CN109323909A - One kind automating separation system for gas inert in small tolerance environmental sample - Google Patents
One kind automating separation system for gas inert in small tolerance environmental sample Download PDFInfo
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- CN109323909A CN109323909A CN201811230380.2A CN201811230380A CN109323909A CN 109323909 A CN109323909 A CN 109323909A CN 201811230380 A CN201811230380 A CN 201811230380A CN 109323909 A CN109323909 A CN 109323909A
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- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
Isolated system is automated for inert gas in small tolerance environmental sample this application discloses a kind of, comprising: vacuum plant, for making system be in vacuum state；Control device, for realizing the automation control of entire inert gas separation；De-watering apparatus, for small tolerance environmental sample gas to be removed water and carbon dioxide under control of the control means；Titanium sponge high temperature adsorption device, for removing the active gases in small tolerance environmental sample gas under control of the control means；Gas-chromatography separator, for isolating argon gas and Krypton in small tolerance environmental sample gas under control of the control means；Inert gas collects measuring device, for collecting respectively and measuring argon gas and Krypton.The application can be realized the automation of Krypton and argon gas in small tolerance environmental sample while separation and Extraction, solve inert gas extract in separation it is time-consuming long, it is complicated for operation, can not processes composition complexity sample, the problems such as sample treatment inefficiency, manual operation error rate is high.
Description
Technical field
This application involves inert gas separation technology fields, more particularly to one kind is for indifferent gas in small tolerance environmental sample
Body automates isolated system.
Background technique
Noble gas activity isotope85Kr,81Kr,39Ar be it is good determine year isotope, based on laser cooling and trapping atoms
Isotope trace analysis methods have important application in geohydrology, efficiently divide from a small amount of environmental sample gas
It is the key link for realizing its application from inert gas is extracted.Environmental sample gas refers mainly to air, underground water, seawater,
Solution gas in glacier, gas componant include that nitrogen, oxygen gas and water, carbon dioxide, methane isoreactivity gas and Krypton, argon gas are lazy
Property gas, usual argon content be a few percent, krypton is lower, only a few millionths.
Currently, inert gas separating and extracting process mainly separation and Extraction Krypton single from the environmental sample of atm number or
Person's argon gas.For the separation and Extraction of Krypton, realized by following 3 step:
The high gas of a large amount of volatility (nitrogen, oxygen, argon gas etc.) is removed first with low temperature distillation or cryogenic absorption,
Krypton is subjected to preliminary concentration；Then the separation that Krypton and other micro gases are realized by gas-chromatography, is typically chosen 5A
Molecular sieve chromatography column realizes Krypton and oxygen, nitrogen, the separation of argon gas, for the sample containing methane, it is also necessary to active carbon
The separation of chromatographic column realization methane and Krypton.This method needs have good temperature to control in low temperature distillation or absorption, mistake
Journey is complex, and can not handle the environmental sample rich in methane.
It generally uses Li-LSX chromatographic column to carry out cryogenic gas-chromatography the separating-purifying of argon gas to be directly separated, this side
Method fills chromatographic column and temperature control has higher requirement, likewise, operating also very complicated, the argon suitable for atm number
Gas separates and the used time is more long, and efficiency is also not very high.
In addition also have and utilize low temperature distillation, the absorption of high temperature titanium furnace and gas phase chromatographic isolation while point for realizing argon gas and Krypton
From, but step is relatively complicated, and purity and efficiency are lower, the used time is more long, and single sample disengaging time was at 5-6 hours.
It can thus be seen that several method described above generally requires preferable temperature control, device is complicated, can not
Processes composition complex environment sample (such as environmental sample rich in methane), the most key, above-mentioned all methods arrive
It there is presently no automation control is realized, manually operates entirely, error rate is high, and treatment effeciency is very low, produces to application very big
Limitation.
Summary of the invention
In view of this, being for what inert gas automation in small tolerance environmental sample separated this application provides a kind of
System can be realized the automation of Krypton and argon gas in small tolerance environmental sample while separation and Extraction, solve inert gas extraction
In separation it is time-consuming long, it is complicated for operation, can not processes composition complexity sample, sample treatment inefficiency, manual operation malfunctions
The problems such as rate is high.
Isolated system is automated for inert gas in small tolerance environmental sample this application provides a kind of, comprising: remove
Water installations, titanium sponge high temperature adsorption device, gas-chromatography separator, inert gas collect measuring device, vacuum plant and control
Device processed；Wherein:
The vacuum plant, for making system be in vacuum state；
The control device, for realizing the automation control of entire inert gas separation；
The de-watering apparatus, for small tolerance environmental sample gas to be removed water and two under the control of the control device
Carbonoxide；
The titanium sponge high temperature adsorption device, for removing small tolerance environmental sample gas under the control of the control device
Active gases in body；
The gas-chromatography separator, for realizing krypton in small tolerance environmental sample under the control of the control device
Being automatically separated between gas and argon gas；
The inert gas collects measuring device, for collecting respectively and measuring argon gas and Krypton.
Preferably, the de-watering apparatus includes: rustless steel container, and 5A molecular sieve is housed in the rustless steel container.
Preferably, the titanium sponge high temperature adsorption device includes: mass flow control meter, titanium sponge high temperature furnace pipe, is mounted in
Titanium sponge and diaphragm gauge in the titanium sponge high temperature furnace pipe；Wherein:
The mass flow control meter enters the sponge for controlling small tolerance environmental sample gas with preset flow velocity
Titanium high temperature furnace pipe；
The diaphragm gauge, for monitoring the air pressure of the titanium sponge high temperature furnace pipe；
The titanium sponge, for removing the active gases in small tolerance environmental sample gas.
Preferably, the gas-chromatography separator includes: active carbon cryotrap, helium carrier gas, chromatographic column group and quadrupole
Bar mass spectrograph, in which:
The active carbon cryotrap, for collecting Krypton and argon gas in small tolerance environmental sample gas；
The helium carrier gas, for Krypton and argon gas to be purged into the chromatographic column group as carrier gas；
The chromatographic column group, for separating Krypton and argon gas；
The quadrupole mass spectrometer, for monitoring the gas componant after the chromatographic column group.
Preferably, it includes: that Krypton collects measuring device and argon gas collection measurement dress that the inert gas, which collects measuring device,
It sets；Wherein:
The Krypton collects measuring device, for collecting and measuring Krypton；
The argon gas collects measuring device, for collecting and measuring argon gas.
Preferably, the vacuum plant include: stainless-steel vacuum pipeline, stainless-steel vacuum adapter, vacuum seal and
Pump group.
Preferably, the control device includes: operated pneumatic valve, cylinder, pneumatic control box and controller.
Preferably, the operated pneumatic valve includes: pneumatic two-way valve, Pneumatic three-way valve, Pneumatic four-way valve.
Preferably, the chromatographic column group includes two 5A molecular sieve chromatography columns.
Preferably, the preset flow velocity is 100~500ml/min.
In conclusion being for what inert gas automation in small tolerance environmental sample separated this application discloses a kind of
System, comprising: de-watering apparatus, titanium sponge high temperature adsorption device, gas-chromatography separator, inert gas collect measuring device, true
Empty device and control device；Wherein: vacuum plant, for making system be in vacuum state；Control device, for realizing entire lazy
Property gas separation automation control；De-watering apparatus, under control of the control means removing small tolerance environmental sample gas
Remove water and carbon dioxide；Titanium sponge high temperature adsorption device, for removing small tolerance environmental sample gas under control of the control means
Active gases in body；Gas-chromatography separator, for isolating small tolerance environmental sample gas under control of the control means
Argon gas and Krypton in body；Inert gas collects measuring device, for collecting respectively and measuring argon gas and Krypton.The application can
It realizes the automation of Krypton and argon gas in small tolerance environmental sample while separation and Extraction, solves inert gas and extract and consumed in separation
Shi Jiu, it is complicated for operation, can not processes composition complexity sample, sample treatment inefficiency, manual operation error rate height etc. asks
Topic.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of application for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is that a kind of system isolated for inert gas automation in small tolerance environmental sample disclosed in the present application is implemented
The structural schematic diagram of example 1；
Fig. 2 is that a kind of system isolated for inert gas automation in small tolerance environmental sample disclosed in the present application is implemented
The structural schematic diagram of example 2；
Fig. 3 is that a kind of system isolated for inert gas automation in small tolerance environmental sample disclosed in the present application is implemented
The structural schematic diagram of example 3；
Fig. 4 is that a kind of system isolated for inert gas automation in small tolerance environmental sample disclosed in the present application is implemented
The structural schematic diagram of example 4；
Fig. 5 is that a kind of system isolated for inert gas automation in small tolerance environmental sample disclosed in the present application is implemented
The structural schematic diagram of example 5.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present application, technical solutions in the embodiments of the present application carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of embodiments of the present application, instead of all the embodiments.It is based on
Embodiment in the application, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall in the protection scope of this application.
As shown in Figure 1, to be disclosed in the present application a kind of for inert gas automation separation in small tolerance environmental sample
The structural schematic diagram of system embodiment 1, the system may include: de-watering apparatus 11, titanium sponge high temperature adsorption device 12, gas phase
Chromatographic separation device 13, inert gas collect measuring device 14, vacuum plant 15 and control device 16；Wherein:
Vacuum plant 15, for making system be in vacuum state；
Control device 16, for realizing the automation control of entire inert gas separation；
De-watering apparatus 11, for small tolerance environmental sample gas to be removed water and titanium dioxide under the control of the control means 16
Carbon；
Titanium sponge high temperature adsorption device 12, for being removed in small tolerance environmental sample gas under the control of the control means 16
Active gases；
Gas-chromatography separator 13, for realizing argon in small tolerance environmental sample gas under the control of the control means 16
Gas and Krypton are automatically separated；
Inert gas collects measuring device 14, for collecting respectively and measuring argon gas and Krypton.
The disclosed work that isolated system is automated for inert gas in small tolerance environmental sample of above-described embodiment is former
Reason are as follows:
When needing to carry out inert gas in small tolerance environmental sample automation separation, controlled first by control device 16
Vacuum plant 15 processed makes separation system be in vacuum state, and small tolerance environmental sample gas to be separated is then passed through water removal dress
It sets in 11, removes the water and carbon dioxide in gas, flow into titanium sponge high temperature adsorption dress with the gas of carbon dioxide by removing water
It sets in 12, the active gases in gas flowed by the removal of titanium sponge high temperature adsorption device 12, the gas after removing active gases
Body is passed through in gas-chromatography separator 13, and gas-chromatography separator 13 isolates the argon gas in small tolerance environmental sample gas
And Krypton, the argon gas isolated and Krypton collect in measuring device 14 in inert gas respectively and are collected and measure.
In conclusion can be realized the automation of Krypton and argon gas in small tolerance environmental sample while separation and Extraction, solve
Inert gas extract in separation it is time-consuming long, it is complicated for operation, can not processes composition complexity sample, sample treatment low efficiency
Under, the problems such as manual operation error rate is high.
As shown in Fig. 2, to be disclosed in the present application a kind of for inert gas automation separation in small tolerance environmental sample
The structural schematic diagram of system embodiment 2, the system may include: de-watering apparatus 21, titanium sponge high temperature adsorption device 22, gas phase
Chromatographic separation device 23, inert gas collect measuring device 24, vacuum plant 25 and control device 26；Wherein:
Vacuum plant 25, for making system be in vacuum state；
Control device 26, for realizing the automation control of entire inert gas separation；
De-watering apparatus 21 includes rust steel container, 5A molecular sieve is housed in rustless steel container, for the control in control device 26
System is lower to remove water and carbon dioxide for small tolerance environmental sample gas by 5A molecular sieve；
Titanium sponge high temperature adsorption device 22, for being removed under the control of control device 26 in small tolerance environmental sample gas
Active gases；
Gas-chromatography separator 23, for realizing argon in small tolerance environmental sample gas under the control of control device 26
Gas and Krypton are automatically separated；
Inert gas collects measuring device 24, for collecting respectively and measuring argon gas and Krypton.
The disclosed work that isolated system is automated for inert gas in small tolerance environmental sample of above-described embodiment is former
Reason are as follows:
When needing to carry out inert gas in small tolerance environmental sample automation separation, controlled first by control device 26
Vacuum plant 25 processed makes separation system be in vacuum state, and small tolerance environmental sample gas to be separated is then passed through water removal dress
It sets in 21, de-watering apparatus 21 includes rustless steel container, and the 5A molecular sieve in rustless steel container, passes through rustless steel container
In 5A molecular sieve remove gas in water and carbon dioxide, through water removal and carbon dioxide gas flow into titanium sponge high temperature inhale
In adsorption device 22, the active gases in gas flowed by the removal of titanium sponge high temperature adsorption device 22, after removing active gases
Gas be passed through in gas-chromatography separator 23, gas-chromatography separator 23 is isolated in small tolerance environmental sample gas
Argon gas and Krypton, the argon gas isolated and Krypton collect in measuring device 24 in inert gas respectively and are collected and measure.
As shown in figure 3, to be disclosed in the present application a kind of for inert gas automation separation in small tolerance environmental sample
The structural schematic diagram of system embodiment 3, the system may include: de-watering apparatus 31, titanium sponge high temperature adsorption device 32, gas phase
Chromatographic separation device 33, inert gas collect measuring device 34, vacuum plant 35 and control device 36；Wherein:
Vacuum plant 35, for making system be in vacuum state；
Control device 36, for realizing the automation control of entire inert gas separation；
De-watering apparatus 31 includes rust steel container, 5A molecular sieve is housed in rustless steel container, for the control in control device 36
System is lower to remove water and carbon dioxide for small tolerance environmental sample gas by 5A molecular sieve；
Titanium sponge high temperature adsorption device 32, comprising: mass flow control meter 321, is mounted in sea at titanium sponge high temperature furnace pipe 322
Titanium sponge 323, diaphragm gauge 324 in continuous titanium high temperature furnace pipe；
Mass flow control meter 321 enters titanium sponge high temperature for controlling small tolerance environmental sample gas with preset flow velocity
Boiler tube 322；
Diaphragm gauge 324, for monitoring the air pressure of titanium sponge high temperature furnace pipe 322；
Titanium sponge 323, for removing the active gases in small tolerance environmental sample gas；
Gas-chromatography separator 33, for realizing argon in small tolerance environmental sample gas under the control of the control unit 36
Gas and Krypton are automatically separated；
Inert gas collects measuring device 34, for collecting respectively and measuring argon gas and Krypton.
The disclosed work that isolated system is automated for inert gas in small tolerance environmental sample of above-described embodiment is former
Reason are as follows:
When needing to carry out inert gas in small tolerance environmental sample automation separation, controlled first by control device 36
Vacuum plant 35 processed makes separation system be in vacuum state, and small tolerance environmental sample gas to be separated is then passed through water removal dress
It sets in 31, de-watering apparatus 31 includes rustless steel container, and the 5A molecular sieve in rustless steel container, passes through rustless steel container
In 5A molecular sieve remove gas in water and carbon dioxide, through water removal and carbon dioxide gas mass flow control count
Under 321 control, entered in titanium sponge high temperature furnace pipe 322 with preset flow velocity (for example, flow velocity of 100~500ml/min), and
It is reacted with the titanium sponge 323 in titanium sponge high temperature furnace pipe 322, other all gas in addition to inert gas are all by titanium sponge
323 reaction absorption.Gas after removing active gases is passed through in gas-chromatography separator 33, and gas-chromatography separator 33 divides
The argon gas and Krypton in small tolerance environmental sample gas are separated out, the argon gas isolated and Krypton are collected in inert gas respectively to be measured
It is collected and measures in device 34.
As shown in figure 4, to be disclosed in the present application a kind of for inert gas automation separation in small tolerance environmental sample
The structural schematic diagram of system embodiment 4, the system may include: de-watering apparatus 41, titanium sponge high temperature adsorption device 42, gas phase
Chromatographic separation device 43, inert gas collect measuring device 44, vacuum plant 45 and control device 46；Wherein:
Vacuum plant 45, for making system be in vacuum state；
Control device 46, for realizing the automation control of entire inert gas separation；
De-watering apparatus 41 includes rust steel container, 5A molecular sieve is housed in rustless steel container, for the control in control device 46
System is lower to remove water and carbon dioxide for small tolerance environmental sample gas by 5A molecular sieve；
Titanium sponge high temperature adsorption device 42, comprising: mass flow control meter 421, is mounted in sea at titanium sponge high temperature furnace pipe 422
Titanium sponge 423, diaphragm gauge 424 in continuous titanium high temperature furnace pipe；
Mass flow control meter 421 enters titanium sponge high temperature for controlling small tolerance environmental sample gas with preset flow velocity
Boiler tube 422；
Diaphragm gauge 424, for monitoring the air pressure of titanium sponge high temperature furnace pipe 422；
Titanium sponge 423, for removing the active gases in small tolerance environmental sample gas；
Gas-chromatography separator 43 includes: active carbon cryotrap 431, helium carrier gas 432, chromatographic column group 433 and quadrupole
Bar mass spectrograph 434；
Active carbon cryotrap 431, for collecting Krypton and argon gas in small tolerance environmental sample gas；
Helium carrier gas 432, for Krypton and argon gas to be purged into chromatographic column group 433 as carrier gas；
Chromatographic column group 433, for separating Krypton and argon gas；
Quadrupole mass spectrometer 434, for monitoring the gas componant after chromatographic column group 433；
Inert gas collects measuring device 44, for collecting respectively and measuring argon gas and Krypton.
The disclosed work that isolated system is automated for inert gas in small tolerance environmental sample of above-described embodiment is former
Reason are as follows:
When needing to carry out inert gas in small tolerance environmental sample automation separation, controlled first by control device 46
Vacuum plant 45 processed makes separation system be in vacuum state, and small tolerance environmental sample gas to be separated is then passed through water removal dress
It sets in 41, de-watering apparatus 41 includes rustless steel container, and the 5A molecular sieve in rustless steel container, passes through rustless steel container
In 5A molecular sieve remove gas in water and carbon dioxide, through water removal and carbon dioxide gas mass flow control count
Under 421 control, entered in titanium sponge high temperature furnace pipe 422 with preset flow velocity (for example, flow velocity of 100~500ml/min), and
It is reacted with the titanium sponge 423 in titanium sponge high temperature furnace pipe 422, other all gas in addition to inert gas are all by titanium sponge
423 reaction absorption.Gas after removing active gases is passed through in active carbon cryotrap 431, and active carbon cryotrap 431 is not by
Rust steel is made, and is provided with active carbon, inert gas Krypton and argon under liquid nitrogen temperature after adsorbable 423 pyroreaction of titanium sponge
Gas, subsequent active carbon cryotrap 431 can be heated, and carry out first time chromatography, and helium carrier gas 432 includes helium flow path, quality stream
Meter and purifying cold-trap, high-purity helium as carrier gas by after 423 pyroreaction of titanium sponge inert gas Krypton and argon gas purging
Into chromatographic column group 433, mass flowmenter is used to control the flow velocity of helium carrier gas 432, and chromatographic column group 433 isolates Krypton and argon gas,
Quadrupole mass spectrometer 434 is located at 433 exit of chromatographic column group, the argon gas and Krypton that moment monitoring is isolated, the argon gas isolated
It is collected in measuring device 44 in inert gas respectively with Krypton and is collected and measures.
As shown in figure 5, to be disclosed in the present application a kind of for inert gas automation separation in small tolerance environmental sample
The structural schematic diagram of system embodiment 5, the system may include: de-watering apparatus 51, titanium sponge high temperature adsorption device 52, gas phase
Chromatographic separation device 53, inert gas collect measuring device 54, vacuum plant 55 and control device 56；Wherein:
Vacuum plant 55, for making system be in vacuum state；
Control device 56, for realizing the automation control of entire inert gas separation；
De-watering apparatus 51 includes rust steel container, 5A molecular sieve is housed in rustless steel container, for the control in control device 56
System is lower to remove water and carbon dioxide for small tolerance environmental sample gas by 5A molecular sieve；
Titanium sponge high temperature adsorption device 52, comprising: mass flow control meter 521, is mounted in sea at titanium sponge high temperature furnace pipe 522
Titanium sponge 523, diaphragm gauge 524 in continuous titanium high temperature furnace pipe；
Mass flow control meter 521 enters titanium sponge high temperature for controlling small tolerance environmental sample gas with preset flow velocity
Boiler tube 522；
Diaphragm gauge 524, for monitoring the air pressure of titanium sponge high temperature furnace pipe 522；
Titanium sponge 523, for removing the active gases in small tolerance environmental sample gas；
Gas-chromatography separator 53 includes: active carbon cryotrap 531, helium carrier gas 532, chromatographic column group 533 and quadrupole
Bar mass spectrograph 534；
Active carbon cryotrap 531, for collecting Krypton and argon gas in small tolerance environmental sample gas；
Helium carrier gas 532, for Krypton and argon gas to be purged into chromatographic column group 533 as carrier gas；
Chromatographic column group 533, for separating Krypton and argon gas；
Quadrupole mass spectrometer 534, for monitoring the gas componant after chromatographic column group 533；
It includes: that Krypton collects measuring device 541 and argon gas collection measuring device 542 that inert gas, which collects measuring device 54,
For collecting respectively and measuring argon gas and Krypton.
The disclosed work that isolated system is automated for inert gas in small tolerance environmental sample of above-described embodiment is former
Reason are as follows:
When needing to carry out inert gas in small tolerance environmental sample automation separation, controlled first by control device 56
Vacuum plant 55 processed makes separation system be in vacuum state, and small tolerance environmental sample gas to be separated is then passed through water removal dress
It sets in 51, de-watering apparatus 51 includes rustless steel container, and the 5A molecular sieve in rustless steel container, passes through rustless steel container
In 5A molecular sieve remove gas in water and carbon dioxide, through water removal and carbon dioxide gas mass flow control count
Under 521 control, entered in titanium sponge high temperature furnace pipe 522 with preset flow velocity (for example, flow velocity of 100~500ml/min), and
It is reacted with the titanium sponge 523 in titanium sponge high temperature furnace pipe 522, other all gas in addition to inert gas are all by titanium sponge
523 reaction absorption.Gas after removing active gases is passed through in active carbon cryotrap 531, and active carbon cryotrap 531 is not by
Rust steel is made, and is provided with active carbon, inert gas Krypton and argon under liquid nitrogen temperature after adsorbable 523 pyroreaction of titanium sponge
Gas, subsequent active carbon cryotrap 531 can be heated, and carry out first time chromatography, and helium carrier gas 532 includes helium flow path, quality stream
Meter and purifying cold-trap, high-purity helium as carrier gas by after 523 pyroreaction of titanium sponge inert gas Krypton and argon gas purging
Into chromatographic column group 533, mass flowmenter is used to control the flow velocity of helium carrier gas 532, and chromatographic column group 533 isolates Krypton and argon gas,
Quadrupole mass spectrometer 534 is located at 533 exit of chromatographic column group, the argon gas and Krypton that moment monitoring is isolated, when monitoring argon gas
When appearance, argon gas is imported into argon gas and collects measuring device 542, when detecting Krypton, Krypton imported into Krypton and collects measurement dress
Set 541.
Specifically, in the above-described embodiments, chromatographic column group may include two 5A molecular sieve chromatography columns.
Specifically, in the above-described embodiments, Krypton is collected measuring device and is made of stainless steel tube, it is provided with active carbon, is had
Vacuum valve sealing, Krypton can be adsorbed under liquid nitrogen temperature, can also individually remove from system, be collected into through gas-chromatography
Krypton can be transferred in collection vessel, Krypton collect measuring device in further include diaphragm gauge, for measuring Krypton
Content.
Specifically, in the above-described embodiments, argon gas is collected measuring device and is made of stainless steel tube, it is provided with active carbon, is had
Vacuum valve sealing, argon gas can be adsorbed under liquid nitrogen temperature, can also individually remove from system, be collected into through gas-chromatography
Argon gas can be transferred in collection vessel, argon gas collect measuring device in further include diaphragm gauge, for measuring argon gas
Content.
Specifically, in the above-described embodiments, vacuum plant includes: stainless-steel vacuum pipeline, stainless-steel vacuum adapter, true
Empty sealing element and pump group, for vacuum condition needed for generating and maintaining gas separation system.
Specifically, in the above-described embodiments, control device part is used to control the automation fortune of entire separation and Extraction process
Row includes hardware components and software section.Hardware components include: operated pneumatic valve, cylinder, pneumatic control box；It is soft in controller
Part part is the control program write based on matlab.Operated pneumatic valve includes pneumatic two-way valve, Pneumatic three-way valve, Pneumatic four-way
Valve, by whether carrying out the switch of control valve to gas.Cylinder is collected in above-mentioned all active carbon cryotraps and krypton argon to be held
All it is placed with cylinder immediately below device, the fixed cool-bag for filling liquid nitrogen in cylinder top, by the way that control whether can be with to gas to cylinder
The lifting for controlling cylinder, to control whether to give cryotrap liquid feeding nitrogen.Pneumatic control box is provided with solenoid valve, relay and
Single-chip microcontroller is the medium for connecting computer and operated pneumatic valve.The high ordinary mail number that computer control single chip computer generates can control solenoid valve
Switch, and then control the on-off of the control gas circuit of pneumatic operated valve and cylinder, the lifting of the switch and cylinder of final control valve.Control
The entire software section of software section processed includes to all diaphragm gauges, mass flowmenter, the reading of quadrupole mass spectrometer data
It completes entire separation in lower control valve switch and the cylinder lifting of meeting some requirements with storage and with this trigger signal and mentions
Take the automatic operating of process.That is, controller, which passes through, reads de-watering apparatus, titanium sponge high temperature adsorption device in control process,
Gas-chromatography separator, inert gas collect measuring device, each senser element (thermometer, film pressure in vacuum plant
Power meter, mass flowmenter, quadrupole mass spectrometer) parameter be presently in state to judge system, and issue correctly instruction and give
Pneumatic control box is to control the lifting of the switch and cylinder of each operated pneumatic valve, the final next state of control system.
In cycles with this, it is finally completed entire separation process.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
Professional further appreciates that, unit described in conjunction with the examples disclosed in the embodiments of the present disclosure
And algorithm steps, can be realized with electronic hardware, computer software, or a combination of the two, in order to clearly demonstrate hardware and
The interchangeability of software generally describes each exemplary composition and step according to function in the above description.These
Function is implemented in hardware or software actually, the specific application and design constraint depending on technical solution.Profession
Technical staff can use different methods to achieve the described function each specific application, but this realization is not answered
Think beyond scope of the present application.
The step of method described in conjunction with the examples disclosed in this document or algorithm, can directly be held with hardware, processor
The combination of capable software module or the two is implemented.Software module can be placed in random access memory (RAM), memory, read-only deposit
Reservoir (ROM), electrically programmable ROM, electrically erasable ROM, register, hard disk, moveable magnetic disc, CD-ROM or technology
In any other form of storage medium well known in field.
The foregoing description of the disclosed embodiments makes professional and technical personnel in the field can be realized or use the application.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the application.Therefore, the application
The embodiments shown herein is not intended to be limited to,
And it is to fit to the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. a kind of automate isolated system for inert gas in small tolerance environmental sample characterized by comprising water removal dress
It sets, titanium sponge high temperature adsorption device, gas-chromatography separator, inert gas collect measuring device, vacuum plant and control fill
It sets；Wherein:
The vacuum plant, for making system be in vacuum state；
The control device, for realizing the automation control of entire inert gas separation；
The de-watering apparatus, for small tolerance environmental sample gas to be removed water and titanium dioxide under the control of the control device
Carbon；
The titanium sponge high temperature adsorption device, for being removed in small tolerance environmental sample gas under the control of the control device
Active gases；
The gas-chromatography separator, for realizing argon in small tolerance environmental sample gas under the control of the control device
Gas and Krypton are automatically separated；
The inert gas collects measuring device, for collecting respectively and measuring argon gas and Krypton.
2. system according to claim 1, which is characterized in that the de-watering apparatus includes: rustless steel container, described stainless
5A molecular sieve is housed in steel container.
3. system according to claim 2, which is characterized in that the titanium sponge high temperature adsorption device includes: mass flow
Control meter, titanium sponge high temperature furnace pipe, titanium sponge and diaphragm gauge in the titanium sponge high temperature furnace pipe；Wherein:
The mass flow control meter enters the titanium sponge height for controlling small tolerance environmental sample gas with preset flow velocity
Warm boiler tube；
The diaphragm gauge, for monitoring the air pressure of the titanium sponge high temperature furnace pipe；
The titanium sponge, for removing the active gases in small tolerance environmental sample gas.
4. system according to claim 3, which is characterized in that the gas-chromatography separator includes: active carbon low temperature
Cold-trap, helium carrier gas, chromatographic column group and quadrupole mass spectrometer, in which:
The active carbon cryotrap, for collecting Krypton and argon gas in small tolerance environmental sample gas；
The helium carrier gas, for Krypton and argon gas to be purged into the chromatographic column group as carrier gas；
The chromatographic column group, for separating Krypton and argon gas；
The quadrupole mass spectrometer, for monitoring the gas componant after the chromatographic column group.
5. system according to claim 4, which is characterized in that it includes: that Krypton is received that the inert gas, which collects measuring device,
Collect measuring device and argon gas collects measuring device；Wherein:
The Krypton collects measuring device, for collecting and measuring Krypton；
The argon gas collects measuring device, for collecting and measuring argon gas.
6. system according to claim 5, which is characterized in that the vacuum plant includes: stainless-steel vacuum pipeline, stainless
Steel vacuum adapter, vacuum seal and pump group.
7. system according to claim 6, which is characterized in that the control device includes: operated pneumatic valve, cylinder, pneumatic
Control box, controller and controller.
8. system according to claim 7, which is characterized in that the operated pneumatic valve includes: pneumatic two-way valve, Pneumatic three-way
Valve, Pneumatic four-way valve.
9. system according to claim 8, which is characterized in that the chromatographic column group includes two 5A molecular sieve chromatography columns.
10. system according to claim 9, which is characterized in that the preset flow velocity is 100~500ml/min.
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| CN109323909B (en) | 2020-10-27 |
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