Comprehensive calibration device and method for partial pressure mass spectrometer and positive pressure leak hole
By using technical means such as static expansion and current limiting small holes in the vacuum pressure mass spectrometer, the problems of large leakage rate positive pressure leakage hole calibration and gas pressure mass spectrometer calibration under vacuum conditions are solved, and various leakage rates are achieved The calibration of positive pressure leakage holes and the normal operation of the vacuum pressure mass spectrometer meet the comprehensive calibration needs in the field of manned space flight.
Patent Information
- Application Number
- CN202411484312.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-23
- Publication Date
- 2025-02-18
- Estimated Expiration
- 2044-10-23
AI Technical Summary
The prior art is difficult to calibrate positive pressure leakage holes with large leakage rates in vacuum pressure mass spectrometers, and cannot simultaneously meet the calibration requirements of gas pressure mass spectrometers under vacuum conditions.
A dynamic flow method based on static expansion is designed to realize calibration of positive pressure leakage holes under positive pressure conditions and vacuum conditions through components such as gas supply system, sample assembly chamber, gas expansion chamber, current limiting hole and injection capillary. Comprehensive calibration scheme for calibration gas sub-pressure mass spectrometer.
The calibration of positive pressure leak holes of various leakage rates is achieved, ensuring that the vacuum pressure mass spectrometer works normally in a high-pressure environment, and meeting the comprehensive calibration requirements for gas composition analysis and positive pressure leak detection in the field of manned space.
Smart Images

Figure CN119469546A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of measurement technology, and in particular to a dynamic flow method vacuum partial pressure mass spectrometer based on static expansion and a positive pressure leak comprehensive calibration device and method. Background Art
[0002] When using a vacuum partial pressure mass spectrometer to calibrate a positive pressure leak, currently only positive pressure leaks with small leak rates can be calibrated. If a positive pressure leak with a large leak rate is calibrated, the gas pressure entering the mass spectrometry analysis room is high. If it is greater than 10 -4 Pa, the vacuum partial pressure mass spectrometer will not work. Therefore, it is necessary to design a calibration device suitable for positive pressure leaks of various leak rates.
[0003] Moreover, in the field of manned space flight, there is a clear demand for the comprehensive calibration of gas composition analysis and positive pressure leak detection. Therefore, it is hoped that the designed positive pressure leak calibration device can simultaneously meet the calibration requirements of the vacuum partial pressure mass spectrometer. Summary of the invention
[0004] In view of this, the present invention provides a dynamic flow method vacuum partial pressure mass spectrometer and positive pressure leak comprehensive calibration device and method based on static expansion, which can realize a comprehensive calibration scheme of calibrating positive pressure leaks under positive pressure conditions and calibrating gas partial pressure mass spectrometers under vacuum conditions in one device.
[0005] In order to solve the above technical problems, the present invention is implemented as follows.
[0006] A partial pressure mass spectrometer and positive pressure leak comprehensive calibration device, comprising: a gas supply system, a positive pressure leak to be measured, a sample preparation chamber, a gas expansion chamber, a sample injection capillary, a flow limiting orifice, a mass spectrometry analysis chamber, a vacuum partial pressure mass spectrometer, and a gas extraction system;
[0007] The gas supply system is connected to the inlet of the positive pressure leak hole through the eighth vacuum valve, the outlet of the positive pressure leak hole is connected to the inlet of the sample preparation chamber through the first vacuum valve, and the eighth vacuum valve is further connected to the inlet of the sample preparation chamber through the seventh vacuum valve; the sample preparation chamber is used to configure the standard gas required for the calibration of the positive pressure leak hole and the vacuum partial pressure mass spectrometer and the gas accumulation during the calibration of the positive pressure leak hole; the outlet of the sample preparation chamber is connected to the inlet of the gas expansion chamber through the second vacuum valve, and the gas in the sample preparation chamber is expanded to the gas expansion chamber by static expansion; the outlet of the gas expansion chamber is connected to the third vacuum valve, which is directly connected to the flow-limiting orifice on the one hand, and is connected to the flow-limiting orifice through the fourth vacuum valve and the injection capillary in series on the other hand; the other end of the flow-limiting orifice is connected to the mass spectrometry analysis chamber; according to the leakage rate of the positive pressure leak hole, the flow-limiting orifice is used to work alone or the flow-limiting orifice and the injection capillary work together to reduce the gas pressure to an acceptable level for the vacuum partial pressure mass spectrometer, and then enter the mass spectrometry analysis chamber; the exhaust system is connected to the mass spectrometry analysis chamber through the fifth vacuum valve;
[0008] The sample preparation room and the gas expansion room are respectively connected to a capacitance film vacuum gauge for measuring the gas pressure in the room; the mass spectrometry analysis room is connected to a vacuum partial pressure mass spectrometer and a magnetic levitation rotor vacuum gauge for measuring the gas partial pressure value and vacuum degree in the mass spectrometry analysis room respectively.
[0009] Preferably, the device further comprises a sixth vacuum valve, one end of which is connected to the pipeline between the eighth vacuum valve and the seventh vacuum valve, and the other end of which is connected to the exhaust system through the fifth vacuum valve.
[0010] The present invention also provides a partial pressure mass spectrometer and a positive pressure leak comprehensive calibration method, using the above calibration device, the method comprising:
[0011] The positive pressure leak calibration includes the following steps:
[0012] Step A1: using a gas supply system to fill the inlet of the positive pressure leak hole with helium at a first pressure through the eighth vacuum valve, and to fill the outlet of the positive pressure leak hole with nitrogen at a second pressure through the eighth vacuum valve, the seventh vacuum valve and the first vacuum valve, wherein the first pressure is greater than the second pressure;
[0013] Step A2: gas flows into the sample preparation chamber under the action of pressure difference to accumulate gas, and the accumulated gas expands to the gas expansion chamber. After the gas pressure change reaches the set value according to the pressure indicated by the second capacitance film vacuum gauge, the third vacuum valve is opened, and the gas enters the mass spectrometry analysis chamber through the flow limiting orifice;
[0014] Step A3: Determine whether the gas partial pressure mass spectrometer is opened normally; if not, open the fourth vacuum valve, use the injection capillary to limit the accumulated gas again, and enter step A4; if it is opened normally, directly enter step A4;
[0015] Step A4: reading the accumulated gas pressure P1 of the positive pressure leak through a gas partial pressure mass spectrometer;
[0016] Step A5: close the first vacuum valve, and the gas supply system introduces standard gas into the sample preparation room; the standard gas enters the mass spectrometry room through the pipeline between the sample preparation room and the mass spectrometry room, and the gas partial pressure mass spectrometer reads the standard gas pressure P2;
[0017] Step A6: Calculate the leakage rate of the positive pressure leak by comparing the accumulated gas pressure P1 of the positive pressure leak with the standard gas pressure P2;
[0018] The calibration of a partial pressure mass spectrometer includes the following steps:
[0019] Step B1: close the first vacuum valve and use the vacuum system to evacuate the pipeline;
[0020] Step B2: the gas supply system inflates the pipeline with an inlet pressure of P3; the inflated gas enters the mass spectrometer analysis chamber through the sample preparation chamber, the gas expansion chamber, and the current limiting component; the current limiting component is a mode in which the current limiting orifice works alone or the current limiting orifice and the injection capillary work together;
[0021] Step B3: using a magnetically suspended rotor vacuum gauge to obtain a pressure value P4 of the mass spectrometry chamber; assuming that the volume ratio C1 is the volume ratio of the gas expansion chamber to the sample preparation chamber, and the volume ratio C2 is the volume ratio of the mass spectrometry chamber to the gas expansion chamber, the partial pressure P5 in the mass spectrometry chamber is obtained by multiplying the inlet pressure P3 by the volume ratio C1 and the volume ratio C2;
[0022] Step B4: Obtain the correction coefficient of the partial pressure mass spectrometer by comparing the partial pressure P5 with the pressure value P4.
[0023] Preferably, the method further comprises, before step A1, using an exhaust system to evacuate both ends of the positive pressure leak.
[0024] Preferably, in step A3, the gas flows into the sample preparation chamber under the action of the pressure difference to accumulate the gas, and the accumulated gas expands into the gas expansion chamber, specifically:
[0025] The gas flows into the sample preparation chamber under the action of the pressure difference for gas accumulation. After the gas pressure change in the sample preparation chamber reaches the set value according to the pressure indicated by the first capacitance film vacuum gauge, the second vacuum valve is opened to allow the accumulated gas to expand into the gas expansion chamber.
[0026] Preferably, the length of the injection capillary is cut according to the gas pressure output by the gas expansion chamber and the gas pressure that the vacuum partial pressure mass spectrometer can withstand, so that the gas pressure drops to a level acceptable to the vacuum partial pressure mass spectrometer before entering the mass spectrometry analysis chamber.
[0027] Beneficial effects:
[0028] (1) The gas pipeline needs to be inflated to a maximum pressure of 8 atmospheres, so a full metal seal is required. The flow of high-pressure gas into the mass spectrometry chamber will cause damage to the vacuum gauge and gas partial pressure mass spectrometer, and contamination of the inner wall of the gas mass spectrometry chamber. Therefore, the gas needs to undergo at least 9 orders of magnitude of attenuation before entering the gas mass spectrometry chamber, and the gas pressure needs to be reduced from 10 5 The Pa level needs to be attenuated to 10 -4 Pa level, and the gas composition cannot change. Therefore, the present invention performs continuous gas attenuation through measures such as gas expansion, flow-limiting orifices, and sampling capillaries to ensure that the working environment of the partial pressure mass spectrometer is normal and the gas composition remains unchanged, which can provide the necessary conditions for the calibration of the vacuum partial pressure mass spectrometer and the positive pressure leak.
[0029] (2) In combination with the magnetically suspended rotor vacuum gauge provided on the vacuum partial pressure mass spectrometer and the calibration scheme provided by the present invention, it is possible to calibrate the vacuum partial pressure mass spectrometer under vacuum conditions with the same set of equipment on the basis of calibrating the positive pressure leak hole, thereby meeting the needs of the manned space flight field for the comprehensive calibration of gas composition analysis and positive pressure leak detection.
[0030] (3) Compared with the flow-limiting orifice, the injection capillary is easy to cut and replace. The length of the injection capillary can be cut or replaced according to the gas pressure output by the gas expansion chamber and the gas pressure that the vacuum partial pressure mass spectrometer can withstand. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Figure 1 It is a schematic diagram of the comprehensive calibration device of the partial pressure mass spectrometer and the positive pressure leak of the present invention.
[0032] Among them, 1-positive pressure leak, 2-first vacuum valve, 5-second vacuum valve, 8-third vacuum valve, 9-fourth vacuum valve, 15-fifth vacuum valve, 17-sixth vacuum valve, 18-seventh vacuum valve, 20-eighth vacuum valve, 3-sample preparation room, 4-first capacitance film vacuum gauge, 6-second capacitance film vacuum gauge, 7-gas expansion chamber, 10-injection capillary, 11-current limiting orifice, 12-mass spectrometry analysis room, 13-vacuum partial pressure mass spectrometer, 14-exhaust system, 16-magnetic levitation rotor vacuum gauge, 19-gas supply system. DETAILED DESCRIPTION
[0033] The present invention is described in detail below with reference to the accompanying drawings and embodiments.
[0034] The present invention provides a comprehensive calibration scheme for a vacuum partial pressure mass spectrometer and a positive pressure leak. The device adds a sampling capillary. When calibrating a positive pressure leak with a large leakage rate, if the vacuum partial pressure mass spectrometer cannot function normally due to excessive pressure, the sampling capillary branch is opened, so that the gas pressure entering the mass spectrometry analysis chamber is attenuated to 10 -4 Pa level, ensuring the normal operation of the vacuum partial pressure mass spectrometer. At the same time, combined with the magnetic suspension rotor vacuum gauge set on the vacuum partial pressure mass spectrometer, the comprehensive calibration scheme provided by the present invention can be used to calibrate the positive pressure leak hole, and the vacuum partial pressure mass spectrometer under vacuum conditions can be calibrated with the same set of equipment, meeting the requirements of comprehensive calibration of gas composition analysis and positive pressure leak detection in the positive pressure environment of the manned space flight field.
[0035] Figure 1 The schematic diagram of the vacuum partial pressure mass spectrometer and the positive pressure leak comprehensive calibration device of the present invention is shown. Figure 1As shown, the device is composed of a positive pressure leak hole 1, a first vacuum valve 2, a second vacuum valve 5, a third vacuum valve 8, a fourth vacuum valve 9, a fifth vacuum valve 15, a sixth vacuum valve 17, a seventh vacuum valve 18, an eighth vacuum valve 20, a sample preparation chamber 3, a first capacitance film vacuum gauge 4, a second capacitance film vacuum gauge 6, a gas expansion chamber 7, a sampling capillary 9, a current limiting orifice 11, a mass spectrometry analysis chamber 12, a vacuum partial pressure mass spectrometer 13, an exhaust system 14, a magnetic suspension rotor vacuum gauge 16, and a gas supply system 19;
[0036] The specific connection relationship is:
[0037] The gas supply system 19 is connected to the inlet of the positive pressure leak hole 1 through the eighth vacuum valve 20, the outlet of the positive pressure leak hole 1 is connected to the inlet of the sample preparation chamber 3 through the first vacuum valve 2, and the eighth vacuum valve 20 is further connected to the inlet of the sample preparation chamber 3 through the seventh vacuum valve 18; the outlet of the sample preparation chamber 3 is connected to the inlet of the gas expansion chamber 7 through the second vacuum valve 5, and the gas in the sample preparation chamber 3 is expanded to the gas expansion chamber 7 by static expansion; the outlet of the gas expansion chamber 7 is connected to the third vacuum valve 8, which is directly connected to the flow limiting hole 11 on the one hand, and is connected to the flow limiting hole 11 through the fourth vacuum valve 9 and the injection capillary 9 connected in series on the other hand; the other end of the flow limiting hole 11 is connected to the mass spectrometry analysis chamber 12; according to the leakage rate of the positive pressure leak hole 1, the flow limiting hole 11 is used to work alone or the flow limiting hole 11 and the injection capillary 9 work together to reduce the gas pressure to the level that the vacuum partial pressure mass spectrometer 13 can accept, and then enter the mass spectrometry analysis chamber 12; the exhaust system 14 is connected to the mass spectrometry analysis chamber 12 through the fifth vacuum valve 15. The sample preparation chamber 3 and the gas expansion chamber 7 are respectively connected to a capacitance film vacuum gauge; the mass spectrometry analysis chamber 12 is connected to a vacuum partial pressure mass spectrometer 13 and a magnetic suspension rotor vacuum gauge 16.
[0038] The working principle of the comprehensive calibration device is:
[0039] Due to the pressure difference between the inlet and outlet of the positive pressure leak hole 1, the gas flows through the positive pressure leak hole in one direction and accumulates statically; the sample preparation room 3 is used to configure the standard gas required for the calibration of the positive pressure leak hole and the vacuum partial pressure mass spectrometer or the gas accumulation during the calibration of the positive pressure leak hole; the gas in the sample preparation room 3 is expanded to the gas expansion chamber 7 by static expansion, and then enters the mass spectrometry analysis room through the limiting flow hole after the pressure drops; the first capacitance film vacuum gauge 4 is used to measure the gas pressure in the sample preparation room, and the second capacitance film vacuum gauge 6 is used to measure the gas pressure in the gas expansion chamber. According to the measured indoor gas pressure, it can be known whether the pressure change in the sample preparation room / gas expansion chamber reaches the set value. If it reaches, the subsequent valve is opened. In practice, the second vacuum valve 5 can also be kept open, and the sample preparation room and the gas expansion chamber are connected. When the pressure change in the gas expansion chamber reaches the set value, the third vacuum valve 8 is opened to allow the gas to enter the mass spectrometry analysis room 12 through the limiting flow component. The mass spectrometry chamber 12 is used to provide a measurement environment for partial pressure measurement of vacuum partial pressure mass spectrometer calibration and partial pressure measurement of leakage gas of positive pressure leak hole. A limited flow element is installed in the mass spectrometry chamber to meet dynamic measurement conditions.
[0040] The flow limiting component in the present invention includes a sampling capillary 10 and a flow limiting orifice 11. The flow limiting orifice 11 works alone or together with the sampling capillary 9. According to the leakage rate of the positive pressure leak hole 1, the flow limiting orifice 11 works alone or together with the sampling capillary 9. The flow of the gas in the gas expansion chamber 10 is limited to reduce the gas pressure to an acceptable level for the vacuum partial pressure mass spectrometer 13, and then enters the mass spectrometry analysis chamber 10, ensuring that the working environment of the partial pressure mass spectrometer 13 is normal and the gas composition remains unchanged, which can provide necessary conditions for the calibration of the vacuum partial pressure mass spectrometer 11 and the positive pressure leak hole 1.
[0041] The magnetically suspended rotor vacuum gauge 16 is used to measure the vacuum degree in the mass spectrometry analysis chamber 12; the vacuum partial pressure mass spectrometer 13 is used to measure the gas partial pressure value in the mass spectrometry analysis chamber; the gas supply system 19 provides the gas of the required pressure to the comprehensive calibration device through the vacuum valve 20; the exhaust system 14 is connected to the device pipeline through the vacuum valve 15, which can remove the gas in the system. The exhaust system has a selective exhaust function, which can improve the exhaust capacity of the exhaust system and reduce the background interference of the mass spectrometry analysis chamber.
[0042] In a preferred embodiment, the device further includes a sixth vacuum valve 17, one end of which is connected to the pipeline between the eighth vacuum valve 20 and the seventh vacuum valve 18, and the other end is connected to the exhaust system 14 through the fifth vacuum valve 15. The sixth vacuum valve 17 can be opened to evacuate the inlet and outlet of the positive pressure leak hole at the beginning of the positive pressure leak hole calibration by using the exhaust system. Because the leakage rate of the positive pressure leak hole varies depending on the type of gas, evacuation can make the gas composition single and the calibration accuracy high.
[0043] The following steps are included in the positive pressure leak calibration:
[0044] Step A0: the eighth vacuum valve is closed, and the inlet and outlet of the positive pressure leak hole are evacuated using the exhaust system 14 .
[0045] Step A1: Use the gas supply system 19 to fill the first pressure of helium into the inlet of the positive pressure leak hole through the eighth vacuum valve 20, and fill the second pressure of nitrogen into the outlet of the positive pressure leak hole through the eighth vacuum valve 20, the seventh vacuum valve 20 and the first vacuum valve 2, and the first pressure is greater than the second pressure. Generally, the second pressure is about 1 atmosphere, and the first pressure is determined according to the parameters of the inlet and outlet of the positive pressure leak hole and the use environment. In one embodiment, the first pressure is 2 atmospheres.
[0046] Step A2: The gas flows into the sample preparation chamber 3 under the action of the pressure difference for gas accumulation, and the accumulated gas expands to the gas expansion chamber 7. After the gas pressure change reaches the set value according to the pressure indicated by the second capacitance film vacuum gauge 6, the third vacuum valve 8 is opened, and the gas enters the mass spectrometry analysis chamber 12 through the flow limiting hole 11.
[0047] Here, the sample preparation chamber 3 and the gas expansion chamber 7 can be connected as a whole, or the pressure change judgment and outlet control can be performed separately. In the latter case, the gas first flows into the sample preparation chamber 3 under the action of the pressure difference to accumulate the gas. After judging that the gas pressure change in the sample preparation chamber 3 reaches the set value according to the pressure shown by the first capacitance film vacuum gauge 4, the second vacuum valve 5 is opened to expand the accumulated gas to the gas expansion chamber 7. After judging that the gas pressure change reaches the set value according to the pressure shown by the second capacitance film vacuum gauge 6, the third vacuum valve 8 is opened to allow the gas to enter the mass spectrometry analysis chamber 12 through the flow limiting orifice 11.
[0048] Step A3: Determine whether the gas partial pressure mass spectrometer 13 is opened normally; if not, open the fourth vacuum valve 9, use the sampling capillary 10 to limit the accumulated gas again, and enter step A4; if it is opened normally, directly enter step A4. The advantage of using the sampling capillary 10 is that, compared with the flow-limiting orifice, the sampling capillary 10 is easy to cut and replace. The length of the sampling capillary 10 can be cut or replaced according to the gas pressure output by the gas expansion chamber and the gas pressure that the vacuum partial pressure mass spectrometer 13 can withstand, so that the gas pressure drops to the level that the vacuum partial pressure mass spectrometer 13 can accept, and then enter the mass spectrometry analysis room.
[0049] Step A4: reading the accumulated gas pressure P1 of the positive pressure leak through the gas partial pressure mass spectrometer 13;
[0050] Step A5: close the first vacuum valve 2, and the gas supply system introduces standard gas into the sample preparation chamber 3; the standard gas enters the mass spectrometry chamber 12 through the pipeline between the sample preparation chamber 3 and the mass spectrometry chamber 12, and the gas partial pressure mass spectrometer 13 reads the standard gas pressure P2.
[0051] Step A6: The leakage rate of the positive pressure leak is calculated by comparing the accumulated gas pressure P1 of the positive pressure leak with the standard gas pressure P2.
[0052] The calibration of the partial pressure mass spectrometer includes the following steps:
[0053] Step B1: close the first vacuum valve 2 and use the vacuum system 14 to evacuate the pipeline.
[0054] Step B2: the gas supply system 19 inflates the pipeline with an intake pressure of P3; the inflated gas enters the mass spectrometry analysis chamber 12 through the sample preparation chamber, the gas expansion chamber, and the current limiting component; the current limiting component is a mode in which the current limiting hole 11 works alone or the current limiting hole 11 and the sampling capillary 9 work together.
[0055] Step B3: Use the magnetically suspended rotor vacuum gauge 16 to obtain the pressure value P4 of the mass spectrometry chamber 12; assume that the volume ratio C1 is the volume ratio of the gas expansion chamber 7 and the sample preparation chamber 3, and the volume ratio C2 is the volume ratio of the mass spectrometry chamber 12 and the gas expansion chamber 7, and the partial pressure P5 in the mass spectrometry chamber 12 is obtained by multiplying the intake pressure P3 by the volume ratio C1 and the volume ratio C2.
[0056] Step B4: Obtain the correction coefficient of the partial pressure mass spectrometer by comparing the partial pressure P5 with the pressure value P4.
[0057] The gas pipeline needs to be inflated to a maximum pressure of 8 atmospheres, so a full metal seal is required. The high-pressure gas flowing into the mass spectrometry chamber will cause damage to the vacuum gauge and the gas partial pressure mass spectrometer, and the inner wall of the gas mass spectrometry chamber will be contaminated. Therefore, the gas needs to undergo at least 9 orders of magnitude of attenuation before entering the gas mass spectrometry chamber, and the gas pressure needs to be reduced from 10 5 The Pa level needs to be attenuated to 10 -4 Pa level, and the gas composition cannot change, so continuous gas attenuation is performed through gas expansion, flow-limiting orifices, injection capillaries and other measures to meet the conditions for calibrating the gas partial pressure mass spectrometer and the positive pressure leak by the dynamic flow method.
[0058] The present invention is of great significance for the comprehensive calibration needs of gas composition analysis and positive pressure leak detection in the manned space field.
[0059] The above specific embodiments only describe the design principle of the present invention. The shapes and names of the components in the description may be different and are not limited. Therefore, those skilled in the art in the field of the present invention may modify or replace the technical solutions recorded in the above embodiments; and these modifications and replacements do not deviate from the creative purpose and technical solutions of the present invention and should all fall within the protection scope of the present invention.
Claims
1. A partial pressure mass spectrometer and positive pressure leak comprehensive calibration device, characterized in that: include: Gas supply system (19), positive pressure leak hole (1) to be tested, sample preparation chamber (3), gas expansion chamber (7), sample injection capillary (10), flow limiting orifice (11), mass spectrometry chamber (12), vacuum partial pressure mass spectrometer (13), and gas extraction system (14); The gas supply system (19) is connected to the inlet of the positive pressure leak hole (1) through the eighth vacuum valve (20), and the outlet of the positive pressure leak hole (1) is connected to the inlet of the sample preparation chamber (3) through the first vacuum valve (2), and the eighth vacuum valve (20) is further connected to the inlet of the sample preparation chamber (3) through the seventh vacuum valve (18); the sample preparation chamber (3) is used to configure the standard gas required for the calibration of the positive pressure leak hole and the vacuum partial pressure mass spectrometer and the gas accumulation during the calibration of the positive pressure leak hole; the outlet of the sample preparation chamber (3) is connected to the inlet of the gas expansion chamber (7) through the second vacuum valve (5), and the gas in the sample preparation chamber (3) is expanded to the gas expansion chamber (7) by static expansion; the outlet of the gas expansion chamber (7) is connected to the inlet of the gas expansion chamber (7) The third vacuum valve (8) is directly connected to the flow-limiting orifice (11) on one hand, and is connected to the flow-limiting orifice (11) through a fourth vacuum valve (9) and a sampling capillary (9) connected in series on the other hand; the other end of the flow-limiting orifice (11) is connected to a mass spectrometry chamber (12); according to the leakage rate of the positive pressure leak hole (1), the flow-limiting orifice (11) is used to work alone or the flow-limiting orifice (11) and the sampling capillary (9) work together to reduce the gas pressure to a level acceptable to the vacuum partial pressure mass spectrometer (13), and then enter the mass spectrometry chamber (12); the exhaust system (14) is connected to the mass spectrometry chamber (12) through the fifth vacuum valve (15); The sample preparation chamber (3) and the gas expansion chamber (7) are respectively connected to capacitance film vacuum gauges (4, 6) for measuring the gas pressure in the chambers; the mass spectrometry chamber (12) is connected to a vacuum partial pressure mass spectrometer (13) and a magnetic suspension rotor vacuum gauge (16) for measuring the gas partial pressure value and vacuum degree in the mass spectrometry chamber (12).
2. The device according to claim 1, characterized in that The device further comprises a sixth vacuum valve (17), one end of which is connected to the pipeline between the eighth vacuum valve (20) and the seventh vacuum valve (18), and the other end of which is connected to the exhaust system (14) through the fifth vacuum valve (15).
3. A comprehensive calibration method for a partial pressure mass spectrometer and a positive pressure leak, characterized in that: Using the device as claimed in claim 1 or 2, the method comprises: The positive pressure leak calibration includes the following steps: Step A1: using the gas supply system (19) to charge helium gas of a first pressure into the inlet of the positive pressure leak hole through the eighth vacuum valve (20), and charging nitrogen gas of a second pressure into the outlet of the positive pressure leak hole through the eighth vacuum valve (20), the seventh vacuum valve (20) and the first vacuum valve (2), wherein the first pressure is greater than the second pressure; Step A2: gas flows into the sample preparation chamber (3) under the action of pressure difference to accumulate gas, and the accumulated gas expands to the gas expansion chamber (7). After judging that the gas pressure change reaches the set value according to the pressure indicated by the second capacitance film vacuum gauge (6), the third vacuum valve (8) is opened, and the gas enters the mass spectrometry analysis chamber (12) through the flow limiting orifice (11); Step A3: Determine whether the gas partial pressure mass spectrometer (13) is opened normally; if not, open the fourth vacuum valve (9), use the sampling capillary (10) to limit the accumulated gas flow again, and enter step A4; if it is opened normally, directly enter step A4; Step A4: reading the accumulated gas pressure P1 of the positive pressure leak hole through the gas partial pressure mass spectrometer (13); Step A5: the first vacuum valve (2) is closed, and the gas supply system introduces standard gas into the sample preparation chamber (3); the standard gas enters the mass spectrometry chamber (12) through the pipeline between the sample preparation chamber (3) and the mass spectrometry chamber (12), and the gas partial pressure mass spectrometer (13) reads the standard gas pressure P2; Step A6: Calculate the leakage rate of the positive pressure leak by comparing the accumulated gas pressure P1 of the positive pressure leak with the standard gas pressure P2; The calibration of a partial pressure mass spectrometer includes the following steps: Step B1: close the first vacuum valve (2) and use the vacuum system (14) to evacuate the pipeline; Step B2: the gas supply system (19) inflates the pipeline with gas, and the inlet pressure is P3; the inflated gas enters the mass spectrometer analysis chamber (12) through the sample preparation chamber, the gas expansion chamber, and the flow limiting component; the flow limiting component is a mode in which the flow limiting hole (11) works alone or the flow limiting hole (11) and the sample injection capillary (9) work together; Step B3: using a magnetically suspended rotor vacuum gauge (16) to obtain a pressure value P4 of the mass spectrometry chamber (12); assuming that the volume ratio C1 is the volume ratio of the gas expansion chamber (7) to the sample preparation chamber (3), and the volume ratio C2 is the volume ratio of the mass spectrometry chamber (12) to the gas expansion chamber (7), and the partial pressure P5 in the mass spectrometry chamber (12) is obtained by multiplying the intake pressure P3 by the volume ratio C1 and the volume ratio C2; Step B4: Obtain the correction coefficient of the partial pressure mass spectrometer by comparing the partial pressure P5 with the pressure value P4.
4. The method according to claim 3, characterized in that The method further comprises, before step A1, using an exhaust system (14) to evacuate both ends of the positive pressure leak hole.
5. The method according to claim 3, characterized in that In step A3, the gas flows into the sample preparation chamber (3) under the action of the pressure difference to accumulate the gas, and the accumulated gas expands into the gas expansion chamber (7) as follows: The gas flows into the sample preparation chamber (3) under the action of the pressure difference to accumulate the gas. After the pressure change of the gas in the sample preparation chamber (3) reaches the set value according to the pressure indicated by the first capacitance film vacuum gauge (4), the second vacuum valve (5) is opened to allow the accumulated gas to expand into the gas expansion chamber (7).
6. The method according to claim 3, characterized in that The length of the injection capillary (10) is cut according to the gas pressure output by the gas expansion chamber and the gas pressure that the vacuum partial pressure mass spectrometer (13) can withstand, so that the gas pressure is reduced to a level that the vacuum partial pressure mass spectrometer (13) can accept, and then enters the mass spectrometry analysis chamber (12).
Citation Information
Patent Citations
Static sampling introduction device and method of calibrating pressure leak hole
CN102494741A
Positive pressure leakage hole calibration device and method based on static accumulation attenuation comparison method
CN104236813A
10-9Pa magnitude vacuum partial pressure calibration device and calibration coefficient acquisition method
CN105136389A
Positive pressure leak hole calibration system and method with lower limit of 10<-10>Pam<3> / s
CN108982021A
Method for analyzing gas
JP2000097910A
Cited By
High-sensitivity leak detection device and method based on low-vacuum accumulation method
CN116858448A