阅读说明：本技术 一种气体采样分析装置和方法 (Gas sampling and analyzing device and method ) 是由 王魁波 吴晓斌 罗艳 谢婉露 于 2020-05-19 设计创作，主要内容包括：本发明公开了一种气体采样分析装置和方法,所述装置包括：真空获取模块、采样模块和气体分析模块；其中,所述气体分析模块分别与所述真空获取模块、和采样模块连接；其中,所述真空获取模块包括限流阀,所述限流阀开启和关闭时,分别实现所述气体分析模块的极限真空和工作真空。因此,采用本申请实施例,可以实现对高压、常压和真空气体进行在线分析；增加气体采样量,提高系统响应速度；消除了气体采样时的分子歧视效应和抽速选择性,实现无损采样分析以及实现气体采样分析装置自带校准,从而提高气体采样分析结果的准确度。(The invention discloses a gas sampling and analyzing device and a method, wherein the device comprises: 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 flow limiting valve, and when the flow limiting valve is opened and closed, the limiting vacuum and the working vacuum of the gas analysis module are respectively realized. Therefore, the online analysis of high-pressure, normal-pressure and vacuum gases can be realized by adopting the embodiment of the application; 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, the nondestructive sampling analysis is realized, the self calibration of a gas sampling analysis device is realized, and the accuracy of a gas sampling analysis result is improved.)

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 content of the first and second substances,

the gas analysis module is respectively connected with the vacuum acquisition module and the sampling module; wherein the content of the first and second substances,

the vacuum acquisition module comprises a flow limiting valve, and when the flow limiting valve is opened and closed, the ultimate vacuum and the working vacuum of the gas analysis module are respectively realized; wherein the content of the first and second substances,

the flow limiting valve is a vacuum valve with a through hole with a proper size formed in a valve plate.

2. A gas sampling analysis apparatus according to claim 1, the apparatus further comprising:

a calibration module; wherein the calibration module is connected with the sampling module.

3. A gas sampling analysis apparatus according to claim 1 or 2,

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 pumping 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 demand of the trompil size on the restriction valve plate includes at least: firstly, the molecular flow pumping speed corresponding to the size of the opening meets the requirement of the vacuum pumping of the analysis chamber. And the pumping speed of the molecular flow corresponding to the size of the opening is not more than 25 percent of the pumping speed of the main pump.

4. A gas sampling analysis apparatus according to claim 3,

the sampling module comprises a process chamber, a valve group, a first regulating valve and a current limiter; the process chamber, the valve group and the flow restrictor are sequentially connected through a sampling pipe, one end of the sampling pipe is inserted into the process chamber, and the other end of the sampling pipe is connected with one end of the valve group; 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 flow restrictor is connected to the gas analysis module through the sampling pipe; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the flow 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,

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 content of the first and second substances,

the analysis chamber can also be respectively connected with the vacuum gauge and the gas analyzer through valves;

wherein, the gas analysis module can at least select a quadrupole mass spectrometer, a time-of-flight mass spectrometer and an ion trap mass spectrometer; wherein;

heaters are arranged on the pipeline and the analysis chamber, and the heaters can bake and degas the sampling pipeline and the analysis chamber.

6. A gas sampling analysis apparatus according to claim 4,

the calibration module comprises a standard gas source and a second regulating valve, the standard gas 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 bank and the sampling pipe connected with the flow 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 a plurality of gases with determined concentration.

7. A gas sampling analysis apparatus according to claim 4,

the sampling module comprises a process chamber, a valve group, a first regulating valve, a vacuum pump and a current limiter; the process chamber, the valve group and the flow restrictor are sequentially connected through a sampling pipe, one end of the sampling pipe is inserted into the process chamber, and the other end of the sampling pipe is connected with one end of the valve group; 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 flow restrictor is connected to the gas analysis module through the sampling pipe; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the flow restrictor through a pipeline, and the other end of the first regulating valve is connected to a vacuum pump through a pipeline. Wherein, the flow restrictor at least adopts a capillary tube, a micropore and a trim valve, and preferentially adopts the capillary tube or the micropore.

8. A gas sampling analysis device according to any one of claims 4 to 7,

when the process cavity is filled with high-pressure or normal-pressure gas, continuous flow sampling is adopted; and when the process cavity is in a vacuum environment, molecular flow sampling is adopted. Accordingly, the diameters of the sampling pipes and the free paths of the gas molecules passing through the sampling pipes are respectively as follows:

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.

9. A gas sampling analysis apparatus according to claim 5, wherein the vacuum acquisition module is configured to evacuate the analysis chamber; the sampling module is used for acquiring the gas to be detected in 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 periodically calibrating the gas sampling and analyzing device.

10. A method of gas sampling analysis using the apparatus of any one of claims 1 to 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 carry out ultimate vacuum pumping on 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 polluting gas, the gas analysis module and the flow limiting valve are closed, the valve bank is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to carry out analysis test on the sampled gas;

closing the valve group and the first regulating valve, and opening the flow limiting valve to continue to carry out ultimate vacuum pumping on the device;

and when the gas analysis module does not monitor the polluting gas, closing the gas sampling analysis device to keep the gas sampling analysis device in a vacuum state.

Technical Field

The invention relates to the technical field of measurement, in particular to a gas sampling and analyzing device and a gas sampling and analyzing method, which can be used for sampling and component analysis of high-pressure, normal-pressure and vacuum gases.

Background

In the industrial production field, 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 to perform feedback control in time to ensure the normal operation of the industrial production. For example: in the synthesis of urea, the ratio of ammonia and carbon dioxide in the synthesis column needs to be maintained within a certain range, and for this purpose, the concentrations of ammonia and carbon dioxide need to be analyzed. This reaction is typically carried out under high pressure, e.g., above 150 atmospheres. For another example, gas lasers have been widely used in industry, and their working medium is often mixed gas. The working pressure range of the working medium is wide, such as 2-6 atmospheric pressures. 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 a discharge cavity of the gas laser need to be analyzed in real time. For another example, an Extreme Ultraviolet (EUV) lithography vacuum system includes a plurality of process chambers with different requirements, and the gas content in each vacuum chamber, such as the composition and partial pressure of H2O, O2, CxHy, and other gases, needs to be closely monitored at any time. Common sampling methods are: volume sampling method, sampling valve, pipeline, micropore and membrane sampling etc. the change of partial pressure ratio can take place for the mixed gas in the transmission process from high-pressure end to low-pressure end, makes the gas composition that actual measurement obtained and the air supply composition in the process cavity are different, and partial trace gas loses even to lead to having reduced the degree of accuracy of gas analysis.

Disclosure of Invention

The embodiment of the application provides a gas sampling and analyzing device and 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, including:

the device comprises a vacuum acquisition module, a sampling module and a gas analysis module; wherein the content of the first and second substances,

the gas analysis module is respectively connected with the vacuum acquisition module and the sampling module; wherein the content of the first and second substances,

the vacuum acquisition module comprises a flow limiting valve, and when the flow limiting valve is opened and closed, the ultimate vacuum and the working vacuum of the gas analysis module are respectively realized; wherein the content of the first and second substances,

the flow limiting valve is a vacuum valve with a through hole with a proper size formed in a valve plate.

Optionally, the apparatus further comprises:

a calibration module; wherein the calibration module is connected with the sampling module.

Optionally, the vacuum obtaining module includes a flow limiting valve, a main pump, an electromagnetic valve, and a backing pump; the flow limiting valve, the main pumping 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 demand of the trompil size on the restriction valve plate includes at least: firstly, the molecular flow pumping speed corresponding to the size of the opening meets the requirement of the vacuum pumping of the analysis chamber. And the pumping speed of the molecular flow corresponding to the size of the opening is not more than 25 percent of the pumping speed of the main pump.

Optionally, the sampling module comprises a process chamber, a valve set, a first regulating valve and a flow restrictor; the process chamber, the valve group and the flow restrictor are sequentially connected through a sampling pipe, one end of the sampling pipe is inserted into the process chamber, and the other end of the sampling pipe is connected with one end of the valve group; 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 flow restrictor is connected to the gas analysis module through the sampling pipe; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the flow 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 includes an analysis chamber, a vacuum gauge and a gas analyzer, and the analysis chamber is respectively connected to the vacuum gauge and the gas analyzer through a pipe; wherein the content of the first and second substances,

the analysis chamber can also be respectively connected with the vacuum gauge and the gas analyzer through valves;

wherein, the gas analysis module can at least select a quadrupole mass spectrometer, a time-of-flight mass spectrometer and an ion trap mass spectrometer; wherein;

heaters are arranged on the pipeline and the analysis chamber, and the heaters can bake and degas the sampling pipeline and the analysis chamber.

Optionally, the calibration module includes a standard gas source and a second regulating valve, the standard gas source is connected to one end of the second regulating valve through a pipeline, and the other end of the second regulating valve is connected to the valve block and the sampling pipe connected to the flow 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 a plurality of gases with determined concentration.

Optionally, the sampling module includes a process chamber, a valve set, a first regulating valve, a vacuum pump, and a flow restrictor; the process chamber, the valve group and the flow restrictor are sequentially connected through a sampling pipe, one end of the sampling pipe is inserted into the process chamber, and the other end of the sampling pipe is connected with one end of the valve group; 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 flow restrictor is connected to the gas analysis module through the sampling pipe; one end of the first regulating valve is connected to the valve group and the sampling pipe connected with the flow restrictor through a pipeline, and the other end of the first regulating valve is connected to a vacuum pump through a pipeline. Wherein, the flow restrictor at least adopts a capillary tube, a micropore and a trim valve, and preferentially adopts the capillary tube or the micropore.

Optionally, when the process chamber is filled with high-pressure or normal-pressure gas, continuous flow sampling is adopted; and when the process cavity is in a vacuum environment, molecular flow sampling is adopted. Accordingly, the diameters of the sampling pipes and the free paths of the gas molecules passing through the sampling pipes are respectively as follows:

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 obtaining module is configured to evacuate the analysis chamber; the sampling module is used for acquiring the gas to be detected in 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 periodically calibrating the gas sampling and analyzing 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 carry out ultimate vacuum pumping on 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 polluting gas, the gas analysis module and the flow limiting valve are closed, the valve bank is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to carry out analysis test on the sampled gas;

closing the valve group and the first regulating valve, and opening the flow limiting valve to continue to carry out ultimate vacuum pumping on the device;

and when the gas analysis module does not monitor the polluting gas, closing the gas sampling analysis device to keep the gas sampling analysis device 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: (1) the method can be used for carrying out online analysis on high-pressure, normal-pressure and vacuum gases, (2) increasing the gas sampling amount and improving the response speed of a system, (3) eliminating the molecular discrimination effect and the pumping speed selectivity during gas sampling so as to realize 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 invention, as claimed.

Drawings

The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.

Fig. 1 is a schematic diagram of an apparatus for gas sampling analysis provided in an embodiment of the present application;

FIG. 2 is a schematic diagram of another gas sampling analysis apparatus provided in 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 disclosure;

FIG. 4 is a process diagram of a gas sampling analysis process provided by an embodiment of the present application;

Detailed Description

The following description and the drawings sufficiently illustrate specific embodiments of the invention to enable those skilled in the art to practice them.

It should be understood that the described embodiments are only some embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the invention, as detailed in the appended claims.

In the description of the present invention, it is to 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 meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art. In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified. "and/or" describes the association relationship of the associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.

To date, common sampling methods for gas sampling analysis are: volume sampling method, sampling valve, pipeline, micropore and membrane sampling etc. the change of partial pressure ratio can take place for the mixed gas in the transmission process from high-pressure end to low-pressure end, makes the gas composition that actual measurement obtained and the air supply composition in the process cavity are different, and partial trace gas loses even to lead to having reduced the degree of accuracy of gas analysis. Accordingly, the present application provides a gas sampling analysis apparatus and method to solve the above-mentioned problems associated with the related art. In the technical scheme provided by the application, the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve are opened to carry out ultimate vacuum pumping on the analysis chamber by closing the valve group, the first regulating valve and the second regulating valve; 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 polluting gas, the gas analysis module and the flow limiting valve are closed, the valve bank is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to carry out analysis test on the sampled gas; closing the valve group and the first regulating valve, and opening the flow limiting valve to continue to carry out ultimate vacuum pumping on the device; when the gas analysis module does not monitor the polluting gas, the gas sampling analysis device is turned off to keep the gas sampling analysis device in a vacuum state, so that the accuracy of gas sampling analysis is improved, and the following detailed description is given by using an exemplary embodiment.

Referring to fig. 1, fig. 1 is a schematic diagram of an apparatus of a gas sampling analysis apparatus provided in an embodiment of the present application, the apparatus includes a vacuum obtaining module, a sampling module, a gas analysis module, and a calibration module, where the vacuum obtaining module includes a current limiting valve 8, a main pump 9, an electromagnetic valve 10, and a backing pump 11, where the current 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 current limiting valve 8 is connected to the main pump 9 through a pipeline, and the other end is connected to the gas analysis 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 to one end of the current limiter 4 through the sampling pipe 2, and the other end of the current limiter 4 is connected to 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 flow restrictor 4 through a pipeline, and the other end of the first regulating valve 12 is connected to a forepump 11 and a pipeline connected to the solenoid valve 10 through a pipeline. 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 gas source 13 and a second regulating valve 14, wherein the standard gas 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 group 3 and the flow restrictor 4 through a pipeline.

Specifically, the process chamber 1 is a container to be tested for gas components, such as an excimer laser discharge chamber, a synthesis tower in the 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 pipe 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 sampling tube 2 is preferably made of stainless steel or quartz glass, and may also be made of silicon-based material or other materials. In addition, the gas flow state in the sampling pipe 2 should be continuous flow, slip flow or molecular flow, and transition flow is avoided as much as possible so as to realize nondestructive sampling. For high or atmospheric pressure gases, continuous flow sampling is suggested; for vacuum environments, molecular flow sampling is suggested. Accordingly, the diameter d of the sampling tube 2 and the gas molecular free path λ are proposed to satisfy the relation:

d≥10λ(1)

d≤λ/10(2)

specifically, the valve group 3 is used for realizing the on-off of gas pressure reduction and sampling pipelines, and a pressure reducing valve, a ball valve, a needle valve, a bellows stop valve, a combination of the two and the like can be adopted according to different air pressures of the process cavity 1.

In particular, the flow restrictor 4 is intended to achieve a gas flow restriction, reducing the inlet flow and the evacuation pressure of the analysis chamber 5. On the other hand, molecular flow sampling of the gas is realized, so that lossless sampling is realized. The flow restrictor 4 is preferably a capillary or a micro-porous, but also a micro-valve or the like, and is preferably made of stainless steel or quartz glass, or a silicon-based material or other materials.

In particular, the analysis chamber 5 communicates with a flow restrictor 4, on which a vacuum gauge 6, a gas analyzer 7 and a flow restriction valve 8 are also fitted. The analysis chamber 5 is typically made of stainless steel or aluminum alloy. The micro-sampled gas from the flow restrictor 4 enters the analysis chamber 5 and is pumped by the main pump 9 through the flow restriction valve 8, thereby creating 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 measures and analyzes the gas components in the analysis chamber 5, and may be a quadrupole mass spectrometer, a time-of-flight mass spectrometer, an ion trap mass spectrometer or other gas analysis instruments. Generally, the gas analyzer 7 is required to operate in a suitable vacuum environment, and therefore the analysis chamber 5 operates in a vacuum range of 10 degrees⁺²～10^-5Pa range.

Specifically, one end of the flow limiting valve 8 is connected with the analysis chamber 5, and the other end is connected with the main pump 9. The flow restriction valve 8 is a vacuum valve having a valve plate provided with a through hole of an appropriate size, and requires special design and manufacture. The main pump 9 is used for pumping ultimate vacuum or working vacuum to the analysis chamber 5, and may be an oil-free vacuum pump such as a molecular pump and an ion pump. When the valve plate of the flow limiting valve 8 is opened, the main pump 9 is completely communicated with the analysis chamber 5, and the vacuum pump 9 has the maximum pumping speed on the analysis chamber 5, so that the analysis chamber 5 can be pumped with extreme vacuum. Ultimate vacuum degree is generally 10^-5～10^-9Pa. when the valve plate of the flow restriction valve 8 is closed, the main pump 9 is connected to the analysis chamber 5 through the opening on the valve plate of the flow restriction valve 8, the pumping speed depends on the size of the opening, and the analysis chamber 5 is pumped with vacuum, generally, the size of the opening on the valve plate should meet the requirements of both the molecular flow pumping speed corresponding to the ① opening size and the vacuum of the analysis chamber 5, and the molecular flow pumping speed corresponding to the ② opening size should not exceed 25% of the pumping speed of the main pump 9, so as to shield the main pump 9And pumping speed fluctuation and selectivity are realized, so that stable lossless sampling analysis is realized.

Specifically, the backing pump 11 is connected to the main pump 9 through the electromagnetic valve 10, and is used for backing the main pump 9. Furthermore, the backing pump 11 is connected to the gas line between the valve block 3 and the flow restrictor 4 by means of 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, a standard gas source 13 is connected to the gas conduit between the valve group 3 and the flow restrictor 4 through a second regulating valve 14. The standard gas source 13 is used to supply a high-purity standard gas to the gas analysis apparatus, and the standard gas is a mixture of a plurality 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, heaters are provided on the sampling pipe and the analysis chamber 5 of the gas sampling and analyzing apparatus. The heater can bake and degas the sampling pipeline and the analysis chamber 5 to obtain good system background and improve the accuracy of gas analysis. In addition, the oven degassing of the analysis chamber 5 by the heater can also eliminate or reduce the contamination of the analysis chamber by hydrocarbons and the like.

Specifically, the gas sampling analysis apparatus needs to be periodically calibrated to ensure the accuracy and repeatability of the analysis results. In the gas sampling analysis device of fig. 1, a standard gas source 13 is connected to the gas line between the valve block 3 and the flow restrictor 4 via a second regulating valve 14. When the gas sampling and analyzing device is calibrated, the standard gas is introduced into the analysis chamber 5 through the second regulating valve 14 and the flow restrictor 4, and the standard gas is analyzed by the gas analyzer 7, in a similar procedure to the gas testing process. If the analyzed gas components and the analyzed gas concentrations are consistent with those of the standard gas, the gas sampling and analyzing device can analyze the gas through calibration. If the analyzed gas components and concentration are inconsistent with the standard gas, the gas sampling and analyzing device needs to be debugged until the calibration requirement is met. The debugging process of the gas sampling analysis device can be baking heating, system background extraction or adjusting parameters of the gas analyzer 7 and the like.

Specifically, in fig. 1 of the gas sampling analysis apparatus, on one hand, a backing pump 11 is connected to a main pump 9 through an electromagnetic valve 10, and is used for backing vacuum pumping of the main pump 9; and on the other hand via a first regulating valve 12 to the gas line connection between the valve block 3 and the flow restrictor 4 for providing the flow restrictor 4 with the desired front-end gas pressure or vacuum. When the process chamber 1 is at different gas or vacuum levels, the single backing pump 11 may not be well compatible with both requirements. Therefore, a vacuum pump 15 can be added to fulfill the above two requirements, respectively, in another gas sampling analysis device as shown in fig. 2, which is different from the gas sampling analysis device of fig. 1 in that a sampling module is different, and the sampling module of the gas sampling analysis device of fig. 2 comprises a process chamber, a valve set, a first regulating valve, a vacuum pump and a flow restrictor; the process chamber 1, the valve group 3 and the current limiter 4 are sequentially connected through a sampling pipe, one end of the sampling pipe is inserted into the process chamber 1, and 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 to one end of a current limiter 4 through a sampling pipe; the other end of the current limiter 4 is connected to a gas analysis module through a sampling pipe; one end of the first regulating valve 12 is connected to the valve block 3 and the sampling pipe connected to the flow 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 an electromagnetic valve 10 and used for pumping backing vacuum for the main pump 9; a vacuum pump 16 is connected via a first regulating valve 12 to the gas line between the valve block 3 and the flow restrictor 4 for providing the flow restrictor 4 with the required front-end gas pressure or vacuum.

In the embodiment of the application, the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve are opened to carry out ultimate vacuum pumping on the analysis chamber by closing the valve group, the first regulating valve and the second regulating valve; 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 polluting gas, the gas analysis module and the flow limiting valve are closed, the valve bank is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to carry out analysis test on the sampled gas; closing the valve group and the first regulating valve, and opening the flow limiting valve to continue to carry out ultimate vacuum pumping on the device; and when the gas analysis module does not monitor the polluting gas, closing the gas sampling analysis device to keep the gas sampling analysis device in a vacuum state. The application has the advantages that: (1) the method can be used for carrying out online analysis on high-pressure, normal-pressure and vacuum gases, (2) increasing the gas sampling amount and improving the response speed of a system, (3) eliminating the molecular discrimination effect and the pumping speed selectivity during gas sampling so as to realize nondestructive sampling analysis, and (4) carrying out automatic calibration.

Referring to fig. 3, a schematic flow chart of a gas sampling analysis method applied to a gas sampling analysis apparatus is provided for an embodiment of the present application. As shown in fig. 3, the method of the embodiment of the present application may include the steps of:

s101, closing the valve group, the first regulating valve and the second regulating valve, and opening a vacuum gauge, a backing pump, an electromagnetic valve, a main extraction valve and a flow limiting valve to carry out ultimate vacuum extraction on an analysis chamber;

in a possible implementation, the analysis chamber 5 is evacuated by closing the valve group 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 flow restriction valve 8. When the analysis chamber 5 reaches a suitable vacuum (e.g. less than 200Pa), the main pump 9 is turned on. And when the vacuum degree in the analysis chamber 5 meets the requirement, the gas analysis module 7 is started to monitor the background of the system in real time.

S102, 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;

in one possible implementation, if the gas analyzer 7 monitors that the system background is clean and free of contaminating gases, the vacuum is continuously pulled until a good system background is obtained and the background data is recorded. Otherwise, the heater 15 is turned on to bake out the gas from the device to eliminate or reduce the contamination until a good system background is obtained.

S103, when the gas analysis module does not monitor the polluting gas, closing the gas analysis module and the flow limiting valve, opening the valve bank, adjusting the first adjusting 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 flow-limiting valve 8 is closed, the valve block 3 is opened, and the first regulating valve 12 is regulated 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 the data is recorded.

S104, closing the valve group and the first regulating valve, and opening the flow limiting valve to continue to carry out ultimate vacuum pumping on the device;

in a possible implementation, after the gas analysis is completed, the valve group 3 and the first regulating valve 12 are closed, the flow limiting valve 8 is opened, and the device is continuously evacuated. If the gas analyzer 7 monitors that the system is free of contaminating gases, vacuum is continuously applied until a good system background is obtained. Otherwise, the heater 15 is turned on to bake out the gas from the device to eliminate or reduce the contamination until a good system background is obtained.

And S105, when the gas analysis module does not monitor the polluting gas, closing the gas sampling analysis device to keep the gas sampling analysis device in a vacuum state.

In a feasible implementation mode, after the sampled gas is exhausted, the gas sampling analysis device is closed to keep the gas sampling analysis device in a vacuum state, so that a good system background can be obtained in the next test. The gas sampling and analyzing device can also be filled with high-purity protective gas, such as 99.999% nitrogen.

For example, as shown in fig. 4, a typical operation flow of a gas sampling and analyzing device includes first background pumping of the system, then gas sampling and analyzing, then sample gas pumping, and finally shutting down the device.

Further, the gas sampling analysis apparatus needs to be periodically calibrated to ensure the accuracy and repeatability of the analysis results. During the periodic calibration of a gas sampling device 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 flow restrictor 4 via a second regulating valve 14. By adopting the steps similar to the gas testing process, firstly, the standard gas is introduced into the analysis chamber 5 through the second regulating valve 14 and the flow restrictor 4, the standard gas is analyzed by the gas analyzer 7, and if the analyzed gas component and concentration are consistent with the standard gas, the gas sampling analysis device is calibrated to perform gas analysis. If the analyzed gas components and concentration are inconsistent with the standard gas, the gas sampling and analyzing device needs to be debugged until the calibration requirement is met. The debugging process of the gas sampling analysis device can be baking heating, system background extraction or adjusting parameters of the gas analyzer 7 and the like.

In the embodiment of the application, the vacuum gauge, the backing pump, the electromagnetic valve, the main pump and the flow limiting valve are opened to carry out ultimate vacuum pumping on the analysis chamber by closing the valve group, the first regulating valve and the second regulating valve; 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 polluting gas, the gas analysis module and the flow limiting valve are closed, the valve bank is opened, the first regulating valve is regulated until the analysis chamber obtains working vacuum, and then the gas analysis module is opened to carry out analysis test on the sampled gas; closing the valve group and the first regulating valve, and opening the flow limiting valve to continue to carry out ultimate vacuum pumping on the device; and when the gas analysis module does not monitor the polluting gas, closing the gas sampling analysis device to keep the gas sampling analysis device in a vacuum state. The application has the advantages that: (1) the method can be used for carrying out online analysis on high-pressure, normal-pressure and vacuum gases, (2) increasing the gas sampling amount and improving the response speed of a system, (3) eliminating the molecular discrimination effect and the pumping speed selectivity during gas sampling so as to realize nondestructive sampling analysis, and (4) carrying out automatic calibration.

It will be understood by those skilled in the art that all or part of the processes of the methods of the embodiments described above can be implemented by a computer program, which can be stored in a computer-readable storage medium, and when executed, can include the processes of the embodiments of the methods described above. The storage medium may be a magnetic disk, an optical disk, a read-only memory or a random access memory.

The above disclosure is only for the purpose of illustrating the preferred embodiments of the present application and is not to be construed as limiting the scope of the present application, so that the present application is not limited thereto, and all equivalent variations and modifications can be made to the present application.