CN111638263B - Gas sampling analysis device and method - Google Patents
Gas sampling analysis device and method Download PDFInfo
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- 238000005070 sampling Methods 0.000 title claims abstract description 165
- 238000004458 analytical method Methods 0.000 title claims abstract description 143
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000007789 gas Substances 0.000 claims abstract description 193
- 238000004868 gas analysis Methods 0.000 claims abstract description 66
- 238000005086 pumping Methods 0.000 claims abstract description 34
- 230000001105 regulatory effect Effects 0.000 claims description 68
- 239000000203 mixture Substances 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 4
- 238000005040 ion trap Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 4
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 230000001066 destructive effect Effects 0.000 description 2
- 238000001900 extreme ultraviolet lithography Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 108010083687 Ion Pumps Proteins 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/24—Suction devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0006—Calibrating gas analysers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/24—Suction devices
- G01N2001/248—Evacuated containers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The application discloses a gas sampling analysis device and a method, wherein the device comprises the following components: the device comprises a vacuum acquisition module, a sampling module and a gas analysis module; the gas analysis module is respectively connected with the vacuum acquisition module and the sampling module; the vacuum acquisition module comprises a limiting valve, and when the limiting valve is opened and closed, the limiting valve realizes the limiting vacuum and the working vacuum of the gas analysis module respectively. Therefore, by adopting the embodiment of the application, the on-line analysis of high-pressure, normal-pressure and vacuum gases can be realized; the gas sampling amount is increased, and the response speed of the system is improved; the molecular discrimination effect and the pumping speed selectivity during gas sampling are eliminated, nondestructive sampling analysis is realized, and the self-contained calibration of the gas sampling analysis device is realized, so that the accuracy of a gas sampling analysis result is improved.
Description
Technical Field
The application relates to the technical field of measurement, in particular to a gas sampling and analyzing device and method, which can be used for sampling and component analysis of high-pressure, normal-pressure and vacuum gases.
Background
In the field of industrial production, it is often necessary to analyze the gas components, partial pressures and concentrations of various process chambers to determine whether the gas contents are within a reasonable range, and perform feedback control in time to ensure the normal operation of industrial production. For example: in urea synthesis, it is necessary to keep the ratio of ammonia and carbon dioxide in the synthesis column within a certain range, and for this purpose, it is necessary to analyze the concentrations of ammonia and carbon dioxide. This reaction is usually carried out in a high pressure environment, such as above 150 atmospheres. For another example, gas lasers have wide industrial applications, where the working medium is often a mixed gas. Working pressure range of working medium is wider, such as 2-6 atmospheres. The performance of the gas laser is closely related to the components and concentration of the working medium gas and the content of the polluting gas in the working medium, and the components and concentration of the gas in the discharge cavity of the gas laser need to be analyzed in real time. For another example, an Extreme Ultraviolet (EUV) lithography machine vacuum system includes a number of process chambers of different requirements, and the gas content in each vacuum chamber needs to be closely monitored at all times, such as the composition and partial pressure of gases such as H2O, O and CxHy. Common sampling methods are: volume sampling, sampling valves, pipelines, micropores, membrane sampling and the like, and the mixed gas can change the pressure dividing ratio in the transmission process from a high-pressure end to a low-pressure end, so that the gas components obtained by actual measurement are different from the gas source components in the process chamber, even part of trace gas is lost, and the accuracy of gas analysis is reduced.
Disclosure of Invention
The embodiment of the application provides a gas sampling analysis device and a gas sampling analysis method. The following presents a simplified summary in order to provide a basic understanding of some aspects of the disclosed embodiments. This summary is not an extensive overview and is intended to neither identify key/critical elements nor delineate the scope of such embodiments. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is presented later.
In a first aspect, an embodiment of the present application provides a gas sampling analysis apparatus, the apparatus including:
the device comprises a vacuum acquisition module, a sampling module and a gas analysis module; wherein,,
the gas analysis module is respectively connected with the vacuum acquisition module and the sampling module; wherein,,
the vacuum acquisition module comprises a limiting valve, and when the limiting valve is opened and closed, the limiting valve realizes the extreme vacuum and the working vacuum of the gas analysis module respectively; wherein,,
the flow limiting valve is a vacuum valve with a through hole with a proper size on a valve plate.
Optionally, the apparatus further includes:
a calibration module; wherein the calibration module is connected with the sampling module.
Optionally, the vacuum acquisition module comprises a flow limiting valve, a main pump, an electromagnetic valve and a backing pump; the flow limiting valve, the main pump, the electromagnetic valve and the backing pump are sequentially connected through pipelines; one end of the flow limiting valve is connected to the main pump through the pipeline, and the other end of the flow limiting valve is connected to the gas analysis module through the pipeline; wherein, the requirement of the trompil size on the restriction valve plate includes at least: (1) molecular flow pumping speed corresponding to the size of the opening meets the requirement of working vacuum pumping of the analysis chamber. (2) The molecular flow pumping speed corresponding to the opening size is not more than 25% of the pumping speed of the main pump.
Optionally, the sampling module comprises a process chamber, a valve group, a first regulating valve and a restrictor; the process chamber, the valve bank and the current limiter are sequentially connected through a sampling tube, one end of the sampling tube is inserted into the process chamber, and the other end of the sampling tube is connected with one end of the valve bank; the other end of the valve group is connected to one end of the flow restrictor through the sampling pipe; the other end of the restrictor is connected to the gas analysis module through the sampling tube; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the restrictor through a pipeline, and the other end of the first regulating valve is connected to the vacuum acquisition module through a pipeline. Optionally, the gas analysis module comprises an analysis chamber, a vacuum gauge and a gas analyzer, wherein the analysis chamber is respectively connected with the vacuum gauge and the gas analyzer through pipelines; wherein,,
the analysis chamber can also be respectively connected with the vacuum gauge and the gas analyzer through valves;
the gas analysis module at least can select a quadrupole mass spectrometer, a time-of-flight mass spectrometer and an ion trap mass spectrometer; wherein;
and heaters are arranged on the pipeline and the analysis chamber, and can bake and degas the sampling pipeline and the analysis chamber.
Optionally, the calibration module comprises a standard air source and a second regulating valve, wherein the standard air source is connected with one end of the second regulating valve through a pipeline, and the other end of the second regulating valve is connected to the valve group and the sampling tube connected with the restrictor through a pipeline; wherein the standard gas source can provide high purity standard gas for the gas analysis device, and the standard gas is a mixture of multiple gases with determined concentrations.
Optionally, the sampling module comprises a process chamber, a valve group, a first regulating valve, a vacuum pump and a restrictor; the process chamber, the valve bank and the current limiter are sequentially connected through a sampling tube, one end of the sampling tube is inserted into the process chamber, and the other end of the sampling tube is connected with one end of the valve bank; the other end of the valve group is connected to one end of the flow restrictor through the sampling pipe; the other end of the restrictor is connected to the gas analysis module through the sampling tube; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the restrictor through a pipeline, and the other end of the first regulating valve is connected to the vacuum pump through a pipeline. The flow restrictor at least adopts a capillary tube, a micropore and a fine tuning valve, and preferably adopts the capillary tube or the micropore.
Optionally, when the process cavity is filled with high-pressure or normal-pressure gas, continuous flow sampling is adopted; when the process cavity is in a vacuum environment, molecular flow sampling is adopted. Accordingly, the relation between the diameter of the sampling tube and the free path of gas molecules passing through the sampling tube is respectively:
d≥10λ(1)
d≤λ/10(2)
wherein d is the diameter of the sampling tube, and lambda is the free path of gas molecules.
Optionally, the vacuum acquisition module is used for vacuumizing the analysis chamber; the sampling module is used for acquiring gas to be detected from the analysis chamber; the gas analysis module is used for detecting and analyzing the gas to be detected in the analysis chamber; the calibration module is used for carrying out periodic calibration on the gas sampling analysis device.
In a second aspect, an embodiment of the present application provides a gas sampling analysis method, including:
closing the valve group, the first regulating valve and the second regulating valve, and opening the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve to pump the ultimate vacuum to the analysis chamber;
when the vacuum degree of the analysis chamber reaches a preset threshold value, starting a gas analysis module to monitor the analysis chamber in real time;
when the gas analysis module does not monitor the polluted gas, the gas analysis module and the flow limiting valve are closed, the valve group is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to analyze and test the sampled gas;
closing the valve group and the first regulating valve, and opening the flow limiting valve to continuously pump the device with extreme vacuum;
when the gas analysis module does not detect the polluted gas, the gas sampling analysis device is closed, so that the gas sampling analysis device is kept in a vacuum state.
The technical scheme provided by the embodiment of the application can have the following beneficial effects:
the application has the advantages that: the method comprises the steps of (1) carrying out on-line analysis on high-pressure, normal-pressure and vacuum gases, (2) increasing the gas sampling amount, improving the response speed of the system, (3) eliminating the molecular discrimination effect and the pumping speed selectivity during gas sampling, thereby realizing nondestructive sampling analysis, and (4) carrying out automatic calibration.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application as claimed.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
FIG. 1 is a schematic diagram of a gas sampling and analyzing apparatus according to an embodiment of the present application;
FIG. 2 is a schematic diagram of another gas sampling analysis apparatus according to an embodiment of the present application;
FIG. 3 is a schematic flow chart of a gas sampling analysis method according to an embodiment of the present application;
FIG. 4 is a schematic diagram of a gas sampling analysis process according to an embodiment of the present application;
Detailed Description
The following description and the drawings sufficiently illustrate specific embodiments of the application to enable those skilled in the art to practice them.
It should be understood that the described embodiments are merely some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary examples do not represent all implementations consistent with the application. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the application as detailed in the accompanying claims.
In the description of the present application, it should be understood that the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. The specific meaning of the above terms in the present application will be understood in specific cases by those of ordinary skill in the art. Furthermore, in the description of the present application, unless otherwise indicated, "a plurality" means two or more. "and/or", describes an association relationship of an association object, and indicates that there may be three relationships, for example, a and/or B, and may indicate: a exists alone, A and B exist together, and B exists alone. The character "/" generally indicates that the context-dependent object is an "or" relationship.
To date, for gas sampling analysis, common sampling methods are: volume sampling, sampling valves, pipelines, micropores, membrane sampling and the like, and the mixed gas can change the pressure dividing ratio in the transmission process from a high-pressure end to a low-pressure end, so that the gas components obtained by actual measurement are different from the gas source components in the process chamber, even part of trace gas is lost, and the accuracy of gas analysis is reduced. Accordingly, the present application has been made to solve the above-mentioned problems occurring in the related art, and provides a gas sampling analysis apparatus and method. In the technical scheme provided by the application, the valve group, the first regulating valve and the second regulating valve are closed, and the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve are opened to pump the ultimate vacuum to the analysis chamber; when the vacuum degree of the analysis chamber reaches a preset threshold value, starting a gas analysis module to monitor the analysis chamber in real time; when the gas analysis module does not monitor the polluted gas, the gas analysis module and the flow limiting valve are closed, the valve group is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to analyze and test the sampled gas; closing the valve group and the first regulating valve, and opening the flow limiting valve to continuously pump the device with extreme vacuum; when the gas analysis module does not detect the polluted gas, the gas sampling analysis device is closed to maintain the vacuum state, so that the accuracy of gas sampling analysis is improved, and the following description is made by adopting an exemplary embodiment.
Referring to fig. 1, fig. 1 is a schematic diagram of an apparatus for gas sampling and analyzing apparatus according to an embodiment of the present application, the apparatus includes a vacuum acquisition module, a sampling module, a gas analyzing module, and a calibration module, wherein the vacuum acquisition module includes a flow limiting valve 8, a main pump 9, an electromagnetic valve 10, and a backing pump 11, wherein the flow limiting valve 8, the main pump 9, the electromagnetic valve 10, and the backing pump 11 are sequentially connected through a pipeline, one end of the flow limiting valve 8 is connected to the main pump 9 through a pipeline, and the other end is connected to the gas analyzing module through a pipeline. The sampling module comprises a process chamber, a valve group, a first regulating valve and a current limiter, wherein the process chamber 1, the valve group 3 and the current limiter 4 are sequentially connected through a sampling pipe 2, one end of the sampling pipe 2 is inserted into the process chamber 1, the other end of the sampling pipe is connected with one end of the valve group 3, the other end of the valve group 3 is connected with one end of the current limiter 4 through the sampling pipe 2, and the other end of the current limiter 4 is connected with the gas analysis module through the sampling pipe; one end of the first regulating valve 12 is connected to the valve block 3 and a sampling pipe connected to the restrictor 4 through a pipe, and the other end of the first regulating valve 12 is connected to the backing pump 11 and a pipe connected to the solenoid valve 10 through a pipe. The gas analysis module comprises an analysis chamber 5, a vacuum gauge 6 and a gas analyzer 7, wherein the analysis chamber 5 is respectively connected with the vacuum gauge 6 and the gas analyzer 7 through pipelines. The calibration module comprises a standard air source 13 and a second regulating valve 14, wherein the standard air source 13 is connected with one end of the second regulating valve 14 through a pipeline, and the other end of the second regulating valve 14 is connected to a sampling pipe connected with the valve bank 3 and the restrictor 4 through a pipeline.
Specifically, the process chamber 1 is a container to be measured for gas components, such as an excimer laser discharge chamber, a synthesis tower in urea industry, a vacuum chamber of an Extreme Ultraviolet (EUV) lithography machine, and the like, and may be other high-pressure, normal-pressure and vacuum containers.
Specifically, one end of the sampling tube 2 extends into the process chamber 1 for sampling at a designated position, and the other end is connected with the valve 3, so that the gas in the process chamber 1 is conveyed to the device. In order to reduce the background of the device as much as possible, the material of the sampling tube 2 is preferably stainless steel or quartz glass, and silicon-based materials or other materials can be selected. In addition, the gas flow regime in the sampling tube 2 should be a continuous flow, a slip flow or a molecular flow, avoiding transitional flows as much as possible in order to achieve a non-destructive sampling. For high pressure or normal pressure gases, continuous flow sampling is recommended; for vacuum environments, molecular flow sampling is recommended. Accordingly, for continuous and molecular flows, the diameter d of the sampling tube 2 and the gas molecular free path λ propose to satisfy the relation:
d≥10λ(1)
d≤λ/10(2)
specifically, the valve group 3 is used for realizing gas decompression and on-off of a sampling pipeline, and a decompression valve, a ball valve, a needle valve, a bellows stop valve, a combination thereof and the like can be adopted according to different air pressures of the process cavity 1.
In particular, the restrictor 4 is designed to limit the flow of gas and to reduce the intake air flow and the vacuum pressure of the analysis chamber 5. On the other hand, molecular flow sampling of the gas is to be achieved in order to achieve non-destructive sampling. The restrictor 4 is preferably a capillary tube or a micropore, and may be a fine tuning valve, etc., and the material is preferably stainless steel or quartz glass, and may be a silicon-based material or other materials.
Specifically, the analysis chamber 5 communicates with the flow restrictor 4, and is further equipped with a vacuum gauge 6, a gas analyzer 7, and a flow restrictor valve 8. The analysis chamber 5 is typically made of stainless steel or aluminum alloy material. The microsampled gas of the restrictor 4 enters the analysis chamber 5 and is pumped away by the main pump 9 through the restrictor valve 8 to create a suitable vacuum in the analysis chamber 5. The vacuum gauge 6 can measure the vacuum level of the analysis chamber 5 and provide data to the control system. The gas analysis module 7 is used for measuring and analyzing the gas component in the analysis chamber 5, and can be a quadrupole mass spectrometer, a time-of-flight mass spectrometer,Ion trap mass spectrometers or other gas analysis instruments, etc. Generally, the gas analyzer 7 needs to operate in a suitable vacuum environment, so the operating vacuum of the analysis chamber 5 is in the range of 10 +2 ～10 -5 Pa range.
Specifically, one end of the restrictor valve 8 is connected to the analysis chamber 5, and the other end is connected to the main pump 9. The restrictor valve 8 is a vacuum valve with a properly sized through hole in the valve plate and requires special design and manufacture. The main pump 9 is used for pumping the analysis chamber 5 with a limiting vacuum or working vacuum, and may be a molecular pump, an ion pump or other oil-free vacuum pump. When the valve plate of the restrictor valve 8 is opened, the main pump 9 is fully communicated with the analysis chamber 5, the true pump 9 has the maximum pumping speed for the analysis chamber 5, and can pump the ultimate vacuum for the analysis chamber 5. The ultimate vacuum is generally 10 -5 ～10 -9 Pa. When the valve plate of the restrictor valve 8 is closed, the main pump 9 communicates with the analysis chamber 5 through an opening in the valve plate of the restrictor valve 8, the pumping rate of which depends on the opening size, for pumping a working vacuum to the analysis chamber 5. Generally, the size of the opening in the valve plate should satisfy both requirements: (1) molecular flow pumping speed corresponding to the opening size meets the requirement of the analysis chamber 5 for pumping working vacuum. (2) The molecular flow pumping speed corresponding to the opening size is not more than 25% of the pumping speed of the main pumping pump 9 so as to shield the pumping speed fluctuation and selectivity of the main pumping pump 9, thereby realizing stable nondestructive sampling analysis.
Specifically, the backing pump 11 is connected to the main pump 9 through a solenoid valve 10 for drawing a backing vacuum for the main pump 9. Furthermore, the backing pump 11 is connected to the gas line between the valve block 3 and the restrictor 4 via a first regulating valve 12. By adjusting the opening of the first regulating valve 12, a desired front-end air pressure or vacuum can be provided to the restrictor 4. The backing pump 11 may be a Roots pump, a screw pump, a scroll dry pump, or the like.
In particular, the standard gas source 13 is connected to the gas conduit between the valve block 3 and the restrictor 4 by means of a second regulating valve 14. The standard gas source 13 is used to provide a high purity standard gas for the gas analysis device, which is a mixture of gases having a certain concentration, such as Kr: ar: ne: he=20: 10:2:1. by adjusting the opening degree of the second regulating valve 14, an appropriate amount of standard gas can be introduced.
Specifically, a heater is provided in the sampling pipe and the analysis chamber 5 of the gas sampling analysis apparatus. The heater can bake and degas the sampling pipe and the analysis chamber 5 to obtain a good system background and improve the accuracy of gas analysis. In addition, the heater toasts and deaerates the analysis chamber 5, and can eliminate or reduce contamination of the analysis chamber by hydrocarbons and the like.
In particular, the gas sampling analysis apparatus requires periodic calibration to ensure accuracy and repeatability of the analysis results. In the gas sampling analysis apparatus of fig. 1, a standard gas source 13 is connected to a gas pipe between the valve block 3 and the restrictor 4 through a second regulating valve 14. When the gas sampling analysis device is calibrated, the standard gas is introduced into the analysis chamber 5 through the second regulating valve 14 and the restrictor 4 by adopting steps similar to a gas test flow, and the standard gas is analyzed by the gas analyzer 7. If the analyzed gas components and concentrations are consistent with the standard gas, it means that the gas sampling analysis apparatus can perform gas analysis by calibration. If the analyzed gas components and concentrations are inconsistent with the standard gas, the gas sampling analysis device is required to be debugged until the calibration requirement is met. The tuning process of the gas sampling analysis apparatus may be bake heating, system pumping background, or adjusting parameters of the gas analyzer 7, etc.
Specifically, in fig. 1 of the gas sampling analysis apparatus, a backing pump 11 is connected to a main pump 9 through a solenoid valve 10, and is used for pumping backing vacuum for the main pump 9; on the other hand, the first regulating valve 12 is connected with the gas pipeline between the valve group 3 and the restrictor 4, so as to provide the front end air pressure or vacuum degree required for the restrictor 4. When the process chambers 1 are at different pressures or vacuum levels, a single backing pump 11 may not be well compatible with both of these needs. A vacuum pump 15 may be added to achieve the two requirements, respectively, as shown in fig. 2, and the gas sampling analysis apparatus differs from the gas sampling analysis apparatus of fig. 1 in that the gas sampling analysis apparatus of fig. 2 includes a process chamber, a valve block, a first regulating valve, a vacuum pump, and a flow restrictor; the process chamber 1, the valve bank 3 and the flow restrictor 4 are sequentially connected through sampling pipes, one end of each sampling pipe is inserted into the process chamber 1, and the other end of each sampling pipe is connected with one end of the valve bank 3; the other end of the valve group 3 is connected to one end of a flow restrictor 4 through a sampling pipe; the other end of the restrictor 4 is connected to a gas analysis module through a sampling tube; one end of the first regulating valve 12 is connected to the valve block 3 and the sampling tube connected to the restrictor 4 through a pipe, and the other end of the first regulating valve 12 is connected to the vacuum pump 16 through a pipe.
Specifically, the backing pump 11 is connected with the main pump 9 through the electromagnetic valve 10 and is used for pumping backing vacuum for the main pump 9; a vacuum pump 16 is connected to the gas conduit between the valve block 3 and the restrictor 4 via a first regulating valve 12 for providing the restrictor 4 with the desired front end gas pressure or vacuum.
In the embodiment of the application, the valve group, the first regulating valve and the second regulating valve are closed, and the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve are opened to pump the ultimate vacuum to the analysis chamber; when the vacuum degree of the analysis chamber reaches a preset threshold value, starting a gas analysis module to monitor the analysis chamber in real time; when the gas analysis module does not monitor the polluted gas, the gas analysis module and the flow limiting valve are closed, the valve group is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to analyze and test the sampled gas; closing the valve group and the first regulating valve, and opening the flow limiting valve to continuously pump the device with extreme vacuum; when the gas analysis module does not detect the polluted gas, the gas sampling analysis device is closed, so that the gas sampling analysis device is kept in a vacuum state. The application has the advantages that: the method comprises the steps of (1) carrying out on-line analysis on high-pressure, normal-pressure and vacuum gases, (2) increasing the gas sampling amount, improving the response speed of the system, (3) eliminating the molecular discrimination effect and the pumping speed selectivity during gas sampling, thereby realizing nondestructive sampling analysis, and (4) carrying out automatic calibration.
Referring to fig. 3, a flow chart of a gas sampling analysis method applied to a gas sampling analysis device is provided in an embodiment of the application. As shown in fig. 3, the method according to the embodiment of the present application may include the following steps:
s101, closing a valve group, a first regulating valve and a second regulating valve, and opening a vacuum gauge, a backing pump, an electromagnetic valve, a main pumping valve and a flow limiting valve to pump extreme vacuum to an analysis chamber;
in one possible implementation, the analysis chamber 5 is evacuated by closing the valve block 3, the first regulating valve 12 and the second regulating valve 14, then opening the vacuum gauge 6, opening the backing pump 11, the solenoid valve 10 and the restrictor valve 8. When the analysis chamber 5 reaches a suitable vacuum level (e.g. less than 200 Pa), the main pump 9 is turned on. And after the vacuum degree in the analysis chamber 5 meets the requirement, starting the gas analysis module 7 to monitor the background of the system in real time.
S102, when the vacuum degree of an analysis chamber reaches a preset threshold value, starting a gas analysis module to monitor the analysis chamber in real time;
in one possible implementation, if the gas analyzer 7 detects that the system background is clean, no contaminating gas, a vacuum is continuously pulled until a good system background is obtained and background data is recorded. Otherwise, the heater 15 is turned on to bake and degas the device to eliminate or mitigate contamination until a good system background is achieved.
S103, when the gas analysis module does not monitor the polluted gas, closing the gas analysis module and the flow limiting valve, opening the valve group and adjusting the first regulating valve until the analysis chamber obtains working vacuum, and then opening the gas analysis module to analyze and test the sampled gas;
in one possible implementation, after a good system background is obtained, the gas analyzer 7 is closed, the restrictor valve 8 is closed, the valve block 3 is opened, and the first regulator valve 12 is adjusted until the analysis chamber 5 obtains a suitable vacuum. The gas analyzer 7 is turned on, an analytical test is performed on the sampled gas, and data is recorded.
S104, closing the valve group and the first regulating valve, and opening the flow limiting valve to continuously pump the device with extreme vacuum;
in one possible implementation, after the gas analysis is completed, the valve block 3 and the first regulating valve 12 are closed, the restrictor valve 8 is opened, and the evacuation of the device is continued. If the gas analyzer 7 monitors that the system is free of contaminating gases, a vacuum is continuously pulled until a good system background is obtained. Otherwise, the heater 15 is turned on to bake and degas the device to eliminate or mitigate contamination until a good system background is achieved.
S105, when the gas analysis module does not monitor the polluted gas, the gas sampling analysis device is closed, so that the gas sampling analysis device is kept in a vacuum state.
In one possible implementation, after the sample gas is exhausted, the gas sampling analysis device is turned off to maintain the vacuum state, so that a good system background is obtained in the next test. The gas sampling analysis apparatus may also be filled with a high purity protective gas, such as 99.999% nitrogen.
For example, as shown in fig. 4, a typical operational flow of a gas sampling analysis device includes first a system bleed background, then a gas sampling analysis, then a sampled gas bleed, and finally closing the device.
Further, the gas sampling analysis apparatus needs to be calibrated periodically to ensure accuracy and repeatability of analysis results. In the case of periodic calibration of a gas sampling apparatus such as that shown in fig. 1, a standard gas source 13 is connected to the gas line between the valve block 3 and the restrictor 4 via a second regulator valve 14. In a similar procedure to the gas test flow, the standard gas is first introduced into the analysis chamber 5 through the second regulating valve 14 and the restrictor 4, and is analyzed by the gas analyzer 7, and if the analyzed gas components and concentrations are consistent with the standard gas, it means that the gas sampling analysis device can perform gas analysis by calibration. If the analyzed gas components and concentrations are inconsistent with the standard gas, the gas sampling analysis device is required to be debugged until the calibration requirement is met. The tuning process of the gas sampling analysis apparatus may be bake heating, system pumping background, or adjusting parameters of the gas analyzer 7, etc.
In the embodiment of the application, the valve group, the first regulating valve and the second regulating valve are closed, and the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve are opened to pump the ultimate vacuum to the analysis chamber; when the vacuum degree of the analysis chamber reaches a preset threshold value, starting a gas analysis module to monitor the analysis chamber in real time; when the gas analysis module does not monitor the polluted gas, the gas analysis module and the flow limiting valve are closed, the valve group is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to analyze and test the sampled gas; closing the valve group and the first regulating valve, and opening the flow limiting valve to continuously pump the device with extreme vacuum; when the gas analysis module does not detect the polluted gas, the gas sampling analysis device is closed, so that the gas sampling analysis device is kept in a vacuum state. The application has the advantages that: the method comprises the steps of (1) carrying out on-line analysis on high-pressure, normal-pressure and vacuum gases, (2) increasing the gas sampling amount, improving the response speed of the system, (3) eliminating the molecular discrimination effect and the pumping speed selectivity during gas sampling, thereby realizing nondestructive sampling analysis, and (4) carrying out automatic calibration.
Those skilled in the art will appreciate that implementing all or part of the above-described methods in the embodiments may be accomplished by computer programs stored in a computer-readable storage medium, which when executed, may include the steps of the embodiments of the methods described above. The storage medium may be a magnetic disk, an optical disk, a read-only memory, a random access memory, or the like.
The foregoing disclosure is illustrative of the present application and is not to be construed as limiting the scope of the application, which is defined by the appended claims.
Claims (10)
1. A gas sampling analysis apparatus, the apparatus comprising:
the device comprises a vacuum acquisition module, a sampling module and a gas analysis module; wherein,,
the gas analysis module is respectively connected with the vacuum acquisition module and the sampling module; wherein,,
the vacuum acquisition module comprises a limiting valve, and when the limiting valve is opened and closed, the limiting valve realizes the extreme vacuum and the working vacuum of the gas analysis module respectively; wherein,,
the flow limiting valve is a vacuum valve with a through hole with a proper size on a valve plate; wherein,,
the requirements for the size of the opening in the valve plate of the restrictor valve at least comprise: the molecular flow pumping speed corresponding to the opening size meets the requirement of the analysis chamber for pumping working vacuum, and the molecular flow pumping speed corresponding to the opening size is not more than 25% of the pumping speed of the main pumping pump.
2. A gas sampling analysis apparatus according to claim 1, wherein the apparatus further comprises:
a calibration module; wherein the calibration module is connected with the sampling module.
3. A gas sampling analysis apparatus according to claim 2, wherein,
the vacuum acquisition module comprises a flow limiting valve, a main pump, an electromagnetic valve and a backing pump; the flow limiting valve, the main pump, the electromagnetic valve and the backing pump are sequentially connected through pipelines; one end of the flow limiting valve is connected to the main pump through the pipeline, and the other end of the flow limiting valve is connected to the gas analysis module through the pipeline.
4. A gas sampling analysis apparatus according to claim 3, wherein,
the sampling module comprises a process chamber, a valve group, a first regulating valve and a flow restrictor; the process chamber, the valve bank and the current limiter are sequentially connected through a sampling tube, one end of the sampling tube is inserted into the process chamber, and the other end of the sampling tube is connected with one end of the valve bank; the other end of the valve group is connected to one end of the flow restrictor through the sampling pipe; the other end of the restrictor is connected to the gas analysis module through the sampling tube; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the restrictor through a pipeline, and the other end of the first regulating valve is connected to the vacuum acquisition module through a pipeline.
5. A gas sampling analysis apparatus according to claim 4, wherein,
the gas analysis module comprises an analysis chamber, a vacuum gauge and a gas analyzer, wherein the analysis chamber is respectively connected with the vacuum gauge and the gas analyzer through pipelines; wherein,,
the analysis chamber can also be respectively connected with the vacuum gauge and the gas analyzer through valves;
the gas analysis module at least can select a quadrupole mass spectrometer, a time-of-flight mass spectrometer and an ion trap mass spectrometer; wherein;
and heaters are arranged on the pipeline and the analysis chamber, and can bake and degas the sampling pipeline and the analysis chamber.
6. A gas sampling analysis apparatus according to claim 4, wherein,
the calibration module comprises a standard air source and a second regulating valve, wherein the standard air source is connected with one end of the second regulating valve through a pipeline, and the other end of the second regulating valve is connected to the valve group and the sampling pipe connected with the restrictor through a pipeline; wherein the standard gas source can provide high purity standard gas for the gas analysis device, and the standard gas is a mixture of multiple gases with determined concentrations.
7. A gas sampling analysis apparatus according to claim 4, wherein,
the sampling module comprises a process chamber, a valve group, a first regulating valve, a vacuum pump and a flow restrictor; the process chamber, the valve bank and the current limiter are sequentially connected through a sampling tube, one end of the sampling tube is inserted into the process chamber, and the other end of the sampling tube is connected with one end of the valve bank; the other end of the valve group is connected to one end of the flow restrictor through the sampling pipe; the other end of the restrictor is connected to the gas analysis module through the sampling tube; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the restrictor through a pipeline, and the other end of the first regulating valve is connected to a vacuum pump through a pipeline; the flow restrictor at least adopts a capillary tube, a micropore and a fine tuning valve, and preferably adopts the capillary tube or the micropore.
8. A gas sampling analysis apparatus according to any one of claims 4 to 7, wherein,
when the process cavity is filled with high-pressure or normal-pressure gas, continuous flow sampling is adopted; when the process cavity is in a vacuum environment, sampling by adopting molecular flow; accordingly, the relation between the diameter of the sampling tube and the free path of gas molecules passing through the sampling tube is respectively:
（1）
（2）
wherein d is the diameter of the sampling tube,is a free path of gas molecules.
9. A gas sampling analysis apparatus according to claim 5, said vacuum acquisition module being adapted to evacuate said analysis chamber; the sampling module is used for acquiring gas to be detected from the analysis chamber; the gas analysis module is used for detecting and analyzing the gas to be detected in the analysis chamber; the calibration module is used for carrying out periodic calibration on the gas sampling analysis device.
10. A method of gas sampling analysis using the apparatus of any one of claims 1-9, the method comprising:
closing the valve group, the first regulating valve and the second regulating valve, and opening the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve to pump the ultimate vacuum to the analysis chamber; the flow limiting valve is a vacuum valve with a through hole with a proper size on a valve plate; wherein, the requirement of the trompil size on the restriction valve plate includes at least: the molecular flow pumping speed corresponding to the opening size meets the requirement of the analysis chamber for pumping working vacuum, and the molecular flow pumping speed corresponding to the opening size does not exceed 25% of the pumping speed of the main pumping pump;
when the vacuum degree of the analysis chamber reaches a preset threshold value, starting a gas analysis module to monitor the analysis chamber in real time;
when the gas analysis module does not monitor the polluted gas, the gas analysis module and the flow limiting valve are closed, the valve group is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to analyze and test the sampled gas;
closing the valve group and the first regulating valve, and opening the flow limiting valve to continuously pump the device with extreme vacuum;
when the gas analysis module does not detect the polluted gas, the gas sampling analysis device is closed, so that the gas sampling analysis device is kept in a vacuum state.
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