ℃ by adding the liquid nitrogen), and the ice is collected in the first accommodating chamber of the cold finger, so that the water vapor in the gas sample is removed.

Further, the purification mechanism 200 further includes an active gas removing assembly 220, the active gas removing assembly 220 is disposed on the housing 100, the active gas removing assembly 220 has a second accommodating cavity, the second accommodating cavity is communicated with the reaction cavity 110, and the active gas removing assembly 220 is used for removing the active gas in the reaction cavity 110. Specifically, the active gas removal assembly 220 is a titanium sponge furnace. The reactive gas removal assembly 220 is vacuum flanged to the housing 100. The gas purification apparatus further includes a second valve 221, the second valve 221 is disposed between the second accommodating chamber and the reaction chamber 110, and the second valve 221 is used for controlling communication or isolation between the second accommodating chamber and the reaction chamber 110.

When the device works, the second valve 221 is opened, the sample gas in the reaction chamber 110 for removing water vapor reacts with the titanium sponge at high temperature, so that the active gas in the gas sample reacts with the active metal titanium to generate non-gas substances which are attached to the titanium sponge, and the active gas in the gas sample is removed. The second valve 221 is closed, and the active gas in the reaction chamber 110 cannot react with the titanium sponge furnace. The metal titanium belongs to very active metal, and can remove other gases except rare gases at high temperature to generate chemical reaction. The titanium sponge has a large number of gaps and a large reaction surface area, can be fully contacted with a gas sample, and is beneficial to improving the reaction rate of the metal titanium and the active gas, thereby improving the efficiency of removing the active gas.

In some embodiments, the purification mechanism 200 further includes a hydrogen removal assembly 230, the hydrogen removal assembly 230 is disposed on the housing 100, the hydrogen removal assembly 230 has a third accommodating cavity, the third accommodating cavity is communicated with the reaction chamber 110, and the hydrogen removal assembly 230 is configured to remove hydrogen in the reaction chamber 110. The hydrogen removal assembly 230 is vacuum flanged to the housing 100. The gas purification apparatus further includes a third valve 231, the third valve 231 is disposed between the third accommodating chamber and the reaction chamber 110, and the third valve 231 is used for controlling the communication or isolation between the third accommodating chamber and the reaction chamber 110. The hydrogen removing assembly 230 can purify the gas sample in the reaction chamber 110 by opening the third valve 231, and the hydrogen removing assembly 230 cannot purify the gas sample in the reaction chamber 110 by closing the third valve 231.

Specifically, the hydrogen removal assembly 230 is a zirconium aluminum pump. A zirconium-aluminum pump, also called a zirconium-aluminum getter pump, uses a zirconium-aluminum alloy getter material (84% zirconium and 16% aluminum) to adsorb active gas at high temperature. It has a high pumping capacity for reactive gases, especially for hydrogen, but it cannot pump inert gases.

The content of helium extracted from natural geological samples is very low, and particularly the concentration of helium isotopes is low. The amount of extracted helium cannot be increased in a laboratory by a method of increasing the amount of a sample, and the extracted helium can be utilized to the maximum extent, so that the helium enters a rare gas mass spectrometer as much as possible for analysis. The gas purification apparatus can be used for purification of helium gas because hydrogen gas has a great influence on helium gas, and it is necessary to ensure that no hydrogen gas is contained in the reaction chamber 110.

Further, the purification mechanism 200 further includes an activated carbon trap 240, the activated carbon trap 240 is disposed on the housing 100, the activated carbon trap 240 has a fourth accommodating cavity, the fourth accommodating cavity is communicated with the reaction cavity 110, and the activated carbon trap 240 is used for separating the rare gas in the reaction cavity 110. The activated carbon trap 240 is vacuum flanged to the housing 100. The purification apparatus further includes a fourth valve 241, the fourth valve 241 is disposed between the fourth accommodating chamber and the reaction chamber 110, and the fourth valve 241 is used for controlling the communication or isolation between the fourth accommodating chamber and the reaction chamber 110. When the fourth valve 241 is opened, the activated carbon trap 240 separates the rare gas in the reaction chamber 110, and when the fourth valve 241 is closed, the activated carbon trap 240 cannot react with the rare gas in the reaction chamber 110.

In some embodiments, the gas purification apparatus further includes a vacuum gauge 300, the vacuum gauge 300 is connected to the vacuum flange of the housing 100, and the vacuum gauge 300 is used for constantly detecting the degree of vacuum in the reaction chamber 110.

The gas purification apparatus further includes a vacuum pump unit 400, the vacuum pump unit 400 being vacuum flange-connected to the housing 100, the vacuum pump unit 400 being used to maintain a vacuum state in the reaction chamber 110. The gas purification apparatus further includes a fifth valve 410, and the housing 100 is connected to the vacuum pump unit 400 through the fifth valve 410. By opening the fifth valve 410, the vacuum pump set 400 can pump air from the reaction chamber 110 to maintain the vacuum state in the reaction chamber 110, and by closing the fifth valve 410, the vacuum pump cannot act on the reaction chamber 110.

In another embodiment, an apparatus for measuring a rare gas isotope includes a gas purification device and a rare gas isotope spectrometer 500, the rare gas isotope spectrometer 500 is disposed on the gas purification device, and the rare gas isotope spectrometer 500 is used for measuring a rare gas in the gas purification device. Specifically, the separated He, Ne, Ar, Kr and Xe components are respectively sent into an isotope spectrometer for isotope measurement, and the relative content and isotope data are obtained.

In another embodiment, as shown in fig. 2, a method for measuring a noble gas isotope includes the steps of:

s1, delivering the gas sample into the reaction chamber 110 of the housing 100;

s2, starting the water vapor removing component 210 to remove the water vapor in the gas sample;

s3, closing the water vapor removal component 210, opening the active gas removal component 220, and removing active gas in the gas sample processed by the water vapor removal component 210;

s4, closing the active gas removal component 220, opening the hydrogen removal component 230, and removing hydrogen in the gas sample processed by the active gas removal component 220;

s5, closing the hydrogen removal assembly 230, and separating the noble gas from the gas sample processed by the active gas removal assembly 220;

s6, the active gas removal module 220 is turned off, the noble gas isotope spectrometer 500 is turned on, and the separated noble gas is subjected to isotope measurement.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.