CN201152868Y - Relative response calibration system for four polar mass spectra gauge - Google Patents
Relative response calibration system for four polar mass spectra gauge Download PDFInfo
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- CN201152868Y CN201152868Y CNU2007201910211U CN200720191021U CN201152868Y CN 201152868 Y CN201152868 Y CN 201152868Y CN U2007201910211 U CNU2007201910211 U CN U2007201910211U CN 200720191021 U CN200720191021 U CN 200720191021U CN 201152868 Y CN201152868 Y CN 201152868Y
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- mass spectrometer
- quadrupole mass
- molecular pump
- mass spectrum
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Abstract
The utility model relates to a relative sensitivity calibration of a quadrupole mass spectrometer, which belongs to the calibration field. The quadrupole mass spectrometer system of the quadrupole mass spectrometer consists of a calibrated quadrupole mass spectrometer, a mass spectrogram chamber, a high-vacuum pressure measurement gauge, a sampling system, a high-vacuum exhausting system and a computer, wherein, the calibrated quadrupole mass spectrometer is used for measuring the gas component content in the mass spectrogram chamber; the mass spectrogram chamber provides the high vacuum environment demanded by the quadrupole mass spectrometer; the high-vacuum pressure measurement gauge is used for exact measurement on the pressure in the mass spectrogram chamber; the sampling system ensures that the known component content gas which meets demand is filled into the mass spectrogram chamber; the high-vacuum exhausting system is used for obtaining high-vacuum environment of the mass spectrogram chamber; the computer is used for measuring data analysis and calibration factor calculation of the calibrated quadrupole mass spectrometer. The quadrupole mass spectrometer system has the advantages that the calibration uncertainty is small, and the difficulty in quadrupole mass spectrometer quantitative analysis can be overcome, and the like.
Description
Technical field
The utility model relates to the relative sensitivity calibration of quadrupole mass spectrometer, belongs to the calibration field.
Technical background
Present mass spectrograph particularly quadrupole mass spectrometer extensively applies to rga, fields such as monitoring of hazardous gas, space environment particle analysis, but because the operating characteristic of quadrupole mass spectrometer self, in use, it is measured absolute sensitivity and changes bigger in time, and irregular following, cause quadrupole mass spectrometer to be mainly used in the qualitative analysis aspect at present, the quantitative test aspect is less with it, quantitatively the difficult uncertainty as a result of carrying out or quantitatively calibrating of calibration operation is big, can't satisfy user's demand, particularly the high reliability request of space product development aspect.
Summary of the invention
The purpose of this utility model provides a kind of simple in structure, quadrupole mass spectrometer partial pressure calibration system that calibration uncertainty is little, easy to use.
The purpose of this utility model is achieved through the following technical solutions:
Quadrupole mass spectrometer relative sensitivity calibration system of the present utility model is by being formed by school quadrupole mass spectrometer, mass spectrum chamber, high vacuum pressure measuring gage, sampling system, fine pumping system, control desk and computing machine.
By the school quadrupole mass spectrometer as shown in Figure 1, be connected on the mass spectrum chamber, adopt the data line that has the RS232 interface to link to each other with computing machine by standard C F35 flange.By the school quadrupole mass spectrometer can be the product of internationally famous manufacturer, as each model quadrupole mass spectrometer of companies such as Inficon, LeyBold, PFEFFIER manufacturing.If by the interface shape of school quadrupole mass spectrometer is not standard C F35 flange-interface, need requirement processing crossover sub according to concrete model.
Mass spectrum chamber adopts spherical structure as shown in Figure 1, makes of stainless steel material, and size can be according to concrete needs design.Leave high vacuum pressure measuring gage standard K F25 flange-interface at its top, adopt standard C F250 flange to link to each other with push-pull valve in the bottom, symmetry leaves by school quadrupole mass spectrometer standard K F35 flange-interface and sample channel standard K F16 flange-interface at the place, equator of ball.
The high vacuum pressure measuring gage links to each other with mass spectrum chamber by standard K F25 flange as shown in Figure 1, and the pressure measurement range requirement of rule is: 1 * 10
-1Pa～1 * 10
-7Pa, calibration uncertainty require can select internationally famous manufacturer for use less than 10%, advise as Penning gauge or capacitor thin film that companies such as Inficon, LeyBold, PFEFFIER make.
Sampling system as shown in Figure 1, it is made up of scattering ball, sample channel, sampling valve, sample introduction interface and the sample introduction pipeline of finding time.The scattering ball is selected the stainless steel material manufacturing for use, is the spherical structure of diameter phi 10mm, and the aperture that the surface has evenly distributed 128 diameter phi 1mm adopts the mode of welding to link to each other with sample channel; Sample channel is selected the stainless steel material manufacturing for use, diameter phi 5mm, length is determined according to the size of mass spectrum chamber, mounting means is that an end adopts welded structure to link to each other with sampling valve, the other end adopts counter flange, links to each other with the scattering ball by the mode of welding, and the technology of employing laser boring is opened the aperture of one 10 μ m on the counter flange; Sampling valve is selected high precision vacuum pressure variable valve for use, and an end links to each other with sample channel by the mode of welding, and the other end links to each other with the sample introduction interface by standard K F16 flange; The sample introduction interface is the three-port structure that stainless steel material is made, and an end links to each other with sampling valve by standard K F16 flange, and an end links to each other by standard K F25 flange and the sample introduction pipeline of finding time, and end usefulness standard K F8 flange links to each other with the sample introduction gas cylinder; Sample introduction pipeline one end of finding time links to each other with the sample introduction interface by standard K F25 flange, and the other end links to each other by standard K F25 flange and the mass spectrum chamber pipeline of finding time.
The fine pumping system as shown in Figure 1, it is made up of find time pipeline, molecular pump 2 and mechanical pump of push-pull valve, molecular pump 1, mass spectrum chamber.Push-pull valve is connected with molecular pump 1 with mass spectrum chamber respectively by standard C F250 flange; The speed of evacuation of molecular pump 1 is 450l/s, and the air intake end links to each other with push-pull valve by standard C F250 flange, and the gas outlet end links to each other by standard K F25 flange and the mass spectrum chamber pipeline of finding time; The mass spectrum chamber three-port structure that the selection for pipeline stainless steel material is made of finding time links to each other with molecular pump 1, molecular pump 2 and the sample introduction pipeline of finding time respectively by standard K F25 flange; The speed of evacuation of molecular pump 2 is 110l/s, and the air intake end links to each other by KF25 flange and the mass spectrum chamber pipeline of finding time, and the gas outlet end links to each other with mechanical pump by standard K F25 flange; The speed of evacuation of mechanical pump is 4l/s, and the air intake end links to each other with molecular pump 2 by standard K F25 flange.
Control desk is shown in Figure 1, is made up of molecular pump 1 control power supply, molecular pump 2 control power supplys, system's switch board.Molecular pump 1 control power supply is installed in system's switch board by screw retention; Molecular pump 2 control power supplys are installed in system's switch board by screw retention, and are positioned at the below of molecular pump 1 control power supply; System's switch board adopts stainless steel material to make, concrete size is formulated as required, put on its panel computing machine and mass spectrum chamber have been installed, molecular pump 1 control power supply, molecular pump 2 control power supplys, push-pull valve, molecular pump 1, mass spectrum chamber find time pipeline, molecular pump 2 and mechanical pump have been installed in inside.
Computing machine is selected general portable computer for use as shown in Figure 1, requires to have the RS232 data-interface, need during use by having the RS232 interface data line with linked to each other by the school quadrupole mass spectrometer, will be installed on computers by the analysis software of school quadrupole mass spectrometer before the calibration.
Principle of work of the present utility model is: utilize sampling system that known component content is provided in mass spectrum chamber, and the gas of pressure stability, by the school quadrupole mass spectrometer mass spectrum chamber gas composition content is scanned, mass spectrum chamber is interior by the ion flow intensity of school component gases and nitrogen gas when obtaining calibration, mass spectrograph is measured the concentration ratio by two kinds of gas composition content in the ratio result of the ion flow intensity of school component gases and nitrogen gas and the sample introduction mixed gas that obtains compare, thereby obtain by the calibration factor of school gas to nitrogen.
The method of work of quadrupole mass spectrometer relative sensitivity calibration system the steps include:
The first step: prepare before the calibration, will be connected on the calibration system, determine the gaseous species that to be calibrated by the school quadrupole mass spectrometer, be ready to and be connected on the sampling system, start the fine pumping system mass spectrum chamber pressure is evacuated to 10 by the school quadrupole mass spectrometer
-5Below the Pa, and the fluctuation of guaranteeing mass spectrum chamber pressure is less than 2%;
Second step: mass spectrum chamber background gas composition scanning of the mass spectrum, start by the school quadrupole mass spectrometer, the gas composition indoor to mass spectrum scans, and utilizes the Computer Analysis need be by the ion flow intensity of school gas and nitrogen component gases;
The 3rd step: by the school gas sampling, open the sampling valve on the sampling system, advance in mass spectrum chamber by the school mixed gas, the sample introduction pressure control is 1 * 10
-3Pa, and guarantee that the fluctuation of mass spectrum chamber internal pressure is less than 2%;
The 4th step: mass spectrum chamber is by school gas composition scanning of the mass spectrum, starts by the school quadrupole mass spectrometer, and the gas composition indoor to mass spectrum scans, and utilizes the Computer Analysis need be by the ion flow intensity of school gas and nitrogen component gases;
The 5th step: calibration factor determines, adopt the methods analyst compared with the nitrogen ion intensity of flow by school gaseous ion intensity of flow by the school quadrupole mass spectrometer to certain by the calibration factor of school gas, specifically adopt formula (1) to calculate.
In the formula:
A
W-by the school quadrupole mass spectrometer to by the calibration factor of school component gases;
I
W-by school component gases sample introduction ion flow intensity, A;
I
W0-by school component gases background ions intensity of flow, A;
I
N-nitrogen component gases sample introduction ion flow intensity, A;
I
N0-nitrogen component gases background ions intensity of flow, A;
C
WIn-sample introduction the gas by school gas composition concentration content, %;
C
NNitrogen component gases concentration content in the-sample introduction gas, %.
The utility model advantage compared with prior art is: the utility model is because employing high precision vacuum pressure variable valve adds the sample introduction structure of gas scattering ball, the sample introduction pressure stability when having guaranteed calibration; The bimolecular pump of selecting for use molecular pump 1 to add molecular pump 2 structure of bleeding can obtain to calibrate needed extra-high vacuum, reduces in the mass spectrum chamber background residual gas to the influence of calibration result; Adopt sensitive relatively Calibration Method, absolute sensitivity changes greatlyyer in time when having reduced quadrupole mass spectrometer and measuring, and irregular governed shortcoming improves the accuracy of calibration result.
Principle of work of the present utility model is: utilize sampling system that known component content is provided in mass spectrum chamber, and the gas of pressure stability, by the school quadrupole mass spectrometer mass spectrum chamber gas composition content is scanned, mass spectrum chamber is interior by the ion flow intensity of school component gases and nitrogen gas when obtaining calibration, mass spectrograph is measured the concentration ratio by two kinds of gas composition content in the ratio result of the ion flow intensity of school component gases and nitrogen gas and the sample introduction mixed gas that obtains compare, thereby obtain by the calibration factor of school gas to nitrogen.
Description of drawings
Fig. 1 is a theory of constitution block diagram of the present utility model.
Among the figure: 1-molecular pump 1 control power supply, 2-molecular pump 2 control power supplys, 3-system switch board, 4-computing machine, 5-are by school quadrupole mass spectrometer, 6-system works platform, 7-mass spectrum chamber, 8-high vacuum pressure measuring gage, 9-scattering ball, 10-sample channel, 11-sampling valve, 12-sample introduction gas interface, 13-sample introduction find time pipeline, 14-push-pull valve, 15-molecular pump 1,16-mass spectrum chamber find time pipeline, 17-molecular pump 2,18-mechanical pump.
Embodiment
As shown in Figure 1, be system architecture synoptic diagram of the present utility model, it is by molecular pump 1 control power supply (1), molecular pump 2 control power supplys (2), system's switch board (3), computing machine (4), formed by school quadrupole mass spectrometer (5), system works platform (6), mass spectrum chamber (7), high vacuum pressure measuring gage (8), scattering ball (9), sample channel (10), sampling valve (11), sample introduction gas interface (12), sample introduction the find time pipeline (16), molecular pump 2 (17), mechanical pump (18) of pipeline (13), push-pull valve (14), molecular pump 1 (15), mass spectrum chamber of finding time.
This calibration system workflow is:
The first step: prepare before the calibration, to be connected on the calibration system by four utmost point school mass spectrographs (5), the definite gaseous species that will be calibrated by the school quadrupole mass spectrometer, be ready to and be connected on the sample introduction gas interface (12) of sampling system, open push-pull valve (14), start mechanical pump (18), molecular pump 1 (15), molecular pump 2 (17) and high vacuum pressure measuring gage (8) successively, mass spectrum chamber (7) pressure is evacuated to 10
-5Below the Pa, and the fluctuation of guaranteeing mass spectrum chamber pressure is less than 2%;
Second step: mass spectrum chamber background gas composition scanning of the mass spectrum, start by school quadrupole mass spectrometer (5), the gas composition in the mass spectrum chamber (7) is scanned, utilizing computing machine (4) to analyze need be by the ion flow intensity of school gas and nitrogen component gases;
The 3rd step: by the school gas sampling, open the sampling valve (11) on the sampling system, advance by the school mixed gas in mass spectrum chamber (7), the sample introduction pressure control is 1 * 10
-3Pa, and guarantee that the fluctuation of mass spectrum chamber internal pressure is less than 2%;
The 4th step: mass spectrum chamber is started by school quadrupole mass spectrometer (5) by school gas composition scanning of the mass spectrum, and the gas composition in the mass spectrum chamber (7) is scanned, and utilizing computing machine (4) to analyze need be by the ion flow intensity of school gas and nitrogen component gases;
The 5th step: calibration factor determines, adopt the methods analyst compared with the nitrogen ion intensity of flow by school gaseous ion intensity of flow by the school quadrupole mass spectrometer to certain by the calibration factor of school gas, specifically adopt formula
(1) calculates.
In the formula:
A
W-by the school quadrupole mass spectrometer to by the calibration factor of school component gases;
I
W-by school component gases sample introduction ion flow intensity, A;
I
W0-by school component gases background ions intensity of flow, A;
I
N-nitrogen component gases sample introduction ion flow intensity, A;
I
N0-nitrogen component gases background ions intensity of flow, A;
C
WIn-sample introduction the gas by school gas composition concentration content, %;
C
NNitrogen component gases concentration content in the-sample introduction gas, %.
The 6th step: when calibration finishes, close sampling valve (11) successively, by quadrupole mass spectrometer (5), high vacuum pressure measuring gage (8), push-pull valve (14), molecular pump 2 (17), molecular pump 1 (15) and mechanical pump (18).
For accurately can repeating of calibration result with～the five step of above-mentioned second step of calculating calibration uncertainty.
Claims (8)
1, quadrupole mass spectrometer relative sensitivity calibration system, it is characterized in that: this system is by by school quadrupole mass spectrometer (5), mass spectrum chamber (7), high vacuum pressure measuring gage (8), sampling system, the fine pumping system, control desk and computing machine (4) are formed, the mixed gas of known component content is provided in mass spectrum chamber by sampling system, by the school quadrupole mass spectrometer the indoor sample introduction gas composition content of mass spectrum is measured, computing machine utilizes known gas component content and is analyzed by the gas composition content measurement result of school quadrupole mass spectrometer, obtains by the school quadrupole mass spectrometer by the calibration factor of school gas and calibration uncertainty.
2. quadrupole mass spectrometer relative sensitivity calibration system according to claim 1 is characterized in that: by the school quadrupole mass spectrometer is to be connected on the mass spectrum chamber by standard C F35 flange, adopts the data line that has the RS232 interface to link to each other with computing machine; If by the interface shape of school quadrupole mass spectrometer is not standard C F35 flange-interface, need requirement processing crossover sub according to concrete model.
3. quadrupole mass spectrometer relative sensitivity calibration system according to claim 1 is characterized in that: mass spectrum chamber adopts spherical structure, makes of stainless steel material, and size can be according to concrete needs design; Leave high vacuum pressure measuring gage (8) flange-interface at its top, adopt standard C F250 flange to link to each other with push-pull valve (14) in the bottom, symmetry leaves by the flange-interface of the flange-interface of school quadrupole mass spectrometer (5) and sample channel (10) at the place, equator of ball.
4. quadrupole mass spectrometer relative sensitivity calibration system according to claim 1 is characterized in that: the high vacuum pressure measuring gage links to each other with mass spectrum chamber (5) by standard K F25 flange, and the pressure measurement range requirement of rule is: 1 * 10
-1Pa～1 * 10
-7Pa, calibration uncertainty require less than 10%, can select Penning gauge or capacitor thin film rule for use.
5. quadrupole mass spectrometer relative sensitivity calibration system according to claim 1 is characterized in that: sampling system is made up of scattering ball (9), sample channel (10), sampling valve (11), sample introduction interface (12) and the sample introduction pipeline (13) of finding time; Scattering ball (9) is selected the stainless steel material manufacturing for use, is spherical structure, and the aperture that the surface has evenly distributed 128 diameter phi 1mm adopts the mode of welding to link to each other with sample channel (10); Sample channel (10) is selected the stainless steel material manufacturing for use, and diameter, length are determined according to the size of mass spectrum chamber; Mounting means is that an end adopts welded structure to link to each other with sampling valve, and the other end adopts counter flange, links to each other with the scattering ball by the mode of welding, and adopts the technology of laser boring to have aperture on the counter flange; Sampling valve (11) is selected high precision vacuum pressure variable valve for use, and an end links to each other with sample channel (10) by the mode of welding, and the other end links to each other with sample introduction interface (12) by flange; Sample introduction interface (12) is the three-port structure that stainless steel material is made, and an end links to each other with sampling valve (11) by flange, and an end links to each other by flange and the sample introduction pipeline (13) of finding time, and end usefulness flange links to each other with the sample introduction gas cylinder; Sample introduction pipeline (13) one ends of finding time link to each other with the sample introduction interface by flange, and the other end links to each other by standard K F25 flange and the mass spectrum chamber pipeline (16) of finding time.
6. quadrupole mass spectrometer relative sensitivity calibration system according to claim 1 is characterized in that: the fine pumping system is made up of find time pipeline (16), molecular pump 2 (17) and mechanical pump (18) of push-pull valve (14), molecular pump 1 (15), mass spectrum chamber; Push-pull valve (14) is connected with molecular pump 1 (15) with mass spectrum chamber (7) respectively by flange; The speed of evacuation of molecular pump 1 (15) is 450l/s, and the air intake end links to each other with push-pull valve (14) by flange, and the gas outlet end links to each other by flange and the mass spectrum chamber pipeline (16) of finding time; The mass spectrum chamber three-port structure that pipeline (16) selects for use stainless steel material to make of finding time links to each other with molecular pump 1 (15), molecular pump 2 (17) and the sample introduction pipeline (13) of finding time respectively by flange; The speed of evacuation of molecular pump 2 (17) is 110l/s, and the air intake end links to each other by flange and the mass spectrum chamber pipeline (16) of finding time, and the gas outlet end links to each other with mechanical pump (18) by flange; The speed of evacuation of mechanical pump (18) is 4l/s, and the air intake end links to each other with molecular pump 2 (17) by flange.
7. quadrupole mass spectrometer relative sensitivity calibration system according to claim 1 is characterized in that: control desk is made up of molecular pump 1 control power supply (1), molecular pump 2 control power supplys (2), system's switch board (3); Molecular pump 1 control power supply (1) is installed in system's switch board (3) by screw retention; Molecular pump 2 control power supplys (2) are installed in system's switch board (3) by screw retention, and are positioned at the below of molecular pump 1 control power supply (1); System's switch board (3) adopts stainless steel material to make, concrete size is formulated as required, put on its panel computing machine (4) and mass spectrum chamber (7) have been installed, molecular pump 1 control power supply (2), molecular pump 2 control power supplys (2), push-pull valve (14), molecular pump 1 (15), mass spectrum chamber find time pipeline (16), molecular pump 2 (17) and mechanical pump (18) have been installed in inside.
8. quadrupole mass spectrometer relative sensitivity calibration system according to claim 7, it is characterized in that: computing machine is selected general portable computer for use, requirement has the RS232 data-interface, need during use by having the RS232 interface data line with linked to each other by the school quadrupole mass spectrometer, will be installed on computers by the analysis software of school quadrupole mass spectrometer before the calibration.
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| Application Number | Priority Date | Filing Date | Title |
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| CNU2007201910211U CN201152868Y (en) | 2007-12-28 | 2007-12-28 | Relative response calibration system for four polar mass spectra gauge |
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| Application Number | Priority Date | Filing Date | Title |
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| CNU2007201910211U CN201152868Y (en) | 2007-12-28 | 2007-12-28 | Relative response calibration system for four polar mass spectra gauge |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101470101B (en) * | 2007-12-28 | 2011-12-21 | 中国航天科技集团公司第五研究院第五一〇研究所 | Relative sensitivity calibration system for quadrupole mass spectrometer |
| CN102608343A (en) * | 2012-03-02 | 2012-07-25 | 中国科学院过程工程研究所 | Gas stable-pressure and quantitative rarefaction component and application thereof |
| CN101726532B (en) * | 2009-12-15 | 2013-01-02 | 中国计量科学研究院 | Preparation method of correction sample of mass spectrometer |
| CN102928154A (en) * | 2012-11-27 | 2013-02-13 | 中国航天科技集团公司第五研究院第五一〇研究所 | Method for reducing error in polar altitude vacuum measurement of ESD (Electro Simulated Desorption) neutral particles |
| CN103308250A (en) * | 2013-04-24 | 2013-09-18 | 兰州空间技术物理研究所 | Device for detecting vacuum performance of low-temperature and heat-insulating pressure container |
-
2007
- 2007-12-28 CN CNU2007201910211U patent/CN201152868Y/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101470101B (en) * | 2007-12-28 | 2011-12-21 | 中国航天科技集团公司第五研究院第五一〇研究所 | Relative sensitivity calibration system for quadrupole mass spectrometer |
| CN101726532B (en) * | 2009-12-15 | 2013-01-02 | 中国计量科学研究院 | Preparation method of correction sample of mass spectrometer |
| CN102608343A (en) * | 2012-03-02 | 2012-07-25 | 中国科学院过程工程研究所 | Gas stable-pressure and quantitative rarefaction component and application thereof |
| CN102928154A (en) * | 2012-11-27 | 2013-02-13 | 中国航天科技集团公司第五研究院第五一〇研究所 | Method for reducing error in polar altitude vacuum measurement of ESD (Electro Simulated Desorption) neutral particles |
| CN102928154B (en) * | 2012-11-27 | 2014-05-28 | 中国航天科技集团公司第五研究院第五一〇研究所 | Method for reducing error in polar altitude vacuum measurement of ESD (Electro Simulated Desorption) neutral particles |
| CN103308250A (en) * | 2013-04-24 | 2013-09-18 | 兰州空间技术物理研究所 | Device for detecting vacuum performance of low-temperature and heat-insulating pressure container |
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Granted publication date: 20081119 Termination date: 20100128 |