CN109323909B - Gas automatic separation system for inertness in small-gas-volume environment sample - Google Patents
Gas automatic separation system for inertness in small-gas-volume environment sample Download PDFInfo
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Abstract
The application discloses a system for inert gas automated separation in a small-gas-volume environment sample, includes: the vacuum device is used for enabling the system to be in a vacuum state; the control device is used for realizing the automatic control of the whole inert gas separation; the water removal device is used for removing water and carbon dioxide from the small-gas-volume environmental sample gas under the control of the control device; the titanium sponge high-temperature adsorption device is used for removing active gas in the sample gas in the small-gas-volume environment under the control of the control device; the gas chromatographic separation device is used for separating argon and krypton from small-gas-quantity environmental sample gas under the control of the control device; and the inert gas collection and measurement device is used for respectively collecting and measuring argon and krypton. The automatic simultaneous separation and extraction of krypton and argon can be realized in the small-gas-volume environmental sample, the problems of time consuming, long time consuming, complex operation, incapability of processing samples with complex components, low sample processing efficiency, high manual operation error rate and the like in the inert gas extraction and separation are solved.
Description
Technical Field
The application relates to the technical field of inert gas separation, in particular to a system for automatically separating inert gas in a small-gas-volume environment sample.
Background
Inert gas radioisotope85Kr，81Kr，39Ar is a good dating isotope, the isotope trace analysis method based on the laser cooling atom has important application in geological hydrology, and the efficient separation and extraction of the inert gas from a small amount of environmental sample gas is a key ring for realizing the application of the inert gas. The environment sample gas mainly refers to air, solution gas in underground water, seawater and glacier, and the gas components include nitrogen, oxygen, water, carbon dioxide, methane, etcActive gases and inert gases such as krypton and argon, usually with argon contents of a few percent, and much lower krypton, only a few parts per million.
At present, the inert gas separation and extraction method mainly extracts krypton gas or argon gas from atmospheric environmental samples in a single separation mode. For the separation and extraction of krypton gas, the method is realized by the following 3 steps:
firstly, removing a large amount of gases (nitrogen, oxygen, argon and the like) with high volatility by low-temperature distillation or low-temperature adsorption, and primarily enriching krypton gas; then, the separation of krypton and a small amount of other gases is realized through gas chromatography, a 5A molecular sieve chromatographic column is generally selected to realize the separation of krypton from oxygen, nitrogen and argon, and for a sample containing methane, an activated carbon chromatographic column is also required to realize the separation of methane and krypton. This method requires good temperature control during cryogenic distillation or adsorption, is complex in process, and cannot process methane-rich environmental samples.
The Li-LSX chromatographic column is generally adopted for low-temperature gas chromatography direct separation for the separation and purification of the argon, the method has higher requirements on chromatographic column filling and temperature control, and the method is also very complex in operation, suitable for the separation of argon with large gas volume, long in service time and not very high in efficiency.
In addition, the separation of argon and krypton is realized simultaneously by low-temperature distillation, high-temperature titanium furnace adsorption and gas chromatography separation, but the steps are complicated, the purity and the efficiency are low, the time is long, and the single sample separation time is 5-6 hours.
It can be seen that the methods described above generally require better temperature control, are complex in apparatus, and cannot process complex environmental samples (such as methane-rich environmental samples), and most importantly, all the methods described above have no automatic control, are operated by manpower, have high error rate and low processing efficiency, and have great limitations on applications.
Disclosure of Invention
In view of this, the application provides a system for the automatic separation of inert gas in a small-gas-volume environmental sample, which can realize the automatic simultaneous separation and extraction of krypton and argon in the small-gas-volume environmental sample, and solves the problems that the inert gas extraction and separation takes a long time, the operation is complex, the sample with complex components cannot be processed, the sample processing efficiency is low, and the manual operation error rate is high.
The application provides a system for inert gas automated separation in a small-gas-volume environmental sample, including: the device comprises a water removal device, a titanium sponge high-temperature adsorption device, a gas chromatography separation device, an inert gas collection and measurement device, a vacuum device and a control device; wherein:
the vacuum device is used for enabling the system to be in a vacuum state;
the control device is used for realizing the automatic control of the whole inert gas separation;
the water removal device is used for removing water and carbon dioxide from the small-gas-volume environmental sample gas under the control of the control device;
the titanium sponge high-temperature adsorption device is used for removing active gas in the small-gas-volume environment sample gas under the control of the control device;
the gas chromatographic separation device is used for realizing automatic separation of krypton and argon in a small-gas-volume environment sample under the control of the control device;
and the inert gas collection and measurement device is used for respectively collecting and measuring argon and krypton.
Preferably, the water removal device comprises: the stainless steel container is filled with the 5A molecular sieve.
Preferably, the titanium sponge high-temperature adsorption device comprises: the device comprises a mass flow controller, a titanium sponge high-temperature furnace tube, titanium sponge arranged in the titanium sponge high-temperature furnace tube and a film pressure gauge; wherein:
the mass flow controller is used for controlling the sample gas in the small-gas-volume environment to enter the titanium sponge high-temperature furnace tube at a preset flow rate;
the film pressure gauge is used for monitoring the air pressure of the titanium sponge high-temperature furnace tube;
the titanium sponge is used for removing active gas in a small-gas-volume environment sample gas.
Preferably, the gas chromatographic separation device comprises: the device comprises an active carbon low-temperature cold trap, helium carrier gas, a chromatographic column group and a quadrupole mass spectrometer, wherein:
the activated carbon low-temperature cold trap is used for collecting krypton gas and argon gas in small-gas-volume environment sample gas;
the helium carrier gas is used as a carrier gas for purging krypton gas and argon gas into the chromatographic column group;
the chromatographic column group is used for separating krypton gas and argon gas;
and the quadrupole mass spectrometer is used for monitoring the gas components after the chromatographic column group.
Preferably, the inert gas collection measurement device includes: a krypton gas collecting and measuring device and an argon gas collecting and measuring device; wherein:
the krypton gas collecting and measuring device is used for collecting and measuring krypton gas;
and the argon gas collecting and measuring device is used for collecting and measuring argon gas.
Preferably, the vacuum device comprises: stainless steel vacuum pipeline, stainless steel vacuum adaptor, vacuum seal and pump package.
Preferably, the control device includes: pneumatic valve, cylinder, pneumatic control box and controller.
Preferably, the pneumatic valve comprises: pneumatic two-way valve, pneumatic three-way valve, pneumatic cross valve.
Preferably, the set of chromatography columns comprises two 5A molecular sieve chromatography columns.
Preferably, the preset flow rate is 100-500 ml/min.
In summary, the present application discloses a system for the automated separation of inert gases in a small-volume environmental sample, comprising: the device comprises a water removal device, a titanium sponge high-temperature adsorption device, a gas chromatography separation device, an inert gas collection and measurement device, a vacuum device and a control device; wherein: the vacuum device is used for enabling the system to be in a vacuum state; the control device is used for realizing the automatic control of the whole inert gas separation; the water removal device is used for removing water and carbon dioxide from the small-gas-volume environmental sample gas under the control of the control device; the titanium sponge high-temperature adsorption device is used for removing active gas in the sample gas in the small-gas-volume environment under the control of the control device; the gas chromatographic separation device is used for separating argon and krypton from small-gas-quantity environmental sample gas under the control of the control device; and the inert gas collection and measurement device is used for respectively collecting and measuring argon and krypton. The automatic simultaneous separation and extraction of krypton and argon can be realized in the small-gas-volume environmental sample, the problems of time consuming, long time consuming, complex operation, incapability of processing samples with complex components, low sample processing efficiency, high manual operation error rate and the like in the inert gas extraction and separation are solved.
Drawings
In order to more clearly illustrate the embodiments of the present application 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 application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a system for automated separation of an inert gas from a small-volume environmental sample according to embodiment 1 of the present disclosure;
FIG. 2 is a schematic block diagram of embodiment 2 of a system for automated separation of inert gas from a small-volume environmental sample as disclosed herein;
FIG. 3 is a schematic diagram of the structure of embodiment 3 of the system for automated separation of inert gas from a small-volume environmental sample disclosed in the present application;
FIG. 4 is a schematic diagram illustrating an embodiment 4 of a system for automated separation of inert gas from a small-volume environmental sample as disclosed herein;
fig. 5 is a schematic structural diagram of embodiment 5 of the system for the automated separation of inert gas from a small-volume environmental sample disclosed in the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, 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 application.
As shown in fig. 1, which is a schematic structural diagram of embodiment 1 of a system for automated separation of inert gas in a small-gas-volume environmental sample disclosed in the present application, the system may include: a water removal device 11, a titanium sponge high-temperature adsorption device 12, a gas chromatography separation device 13, an inert gas collection and measurement device 14, a vacuum device 15 and a control device 16; wherein:
a vacuum device 15 for making the system in a vacuum state;
a control device 16 for realizing the automatic control of the whole inert gas separation;
a water removal device 11 for removing water and carbon dioxide from the small-volume environmental sample gas under the control of the control device 16;
the titanium sponge high-temperature adsorption device 12 is used for removing active gas in the sample gas in the small-gas-volume environment under the control of the control device 16;
the gas chromatographic separation device 13 is used for realizing the automatic separation of argon and krypton in the small-gas-volume environmental sample gas under the control of the control device 16;
and an inert gas collection and measurement device 14 for respectively collecting and measuring argon gas and krypton gas.
The working principle of the system for automatically separating the inert gas in the small-gas-volume environmental sample disclosed by the embodiment is as follows:
when the inert gas in the small-gas-amount environment sample needs to be automatically separated, the control device 16 controls the vacuum device 15 to enable the separation system to be in a vacuum state, then the small-gas-amount environment sample gas to be separated is introduced into the water removal device 11 to remove water and carbon dioxide in the gas, the gas subjected to water removal and carbon dioxide flow into the titanium sponge high-temperature adsorption device 12, the active gas in the flowing gas is removed through the titanium sponge high-temperature adsorption device 12, the gas subjected to active gas removal is introduced into the gas chromatography separation device 13, the gas chromatography separation device 13 separates the argon and the krypton in the small-gas-amount environment sample gas, and the separated argon and krypton are respectively collected and measured in the inert gas collection measuring device 14.
In conclusion, the automatic simultaneous separation and extraction of krypton and argon in a small-gas-volume environment sample can be realized, and the problems that the time is long, the operation is complex, the sample with complex components cannot be processed, the sample processing efficiency is low, the manual operation error rate is high and the like in the inert gas extraction and separation are solved.
As shown in fig. 2, which is a schematic structural diagram of embodiment 2 of the system for automatically separating inert gas from a small-gas-volume environmental sample disclosed in the present application, the system may include: a water removal device 21, a titanium sponge high-temperature adsorption device 22, a gas chromatography separation device 23, an inert gas collection and measurement device 24, a vacuum device 25 and a control device 26; wherein:
a vacuum device 25 for making the system in a vacuum state;
a control device 26 for realizing the automatic control of the whole inert gas separation;
the water removal device 21 comprises a stainless steel container, wherein a 5A molecular sieve is arranged in the stainless steel container and is used for removing water and carbon dioxide from the small-gas-volume environmental sample gas through the 5A molecular sieve under the control of the control device 26;
the titanium sponge high-temperature adsorption device 22 is used for removing active gas in the small-gas-volume environmental sample gas under the control of the control device 26;
the gas chromatographic separation device 23 is used for realizing the automatic separation of argon and krypton in the small-gas-volume environmental sample gas under the control of the control device 26;
and an inert gas collection and measurement device 24 for respectively collecting and measuring argon gas and krypton gas.
The working principle of the system for automatically separating the inert gas in the small-gas-volume environmental sample disclosed by the embodiment is as follows:
when the inert gas in the small-gas-volume environment sample needs to be automatically separated, the control device 26 controls the vacuum device 25 to enable the separation system to be in a vacuum state, then the small-volume environmental sample gas to be separated is introduced into a water removal device 21, the water removal device 21 comprises a stainless steel container and a 5A molecular sieve arranged in the stainless steel container, water and carbon dioxide in the gas are removed through a 5A molecular sieve in a stainless steel container, the gas after water and carbon dioxide removal flows into a titanium sponge high-temperature adsorption device 22, removing active gas in the inflowing gas by a titanium sponge high-temperature adsorption device 22, introducing the gas after removing the active gas into a gas chromatography separation device 23, the gas chromatographic separation device 23 separates argon and krypton from a small amount of environmental sample gas, and the separated argon and krypton are collected and measured in the inert gas collection and measurement device 24, respectively.
As shown in fig. 3, which is a schematic structural diagram of embodiment 3 of the system for automatically separating inert gas from a small-gas-volume environmental sample disclosed in the present application, the system may include: a water removal device 31, a titanium sponge high-temperature adsorption device 32, a gas chromatography separation device 33, an inert gas collection and measurement device 34, a vacuum device 35 and a control device 36; wherein:
a vacuum device 35 for making the system in a vacuum state;
a control device 36 for realizing the automatic control of the whole inert gas separation;
the water removal device 31 comprises a stainless steel container, wherein a 5A molecular sieve is arranged in the stainless steel container and is used for removing water and carbon dioxide from the small-gas-volume environmental sample gas through the 5A molecular sieve under the control of the control device 36;
titanium sponge high temperature adsorption equipment 32 includes: a mass flow controller 321, a titanium sponge high-temperature furnace tube 322, titanium sponge 323 arranged in the titanium sponge high-temperature furnace tube, and a film pressure gauge 324;
the mass flow controller 321 is used for controlling the sample gas in the small-gas-volume environment to enter the titanium sponge high-temperature furnace tube 322 at a preset flow rate;
a film pressure gauge 324 for monitoring the pressure of the titanium sponge high temperature furnace tube 322;
the titanium sponge 323 is used for removing active gas in the small-gas-volume environmental sample gas;
the gas chromatographic separation device 33 is used for realizing the automatic separation of argon and krypton in the small-gas-volume environmental sample gas under the control of the control device 36;
and an inert gas collection and measurement device 34 for respectively collecting and measuring argon gas and krypton gas.
The working principle of the system for automatically separating the inert gas in the small-gas-volume environmental sample disclosed by the embodiment is as follows:
when inert gas in a small-gas-volume environment sample needs to be automatically separated, firstly, the control device 36 controls the vacuum device 35 to enable the separation system to be in a vacuum state, then the small-gas-volume environment sample gas to be separated is introduced into the water removal device 31, the water removal device 31 comprises a stainless steel container and a 5A molecular sieve arranged in the stainless steel container, water and carbon dioxide in the gas are removed through the 5A molecular sieve in the stainless steel container, the gas subjected to water removal and carbon dioxide enters the titanium sponge high-temperature furnace tube 322 at a preset flow rate (for example, the flow rate of 100-500 ml/min) under the control of the mass flow controller 321, and reacts with the titanium sponge 323 in the titanium sponge high-temperature furnace tube 322, and all other gases except the inert gas are adsorbed by the reaction of the titanium sponge 323. The gas from which the active gas is removed is introduced into a gas chromatography separation device 33, the gas chromatography separation device 33 separates argon and krypton from the small-amount environmental sample gas, and the separated argon and krypton are respectively collected and measured in an inert gas collection and measurement device 34.
As shown in fig. 4, which is a schematic structural diagram of embodiment 4 of the system for automatically separating inert gas from a small-gas-volume environmental sample disclosed in the present application, the system may include: a water removal device 41, a titanium sponge high-temperature adsorption device 42, a gas chromatography separation device 43, an inert gas collection and measurement device 44, a vacuum device 45 and a control device 46; wherein:
a vacuum device 45 for making the system in a vacuum state;
a control device 46 for realizing the automatic control of the whole inert gas separation;
the water removal device 41 comprises a stainless steel container, wherein a 5A molecular sieve is arranged in the stainless steel container and is used for removing water and carbon dioxide from the small-gas-volume environmental sample gas through the 5A molecular sieve under the control of the control device 46;
titanium sponge high temperature adsorption equipment 42 includes: a mass flow controller 421, a titanium sponge high-temperature furnace tube 422, titanium sponge 423 arranged in the titanium sponge high-temperature furnace tube, and a film pressure gauge 424;
the mass flow controller 421 is used for controlling the sample gas in the small-gas-volume environment to enter the titanium sponge high-temperature furnace tube 422 at a preset flow rate;
a film pressure gauge 424 for monitoring the pressure of the titanium sponge high temperature furnace tube 422;
the titanium sponge 423 is used for removing active gas in the small-gas-volume environmental sample gas;
the gas chromatography separation apparatus 43 includes: an activated carbon cryotrap 431, a helium carrier gas 432, a chromatographic column group 433 and a quadrupole mass spectrometer 434;
the activated carbon cryotrap 431 is used for collecting krypton and argon in small-volume environment sample gas;
a chromatographic column group 433 for separating krypton gas and argon gas;
a quadrupole mass spectrometer 434 for monitoring the gas composition behind the column group 433;
and an inert gas collection and measurement device 44 for collecting and measuring argon gas and krypton gas, respectively.
The working principle of the system for automatically separating the inert gas in the small-gas-volume environmental sample disclosed by the embodiment is as follows:
when the inert gas in the small-gas-volume environment sample needs to be automatically separated, firstly, the control device 46 controls the vacuum device 45 to enable the separation system to be in a vacuum state, then the small-gas-volume environment sample gas to be separated is introduced into the water removal device 41, the water removal device 41 comprises a stainless steel container and a 5A molecular sieve arranged in the stainless steel container, water and carbon dioxide in the gas are removed through the 5A molecular sieve in the stainless steel container, the gas subjected to water removal and carbon dioxide enters the titanium sponge high-temperature furnace tube 422 at a preset flow rate (for example, the flow rate of 100-500 ml/min) under the control of the mass flow controller 421, and reacts with the titanium sponge 423 in the titanium sponge high-temperature furnace tube 422, and all other gases except the inert gas are adsorbed by the titanium sponge 423. The gas after the active gas removal is introduced into an active carbon cryotrap 431, the active carbon cryotrap 431 is made of stainless steel, active carbon is filled in the active carbon cryotrap 431, inert gases of krypton and argon after the high-temperature reaction of the titanium sponge 423 can be adsorbed at the temperature of liquid nitrogen, then the active carbon cryotrap 431 can be heated, the first chromatography is carried out, a helium carrier gas 432 comprises a helium flow path, a mass flow meter and a purification cryotrap, the inert gases of krypton and argon after the high-temperature reaction of the titanium sponge 423 are blown into a chromatographic column group 433 by using high-purity helium as the carrier gas, the mass flow meter is used for controlling the flow rate of the helium carrier gas 432, the krypton and argon are separated out from the chromatographic column group 433, a quadrupole mass spectrometer 434 is positioned at the outlet of the chromatographic column group 433, the separated argon and krypton are monitored at any time, and are respectively collected and measured in an inert gas collection and measurement device 44.
As shown in fig. 5, which is a schematic structural diagram of embodiment 5 of the system for automatically separating inert gas from a small-gas-volume environmental sample disclosed in the present application, the system may include: a water removal device 51, a titanium sponge high-temperature adsorption device 52, a gas chromatography separation device 53, an inert gas collection and measurement device 54, a vacuum device 55 and a control device 56; wherein:
a vacuum device 55 for making the system in a vacuum state;
a control device 56 for realizing the automatic control of the whole inert gas separation;
the water removal device 51 comprises a stainless steel container, wherein a 5A molecular sieve is filled in the stainless steel container and is used for removing water and carbon dioxide from the small-gas-volume environmental sample gas through the 5A molecular sieve under the control of the control device 56;
titanium sponge high temperature adsorption device 52 includes: a mass flow controller 521, a titanium sponge high-temperature furnace tube 522, titanium sponge 523 arranged in the titanium sponge high-temperature furnace tube, and a film pressure gauge 524;
the mass flow controller 521 is used for controlling the sample gas in the small-gas-volume environment to enter the titanium sponge high-temperature furnace tube 522 at a preset flow rate;
a film pressure gauge 524 for monitoring the pressure of the titanium sponge high-temperature furnace tube 522;
the titanium sponge 523 is used for removing active gas in the small-gas-volume environmental sample gas;
the gas chromatography separation device 53 includes: an active carbon low-temperature cold trap 531, a helium carrier gas 532, a chromatographic column group 533 and a quadrupole mass spectrometer 534;
the activated carbon low-temperature cold trap 531 is used for collecting krypton gas and argon gas in the small-gas-volume environment sample gas;
a column group 533 for separating krypton and argon;
a quadrupole mass spectrometer 534 for monitoring the gas composition behind the column set 533;
the inert gas collection measurement device 54 includes: and the krypton gas collecting and measuring device 541 and the argon gas collecting and measuring device 542 are used for respectively collecting and measuring argon gas and krypton gas.
The working principle of the system for automatically separating the inert gas in the small-gas-volume environmental sample disclosed by the embodiment is as follows:
when the inert gas in the small-gas-volume environment sample needs to be automatically separated, firstly, the control device 56 controls the vacuum device 55 to enable the separation system to be in a vacuum state, then the small-gas-volume environment sample gas to be separated is introduced into the water removal device 51, the water removal device 51 comprises a stainless steel container and a 5A molecular sieve arranged in the stainless steel container, water and carbon dioxide in the gas are removed through the 5A molecular sieve in the stainless steel container, the gas subjected to water removal and carbon dioxide enters the titanium sponge high-temperature furnace tube 522 at a preset flow rate (for example, the flow rate of 100-500 ml/min) under the control of the mass flow controller 521 and reacts with the titanium sponge 523 in the titanium sponge high-temperature furnace tube 522, and all other gases except the inert gas are adsorbed by the titanium sponge 523. The gas from which the active gas is removed is introduced into an active carbon cryotrap 531, the active carbon cryotrap 531 is made of stainless steel and filled with active carbon, the inert gases krypton and argon after the high-temperature reaction of the titanium sponge 523 can be adsorbed at the liquid nitrogen temperature, then the activated carbon low-temperature cold trap 531 can be heated to perform primary chromatography, the helium carrier gas 532 comprises a helium flow path, a mass flow meter and a purification cold trap, the inert gases krypton and argon after the high-temperature reaction of the titanium sponge 523 are swept into the chromatographic column group 533 by using high-purity helium as carrier gas, the mass flow meter is used for controlling the flow rate of the helium carrier gas 532, the krypton and argon are separated out from the chromatographic column group 533, the quadrupole mass spectrometer 534 is positioned at the outlet of the chromatographic column group 533, the separated argon and krypton are monitored at any time, when argon is detected, argon is introduced into the argon collection and measurement device 542, and when krypton is detected, krypton is introduced into the krypton collection and measurement device 541.
Specifically, in the above embodiment, the set of columns may comprise two 5A molecular sieve columns.
Specifically, in the above embodiment, the krypton collecting and measuring device is made of a stainless steel tube, filled with activated carbon, sealed by a vacuum valve, and capable of adsorbing krypton at the liquid nitrogen temperature or being detached from the system separately, and the krypton collected by the gas chromatograph can be transferred to a collecting container, and the krypton collecting and measuring device further includes a membrane pressure gauge for measuring the content of krypton.
Specifically, in the above embodiment, the argon gas collecting and measuring device is made of a stainless steel tube, is filled with activated carbon, is sealed by a vacuum valve, can adsorb argon gas at liquid nitrogen temperature, and can also be detached from the system independently, the argon gas collected by the gas chromatograph can be transferred to a collecting container, and the argon gas collecting and measuring device further comprises a film pressure gauge for measuring the content of the argon gas.
Specifically, in the above embodiment, the vacuum apparatus includes: stainless steel vacuum tubing, stainless steel vacuum adapters, vacuum seals and pump sets for creating and maintaining the vacuum conditions required for the gas separation system.
Specifically, in the above embodiment, the control device part is used to control the automatic operation of the whole separation and extraction process, and includes a hardware part and a software part. The hardware part comprises: the pneumatic valve, the air cylinder and the pneumatic control box; the software part in the controller is a control program written based on matlab. The pneumatic valve comprises a pneumatic two-way valve, a pneumatic three-way valve and a pneumatic four-way valve, and the opening and closing of the valve are controlled by whether air is supplied or not. The cylinder is arranged under all the activated carbon low-temperature cold traps and krypton-argon collecting containers, the heat-insulating container filled with liquid nitrogen is fixed at the top end of the cylinder, and the lifting of the cylinder can be controlled by controlling whether to supply gas to the cylinder or not, so that whether to supply liquid nitrogen to the low-temperature cold traps or not is controlled. The pneumatic control box is internally provided with an electromagnetic valve, a relay and a singlechip which are media for connecting a computer and the pneumatic valve. The high-level signal generated by the computer control singlechip can control the opening and closing of the electromagnetic valve, further control the on-off of the control gas circuit of the pneumatic valve and the cylinder, and finally control the opening and closing of the valve and the lifting of the cylinder. The whole software part of the control software part comprises reading and storing data of all the film pressure gauges, the mass flow meters and the quadrupole mass spectrometers, and controls the valve switch and the cylinder to lift according to the trigger signal under the condition of meeting a certain condition, thereby completing the automatic operation of the whole separation and extraction process. Namely, in the control process, the controller judges the current state of the system by reading parameters of the dewatering device, the titanium sponge high-temperature adsorption device, the gas chromatography separation device, the inert gas collection and measurement device and various sensing devices (a thermometer, a film pressure gauge, a mass flow meter and a quadrupole mass spectrometer) in the vacuum device, and sends correct instructions to the pneumatic control box so as to control the opening and closing of various pneumatic valves and the lifting of the air cylinder, and finally the next state of the system is controlled. The whole separation process is finally completed by repeating the steps.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
Those of skill would further appreciate that the various illustrative elements and algorithm steps described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both, and that the various illustrative components and steps have been described above generally in terms of their functionality in order to clearly illustrate this interchangeability of hardware and software. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the implementation. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present application.
The steps of a method or algorithm described in connection with the embodiments disclosed herein may be embodied directly in hardware, in a software module executed by a processor, or in a combination of the two. A software module may reside in Random Access Memory (RAM), memory, Read Only Memory (ROM), electrically programmable ROM, electrically erasable programmable ROM, registers, hard disk, a removable disk, a CD-ROM, or any other form of storage medium known in the art.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Accordingly, the application is not intended to be limited to the embodiments shown herein,
but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A system for automated separation of an inert gas from a small volume environmental sample, comprising: the device comprises a water removal device, a titanium sponge high-temperature adsorption device, a gas chromatography separation device, an inert gas collection and measurement device, a vacuum device and a control device; wherein:
the vacuum device is used for enabling the system to be in a vacuum state;
the control device is used for realizing the automatic control of the whole inert gas separation;
the water removal device is used for removing water and carbon dioxide from the small-gas-volume environmental sample gas under the control of the control device;
the titanium sponge high-temperature adsorption device is used for removing active gas in the small-gas-volume environment sample gas under the control of the control device;
the gas chromatographic separation device is used for realizing automatic separation of argon and krypton in small-gas-volume environmental sample gas through a chromatographic column group under the control of the control device, wherein the chromatographic column group comprises two 5A molecular sieve chromatographic columns;
and the inert gas collection and measurement device is used for respectively collecting and measuring argon and krypton.
2. The system of claim 1, wherein the water removal device comprises: the stainless steel container is filled with the 5A molecular sieve.
3. The system of claim 2, wherein the titanium sponge high temperature sorption device comprises: the device comprises a mass flow controller, a titanium sponge high-temperature furnace tube, titanium sponge arranged in the titanium sponge high-temperature furnace tube and a film pressure gauge; wherein:
the mass flow controller is used for controlling the sample gas in the small-gas-volume environment to enter the titanium sponge high-temperature furnace tube at a preset flow rate;
the film pressure gauge is used for monitoring the air pressure of the titanium sponge high-temperature furnace tube;
the titanium sponge is used for removing active gas in a small-gas-volume environment sample gas.
4. The system of claim 3, wherein the gas chromatography separation device comprises: the device comprises an active carbon low-temperature cold trap, helium carrier gas, a chromatographic column group and a quadrupole mass spectrometer, wherein:
the activated carbon low-temperature cold trap is used for collecting krypton gas and argon gas in small-gas-volume environment sample gas;
the helium carrier gas is used as a carrier gas for purging krypton gas and argon gas into the chromatographic column group;
the chromatographic column group is used for separating krypton gas and argon gas;
and the quadrupole mass spectrometer is used for monitoring the gas components after the chromatographic column group.
5. The system of claim 4, wherein the inert gas collection measurement device comprises: a krypton gas collecting and measuring device and an argon gas collecting and measuring device; wherein:
the krypton gas collecting and measuring device is used for collecting and measuring krypton gas;
and the argon gas collecting and measuring device is used for collecting and measuring argon gas.
6. The system of claim 5, wherein the vacuum device comprises: stainless steel vacuum pipeline, stainless steel vacuum adaptor, vacuum seal and pump package.
7. The system of claim 6, wherein the control device comprises: pneumatic valve, cylinder, pneumatic control box and controller.
8. The system of claim 7, wherein the pneumatic valve comprises: pneumatic two-way valve, pneumatic three-way valve, pneumatic cross valve.
9. The system of claim 8, wherein the predetermined flow rate is 100 to 500 ml/min.
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