CN216871896U - Mass spectrometer partial pressure calibration system - Google Patents

Mass spectrometer partial pressure calibration system Download PDF

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Publication number
CN216871896U
CN216871896U CN202123335712.3U CN202123335712U CN216871896U CN 216871896 U CN216871896 U CN 216871896U CN 202123335712 U CN202123335712 U CN 202123335712U CN 216871896 U CN216871896 U CN 216871896U
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pressure
vacuum
calibration
mass spectrometer
gas
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朱伟平
彭先德
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Yirui Image Technology Chengdu Co ltd
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Yirui Image Technology Chengdu Co ltd
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Abstract

The utility model provides a mass spectrometer partial pressure calibration system, which comprises an air inlet system, an air exhaust system and a pressure and ion current measurement system, wherein the pressure and ion current measurement system is respectively communicated with the air inlet system and the air exhaust system; the gas inlet system is used for providing calibration gas with required pressure for the pressure and ion current measuring system; the air exhaust system is used for providing a low-pressure environment for the air inlet system and providing a required vacuum environment for the pressure and ion current measuring system; the pressure and ion current measuring system is used for simultaneously measuring the pressure of the vacuum cavity and the ion current corresponding to the calibration gas under the pressure. The mass spectrometer partial pressure calibration system has the advantages of simple structure, low cost and controllable measurement accuracy, and has good popularization and application prospects in mass spectrometer research and production enterprises.

Description

Mass spectrometer partial pressure calibration system
Technical Field
The utility model relates to the technical field of mass spectrometry, in particular to a mass spectrometer partial pressure calibration system.
Background
The mass spectrometer is an instrument for analyzing chemical components of gas by measuring partial pressure, has extremely high resolution and sensitivity in the aspect of gas component analysis, and is widely applied to the technical field of residual gas analysis. The working principle of mass spectrometers, such as quadrupole mass spectrometers which are widely used at present, is that an ion source ionizes a measured substance into ions and enters a mass filter, an electric field of the mass filter is adjusted, the measured substance is separated according to a certain mass-to-charge ratio (m/z), and finally, an ion detector measures the amount of the separated ions, thereby forming a mass spectrum. As can be known from the principle of a quadrupole mass spectrometer, an ion current of a specific mass-to-charge ratio (m/z) is measured by an ion detector, the ion current is related to factors such as the ionization amount of gas by the mass spectrometer, the number of ions entering a mass filter, and the like, and the mass spectrometer needs to analyze a substance partial pressure corresponding to the mass-to-charge ratio, so that the mass spectrometer needs to be subjected to partial pressure calibration to establish a functional relationship between the calibration gas partial pressure and the corresponding ion current.
Through years of research accumulation, the calibration technology of the mass spectrometer is greatly developed, and China also obtains good research results in the aspect of calibration of the quadrupole mass spectrometer. However, the structure of the current main mass spectrometry calibration system is very complex, and the construction cost is high, for example, mass spectrometry calibration systems established by Qinghua university and Lanzhou space technology and physics research institute have high technical requirements and high cost pressure for establishing a set of such complex mass spectrometry partial pressure calibration system for general mass spectrometry research enterprises, and the popularization and application of such mass spectrometry partial pressure calibration systems are greatly limited.
In addition, the mass spectrometer is a precision measuring instrument, and a calibration system of the mass spectrometer needs to introduce a very weak flow of calibration gas when performing partial pressure calibration, and the gas inlet rate of the calibration gas is required to be controlled at 10-7~10-1(Pa · L/s) range, whereas conventional mass flowmeters do not function at all. For example, a soap film flow meter, the limit measurement value is greater than 10-2(Pa · L/s), the measurement requirements for very low flow introduction for mass spectrometer partial pressure calibration are simply not met, and the control limit for gas flow for gas mass flowmeters is much higher. Therefore, how to introduce a trace amount of calibration gas into the reactorIs an important factor for restricting a mass spectrometer calibration system.
In view of the above, it is necessary to provide a mass spectrometer partial pressure calibration system to solve the problems of high technical requirements, complex structure, difficulty in controlling and measuring trace gases, and high cost and pressure of the existing mainstream mass spectrometer partial pressure calibration system, and greatly improve the application prospects in mass spectrometer research and production enterprises.
SUMMERY OF THE UTILITY MODEL
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a mass spectrometer partial pressure calibration system, which is used to solve the problems of high technical requirements, complex structure, difficulty in introducing trace calibration gas, and high cost and pressure of the current mainstream mass spectrometer partial pressure calibration system in the prior art.
To achieve the above and other related objects, the present invention provides a mass spectrometer partial pressure calibration system, comprising: the device comprises an air inlet system, an air exhaust system and a pressure and ion current measuring system, wherein the pressure and ion current measuring system is respectively communicated with the air inlet system and the air exhaust system, and the air inlet system is communicated with the air exhaust system; the gas inlet system provides calibration gas with required pressure for the pressure and ion current measurement system by regulating the gas pressure at the gas inlet end of the standard leak hole through the standard leak hole; the air pumping system is used for providing a low-pressure environment for the air inlet system and providing a required vacuum environment for the pressure and ion current measuring system; the pressure and ion current measuring system simultaneously and respectively measures the pressure of the vacuum cavity and the ion current corresponding to the calibration gas under the pressure through the vacuum return mass spectrometer.
Optionally, the air inlet system comprises a standard air source, a pressure reducing valve, a positive and negative pressure gauge, a standard leak hole, a vacuum ball valve and a four-way joint, and the four-way joint is communicated by a stainless steel pipeline and is used for communicating the pressure reducing valve, the positive and negative pressure gauge, the standard leak hole and the vacuum ball valve; the standard gas source is communicated with the pressure reducing valve and used for providing calibration gas; the vacuum ball valve is used for communicating the air exhaust system, and the pressure reducing valve and the vacuum ball valve are used for reducing the pressure of high-pressure gas provided by the standard gas source to the pressure required by measurement; the positive and negative pressure gauges are used for accurately reading the pressure at the air inlet end of the standard leak hole; and the standard leak hole is communicated with the pressure and ion current measuring system through a stainless steel pipe.
Optionally, the standard gas source is a cylinder filled with a calibration gas, which is argon.
Optionally, the air pumping system comprises a mechanical pump, a molecular pump, a first vacuum valve, a second vacuum valve and a three-way joint, and the mechanical pump, the molecular pump, the first vacuum valve, the second vacuum valve and the three-way joint are communicated with each other through a corrugated pipe; the first vacuum valve is positioned between the mechanical pump and the molecular pump; the second vacuum valve is positioned at the other end of the molecular pump and is used for communicating the pumping system with the pressure and ion current measuring system; the three-way joint is respectively communicated with the mechanical pump, the first vacuum valve and a vacuum ball valve of the air inlet system; the mechanical pump is used for providing a vacuum environment for normal operation of the molecular pump and providing a low-pressure environment for the air inlet system according to requirements; the molecular pump is used for providing a required vacuum environment for the pressure and ion current measuring system; the first vacuum valve and the second vacuum valve are used for providing protection for the air exhaust system.
Optionally, the pressure and ion current measurement system includes a vacuum chamber, a vacuum return, a mass spectrometer, and a communication pipe.
Optionally, the vacuum chamber and the mass spectrometer are respectively symmetrically arranged at the left side and the right side of the vacuum chamber.
Optionally, the vacuum chamber is a horizontal cylinder.
Optionally, the calibration gas inlet pipe is disposed at the top of the vacuum chamber, and the pumping port of the pumping system is disposed at the bottom of the vacuum chamber.
As described above, the mass spectrometer partial pressure calibration system of the present invention has the following beneficial effects: 1. the utility model uses the standard leak hole as a control device for calibrating the micro-flow of the gas, utilizes the characteristic that the standard leak hole meets the Hagen Poiseuille law, and realizes the purpose by adjusting the gas pressure at the gas inlet end of the standard leak holeThe accurate control of the inlet rate of the calibration gas, i.e. the leakage rate Q of the standard leakCalibrationHas a large adjustable range of 10-7~10-1(Pa.L/s), effectively solving the problem that the conventional flow controller can not control and measure the trace gas; in addition, the standard leak is relatively cheap, and has high advantage in the aspect of system cost control. 2. The system leakage rate Q of the utility modelSystem for controlling a power supplyThe system can accurately measure the leakage rate Q of the system through a standard methodSystemAnd calibration gas admission rate QCalibrationUnder the condition of accurate control, the proportion eta of the calibration gas in the vacuum cavity can be accurately calculated through the following relational expression: eta is QCalibration/(QCalibration+QSystem for controlling a power supply) Thus, the partial pressure P of the calibration gasCalibrationMeasuring vacuum cavity pressure P with vacuum returnCavity bodySatisfies the following relationship: pCalibration=η×PCavity bodyBy the method, the partial pressure of the calibration gas in the vacuum cavity can be accurately measured and calculated, the system error of the partial pressure calibration system is reduced, and the accuracy of the partial pressure calibration system is improved. 3. The pressure of the vacuum cavity can be controlled at 10 by configuring a suitable air pumping system-6~10-1And the adjustable vacuum degree range is large in the Pa range, so that the partial pressure calibration requirement of the mass spectrometer can be well met. 4. The utility model has simple structure, low cost and controllable measurement accuracy, and has good popularization and application prospect in mass spectrometer research and production enterprises.
Drawings
Fig. 1 shows a schematic structure of a partial pressure calibration system of a mass spectrometer according to the present invention.
Fig. 2 is a schematic flow chart of a partial pressure calibration method of a mass spectrometer according to the partial pressure calibration system of the utility model.
Description of the element reference numerals
101 standard gas source
102 pressure reducing valve
103 positive and negative pressure gauge
104 standard leak
105 vacuum ball valve
106 four-way joint
201 mechanical pump
202 molecular pump
203 first vacuum valve
204 second vacuum valve
205 three-way joint
301 vacuum chamber
302 vacuum return
303 mass spectrometer
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure of the present invention.
Please refer to fig. 1-2. It should be understood that the structures, ratios, sizes, and the like shown in the drawings and described in the specification are only used for matching with the disclosure of the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions under which the present invention can be implemented, so that the present invention has no technical significance, and any structural modification, ratio relationship change, or size adjustment should still fall within the scope of the present invention without affecting the efficacy and the achievable purpose of the present invention. In addition, the terms "upper", "lower", "left", "right", "middle" and "one" used in the present specification are used for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms may be changed or adjusted without substantial change in the technical content.
The utility model takes the standard leak hole as a control device for calibrating the gas flow, utilizes the characteristic that the standard leak hole meets the Hagen Poiseuille law, and adjusts the standard leak holeAnd the gas pressure at the gas inlet end of the standard leak hole realizes the accurate control of the leak rate of the standard leak hole, namely the gas inlet rate of the calibration gas. The control precision of the air inlet rate of the calibration gas is high, and the leakage rate of the standard leak hole is the air inlet rate Q of the calibration gasCalibrationHas a wide adjustable range of 10-7~10-1(Pa·L/s)。
The system leakage rate Q of the utility modelSystem for controlling a power supplyLess than 10-6(Pa.L/s), which requires accurate measurement when performing gas calibration, and the gas inlet rate Q is determined by the calibration gas when performing partial pressure calibrationCalibrationSystem leakage rate Q with the system itselfSystem for controlling a power supplyThe ratio η of the partial pressure of the calibration gas to the total pressure of the calibration system, i.e. the pressure of the vacuum chamber, is a known value:
η=Qcalibration/(QCalibration+QSystem for controlling a power supply) (1)
Thus, in performing a mass spectrometer partial pressure calibration, the partial pressure P of the calibration gasCalibrationPressure P of vacuum cavity measured with vacuum returnCavity bodySatisfies the following relationship:
Pcalibration=η×PCavity body (2)
In the utility model, the pressure of the vacuum cavity is determined by the mutual balance of the air inlet rate of the calibration gas and the air extraction rate of the air extraction system, so that the pressure of the vacuum cavity is in a stable dynamic balance process in the test process, and the pressure of the vacuum cavity is directly measured by a vacuum return. The pressure range of the vacuum cavity can be controlled to be 10 by selecting a proper air pumping system-6~10-1Within Pa, the vacuum degree in the range can well meet the calibration requirement of the mass spectrometer.
Example one
As shown in fig. 1, in order to implement the above functions, the present invention provides a mass spectrometer partial pressure calibration system, which includes: the device comprises an air inlet system, an air exhaust system and a pressure and ion current measuring system, wherein the pressure and ion current measuring system is respectively communicated with the air inlet system and the air exhaust system, and the air inlet system is communicated with the air exhaust system; the gas inlet system provides calibration gas with required pressure for the pressure and ion current measuring system by regulating the gas pressure at the gas inlet end of the standard leak hole 104 through the standard leak hole 104; the air exhaust system is used for providing a low-pressure environment for the air inlet system and providing a required vacuum environment for the pressure and ion current measuring system; the pressure and ion current measuring system simultaneously and respectively measures the ion current corresponding to the calibration gas under the pressure of the vacuum cavity 301 and the pressure through the vacuum manifold 302 and the mass spectrometer 303.
As shown in fig. 1, the air intake system includes, as an example, a standard air source 101, a pressure reducing valve 102, a positive-negative pressure gauge 103, a standard leak hole 104, a vacuum ball valve 105, and a four-way joint 106, and is communicated by a stainless pipe, and the four-way joint 106 is used for communicating the pressure reducing valve 102, the positive-negative pressure gauge 103, the standard leak hole 104, and the vacuum ball valve 105.
In this embodiment, the standard gas source 101 is a steel cylinder filled with a calibration gas for providing the calibration gas, the standard gas is argon, and an argon pressure provided by the standard gas, that is, an outlet pressure of the argon cylinder, is 10 Mpa.
The pressure reducing valve 102 is connected to the argon bottle, high-pressure argon gas discharged from the argon bottle is reduced to required pressure, and the range of the pressure reducing valve 102 is 0-2.5 MPa. It should be noted here that the pressure value output by the pressure reducing valve 102 is relative to the standard atmospheric pressure, i.e. the pressure reducing valve 102 cannot provide a pressure value lower than one atmosphere (i.e. 0.1MPa), and a pressure value lower than 0.1MPa needs to be obtained by the vacuum ball valve 105.
One end of the vacuum ball valve 105 is connected with the four-way joint 106, the other end of the vacuum ball valve is connected with the three-way joint of the air exhaust system, and a pressure value lower than 0.1MPa is obtained by opening the vacuum ball valve 105.
The positive and negative pressure gauges 103 are communicated with the four-way joint 106 and used for accurately reading the pressure of the calibration gas at the gas inlet end of the standard leak hole 104, the positive pressure of the positive and negative pressure gauges 103 is higher than the atmospheric pressure, and the negative pressure is lower than the atmospheric pressure, so that the absolute pressure at the gas inlet end of the standard leak hole 104 can be accurately calculated through the reading of the positive and negative pressure gauges 103, and the leak rate of the standard leak hole 104, namely the gas inlet rate of the calibration gas, can be accurately calculated and controlled.
The standard leak hole 104 is used for providing a trace amount of calibration gas for the mass spectrometer partial pressure calibration system, and the calibration gas is accurately controlled by adjusting the pressure of the calibration gas at the gas inlet end. In this embodiment, when the absolute pressure of the air inlet end of the standard leak hole 104 is set to 0.1MPa, the leak rate is 2 × 10-4(Pa · L/s); therefore, when the absolute pressure range of the air inlet end of the standard leak hole 104 is set to be 0.001 MPa-3.5 MPa, the adjustable range of the air inlet rate of the calibration gas is 10 according to the Hagan Poiseue's law-7~10-1(Pa·L/s)。
As shown in fig. 1, the gas-pumping system includes a mechanical pump 201, a molecular pump 202, a first vacuum valve 203, a second vacuum valve 204 and a three-way joint 205, and are communicated with each other by a bellows; the first vacuum valve 203 is positioned between the mechanical pump 201 and the molecular pump 202; the second vacuum valve 204 is located at the other end of the molecular pump 202 and is used for communicating the pumping system and the pressure and ion current measurement system; the three-way joint 205 is respectively communicated with the mechanical pump 201, the first vacuum valve 203 and the vacuum ball valve 105 of the air inlet system;
the mechanical pump 201 is used for providing a vacuum environment for normal operation of the molecular pump 202, and simultaneously providing a low-pressure environment for the air intake system according to requirements; the molecular pump 202 is used for providing a required vacuum environment for the pressure and ion current measurement system; the first vacuum valve 203 and the second vacuum valve 204 are opened or closed according to the requirements of the mass spectrometer partial pressure calibration system, and are used for providing protection for the gas extraction system.
In this embodiment, the mechanical pump 201 is respectively communicated with the first vacuum valve 203 and the vacuum ball valve 105 of the air inlet system through the three-way joint 205, and can provide a pressure lower than 50Pa for the molecular pump 202 to match the normal operation of the molecular pump 202, and can be used for adjusting the low pressure required by the air inlet end of the standard leak 104.The molecular pump is connected with a vacuum cavity 301 of the partial pressure and ion current measurement system through a second vacuum valve 202 and 204, the vacuum cavity 301 is provided with an air extraction rate of 40(L/s) under the cooperation of the mechanical pump 201, and the ultimate vacuum degree of the molecular pump 202 is 5 multiplied by 10-8Pa。
As shown in fig. 1, the pressure and ion current measuring system includes, as an example, a vacuum cavity 301, a vacuum return 302, a mass spectrometer 303, and a communication pipe, where the vacuum return 302 and the mass spectrometer 303 are symmetrically disposed on the left and right sides of the vacuum cavity 301 respectively. The vacuum cavity 301 is a horizontal cylinder; the air inlet pipeline of the calibration gas is arranged at the top of the vacuum cavity 301, and the pumping port of the pumping system is arranged at the bottom of the vacuum cavity 301.
It should be noted that the vacuum gauge 302 and the mass spectrometer 303 are respectively symmetrically disposed at the left and right sides of the vacuum cavity 301, so that flow fields of calibration gas at probes of the vacuum gauge 302 and the mass spectrometer 303 are the same, that is, pressures tend to be consistent, and system errors are reduced; when calibration measurement is performed, the vacuum gauge 302 and the mass spectrometer 303 simultaneously measure the pressure of the vacuum cavity 301 and the ion current corresponding to the calibration gas, respectively, as basic data for calibration.
Example two
As shown in fig. 2, the present invention further provides a partial pressure calibration method for a mass spectrometer partial pressure calibration system based on the first embodiment, wherein the partial pressure calibration process mainly includes 4 steps, which are respectively a system leak rate test, a calibration gas introduction, a cavity pressure and ion current calibration measurement, and a calibration gas partial pressure and ion current function relationship establishment, and the specific calibration process is shown in fig. 2. The flow of the differential pressure calibration method will be described in detail below.
S1 system leak rate test: closing the pressure reducing valve 102, opening the vacuum ball valve 105, and opening the mechanical pump 201, so that the pressure at the exhaust end of the molecular pump 202 and the pressure at the air inlet end of the standard leak hole 104 are lower than 50Pa, and according to Hagan Poisbee's law, the leak rate at the air inlet end of the standard leak hole 104 is far lower than that of the general vacuum ball valve 105 under the pressure conditionTherefore, the standard leak 104 at this time is equivalent to the closed state. The molecular pump 202 is started to pump the vacuum chamber 301 to 10 deg.C-5Pa or less. The system leakage rate Q of the vacuum cavity 301 is accurately measured by adopting a vacuum system leakage rate test method of the national standard vacuum technology vacuum system leakage rate test method (GB/T32218-2015)System for controlling a power supply
S2 introducing calibration gas: when the pressure of the vacuum chamber 301 is 10 deg.C-5And below Pa, opening the pressure reducing valve 102, introducing calibration gas into the air inlet end of the standard leak hole 104, opening and closing the pressure reducing valve 102 for multiple times in order to empty impurity gases such as air at the front end of the standard leak hole 104, and purging the pipeline space at the air inlet end of the standard leak hole 104 by matching with opening and closing the vacuum ball valve 105. And adjusting the pressure of the calibration gas at the air inlet end of the standard leak hole 104, wherein the adjustment of the pressure is mainly performed through the matching of the pressure reducing valve 102 and the vacuum ball valve 105, when the pressure at the air inlet end of the standard leak hole 104 is higher than 1 standard atmospheric pressure, the adjustment is mainly performed through the pressure reducing valve 102, and when the pressure at the air inlet end of the standard leak hole 104 is lower than 1 standard atmospheric pressure, the adjustment is performed through the vacuum ball valve 105. The pressure of the pipeline at the air inlet end of the standard leak hole 104 is accurately read mainly through the positive and negative pressure gauge 103 and converted into absolute pressure. The air inlet rate of the calibration gas in the vacuum cavity 301 can be controlled to be 10 through the cooperation of the pressure reducing valve 102 and the vacuum ball valve 105-7~10-1(Pa · L/s).
S3 calibrating and measuring the cavity pressure and the ion current: in a state where the gas inlet system and the gas exhaust system operate simultaneously, the pressure of the calibration gas entering the vacuum cavity 301 is in a smooth dynamic equilibrium state, and the vacuum gauge 302 and the mass spectrometer 303 respectively measure the pressure of the vacuum cavity 301 and the ion current corresponding to the calibration gas under the pressure simultaneously. The mass spectrometer measures the ion current value I corresponding to the calibration gasCalibration 1Simultaneously recording the vacuum return 302 reading PCavity 1(ii) a Adjusting the air inlet rate of the calibration gas, and after the pressure of the vacuum cavity 301 reaches dynamic balance, adjusting the massMeasuring ion current value I corresponding to calibration gas by spectrometerCalibration 2While recording the vacuum return 302 reading PCavity 2(ii) a By analogy, n groups of corresponding I are respectively measuredCalibration iValue and PCavity i
S4 establishes a calibration gas partial pressure as a function of ion current: will PCavity iSubstituting the value into formula (2) to obtain partial pressure value P corresponding to calibration gasCalibration i. Obtaining ion current values corresponding to the calibration gases measured by the n groups of mass spectrometers and partial pressure values (I) corresponding to the calibration gases through the stepsCalibration i,PCalibration i) Establishing a linear function relation between the ion current corresponding to the calibration gas and the partial pressure corresponding to the calibration gas by adopting a mathematical analysis method:
Pcalibration i=F(ICalibration i) (3)
Formula (3) is a relationship between an ion current corresponding to a mass-to-charge ratio of a calibration gas measured by a mass spectrometer and a partial pressure of the calibration gas, and the functional relationship of formula (3) is generally a linear functional relationship.
In this embodiment, a least square method is preferably used as the mathematical analysis method to establish a linear functional relationship between the ion current and the partial pressure of the calibration gas corresponding to the mass-to-charge ratio of the calibration gas:
Pcalibration i=aICalibration i+b (4)
In the formula (4), a is a slope and b is an intercept.
By replacing the calibration gas and following the above steps S1 to S4, different partial pressures of the calibration gas as a function of the corresponding ion current can be obtained.
In summary, the present invention provides a mass spectrometer partial pressure calibration system, which includes: the device comprises an air inlet system, an air exhaust system and a pressure and ion current measuring system, wherein the pressure and ion current measuring system is respectively communicated with the air inlet system and the air exhaust system, and the air inlet system is communicated with the air exhaust system; the air inlet system passes through a standard leak hole and adjusts the air pressure at the air inlet end of the standard leak hole to be the pressureProviding a calibration gas at a desired pressure with the ion current measurement system; the air exhaust system is used for providing a low-pressure environment for the air inlet system and providing a required vacuum environment for the pressure and ion current measuring system; the pressure and ion current measuring system is used for simultaneously measuring the pressure of the vacuum cavity and the ion current corresponding to the calibration gas under the pressure. The utility model takes the standard leak hole as a control device for calibrating the micro-flow of the gas, utilizes the characteristic that the standard leak hole meets the Harbin Poiseue law, and realizes the accurate control of the gas inlet rate of the calibration gas by adjusting the gas pressure at the gas inlet end of the standard leak hole, wherein the gas inlet rate of the calibration gas is the leak rate Q of the standard leak holeCalibrationHas a large adjustable range of 10-7~10-1(Pa.L/s), effectively solving the problem that the conventional flow controller can not control and measure the trace gas; in addition, the standard leak is relatively cheap, and has higher advantage in the aspect of system cost control; the system leakage rate Q of the utility modelSystem for controlling a power supplyThe system can accurately measure the leakage rate Q of the system through a standard methodSystem for controlling a power supplyAnd calibration gas admission rate QCalibrationUnder the condition of accurate control, the proportion eta of the calibration gas in the vacuum cavity can be accurately calculated through the following relational expression: eta is QCalibration/(QCalibration+QSystem for controlling a power supply) Thus, the partial pressure P of the calibration gasCalibrationMeasuring vacuum cavity pressure P with vacuum returnCavity bodySatisfies the following relationship: pCalibration=η×PCavity bodyBy the method, the partial pressure of the calibration gas in the vacuum cavity can be accurately measured and calculated, the system error of the partial pressure calibration system is reduced, and the accuracy of the partial pressure calibration system is improved; the pressure of the vacuum cavity can be controlled at 10 by configuring a suitable air pumping system-6~10-1The adjustable vacuum degree range is large within the Pa range, and the requirement of partial pressure calibration of a mass spectrometer can be well met; the utility model has simple structure, low cost and controllable measurement accuracy, and has good popularization and application prospect in mass spectrometer production enterprises. Therefore, the utility model effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the utility model. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (8)

1. A mass spectrometer partial pressure calibration system, comprising: the device comprises an air inlet system, an air exhaust system and a pressure and ion current measuring system, wherein the pressure and ion current measuring system is respectively communicated with the air inlet system and the air exhaust system, and the air inlet system is communicated with the air exhaust system;
the gas inlet system provides calibration gas with required pressure for the pressure and ion current measurement system by regulating the gas pressure at the gas inlet end of the standard leak hole through the standard leak hole;
the air exhaust system is used for providing a low-pressure environment for the air inlet system and providing a required vacuum environment for the pressure and ion current measuring system;
the pressure and ion current measuring system simultaneously and respectively measures the pressure of the vacuum cavity and the ion current corresponding to the calibration gas under the pressure through the vacuum return mass spectrometer.
2. The mass spectrometer partial pressure calibration system of claim 1, wherein: the air inlet system comprises a standard air source, a pressure reducing valve, a positive and negative pressure gauge, a standard leak hole, a vacuum ball valve and a four-way joint, and is communicated by a stainless steel pipeline, and the four-way joint is used for communicating the pressure reducing valve, the positive and negative pressure gauge, the standard leak hole and the vacuum ball valve; the standard gas source is communicated with the pressure reducing valve and is used for providing calibration gas; the vacuum ball valve is used for communicating the air exhaust system, and the pressure reducing valve and the vacuum ball valve are used for reducing the pressure of the high-pressure air provided by the standard air source to the pressure required by measurement; the positive and negative pressure gauge is used for accurately reading the pressure at the air inlet end of the standard leak hole; and the standard leak hole is communicated with the pressure and ion current measuring system through a stainless steel pipe.
3. The mass spectrometer partial pressure calibration system of claim 2, wherein: the standard gas source is a steel cylinder filled with calibration gas, and the calibration gas is argon.
4. The mass spectrometer partial pressure calibration system of claim 1, wherein: the air pumping system comprises a mechanical pump, a molecular pump, a first vacuum valve, a second vacuum valve and a three-way joint, and the mechanical pump, the molecular pump, the first vacuum valve, the second vacuum valve and the three-way joint are communicated with each other through a corrugated pipe; the first vacuum valve is positioned between the mechanical pump and the molecular pump, and the second vacuum valve is positioned at the other end of the molecular pump and is used for communicating the pumping system with the pressure and ion current measuring system; the three-way joint is respectively communicated with the mechanical pump, the first vacuum valve and a vacuum ball valve of the air inlet system; the mechanical pump is used for providing a vacuum environment for normal operation of the molecular pump and providing a low-pressure environment for the air inlet system according to requirements; the molecular pump is used for providing a required vacuum environment for the pressure and ion current measuring system; the first vacuum valve and the second vacuum valve are used for providing protection for the air exhaust system.
5. The mass spectrometer partial pressure calibration system of claim 1, wherein: the pressure and ion current measuring system comprises a vacuum cavity, a vacuum return, a mass spectrometer and a communicating pipeline.
6. The mass spectrometer partial pressure calibration system of claim 5, wherein: the vacuum return and the mass spectrometer are respectively and symmetrically arranged on the left side and the right side of the vacuum cavity.
7. The mass spectrometer partial pressure calibration system of claim 5, wherein: the vacuum cavity is a horizontal cylinder.
8. The mass spectrometer partial pressure calibration system of claim 7, wherein: the air inlet pipeline of the calibration gas is arranged at the top of the vacuum cavity, and the air exhaust port of the air exhaust system is arranged at the bottom of the vacuum cavity.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118032099A (en) * 2024-04-15 2024-05-14 成都工业学院 Flow detector linear interval testing instrument and method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118032099A (en) * 2024-04-15 2024-05-14 成都工业学院 Flow detector linear interval testing instrument and method

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