CN110085504A - A kind of ion source system and miniaturization mass spectrograph based on aperture in-situ sampling interface - Google Patents
A kind of ion source system and miniaturization mass spectrograph based on aperture in-situ sampling interface Download PDFInfo
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- CN110085504A CN110085504A CN201910383449.3A CN201910383449A CN110085504A CN 110085504 A CN110085504 A CN 110085504A CN 201910383449 A CN201910383449 A CN 201910383449A CN 110085504 A CN110085504 A CN 110085504A
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- ion source
- aperture
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- sample
- source
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
Abstract
The invention discloses a kind of ion source system based on aperture in-situ sampling interface and miniaturization mass spectrographs, and miniaturization mass spectrograph is using ion source system of the present invention as ion source.Only with vacuum ionic source, wherein vacuum ionic source is connect with sample to be tested by aperture, is applicable to the detection of gaseous sample.Mass spectrograph provided by the invention is using aperture as in-situ sampling interface, its conductance is kept constant at work, quantitatively calibrating can be carried out to the mass discrimination in sampling process, it is short to sample transmission path, it therefore can be with quick response, amount of ions in detection device can be increased using internal ionization, and the stability that continuous sample introduction guarantees vacuum degree may be implemented, improve mass spectrometric scanning speed.
Description
Technical field
The present invention relates to mass spectral analysis fields, and in particular to a kind of ion source system of the in-situ sampling interface based on aperture
And miniaturization mass spectrograph.
Background technique
Mass spectrograph is a kind of instrument that can measure mixed gas partial pressure.In Homeland Security, environment measuring, space probation,
Medical treatment & health etc. has a wide range of applications.Mass spectrograph is mainly by ionization device, detector and ion binding structure composition.It presses
Quadrupole mass spectrometer, ion trap mass spectrometer, time of-flight mass spectrometer etc. are broadly divided into according to structure and principle.
In recent years, since the demand analyzed in real time on-line quick detection and scene is more and more, and mass spectrograph is minimized
The demand easy to carry that can satisfy field assay and one of the research hotspot for becoming international field of mass spectrometry.The interface of in-situ study
Excessively high air pressure is one of major limitation of small spectrometer.Since the exhaust capacity of small spectrometer is limited, it is therefore necessary to will be into
Enter the gas flow in vacuum system and drops to extremely low, in-situ sampling interface current limiting and the big shadow of gas transport two in a mass spectrometer
It rings.It can be used for minimizing the discontinuous atmospheric pressure interface for only releasing university's development from sufferings of mass spectrograph in-situ sampling interface so far
With continuity atmospheric pressure interface two ways.Noncontinuity atmospheric pressure interface is in order to guarantee that vacuum level requirements must be with discontinuous
Mode sample introduction, sample injection time is shorter, reduces scanning speed and system stability, and continuity atmospheric pressure interface is made using capillary
For interface element, continuous sample introduction can be carried out, but increases transmission path, therefore sample losses are high, the response time is longer.Mesh
Before until, miniaturization mass spectrograph is there are two types of Ionization mode: first is that outer ion, second is that internal ionization.Internal ionization
Be only used for gaseous sample, and outer ion due to ion transmission efficiency and vacuum degree requirement in miniaturization mass spectrograph very
It is few to use.
Summary of the invention
To overcome existing miniaturization mass spectrograph in-situ sampling interface surface sweeping speed slow, system stability difference or transmission path are long
A series of technological deficiencies such as the response time is slow, find a kind of wider array of in-situ sampling interface system of applicability, the purpose of the present invention
It is to provide a kind of ion source system based on aperture in-situ sampling interface；Another purpose of the invention is to provide a kind of miniaturization
Mass spectrograph.
The ion source system of in-situ sampling interface provided by the invention, including vacuum ionic source, wherein the vacuum ionic
Source upstream is connected with sample to be detected.
In above-mentioned ion source system, the vacuum ionic source is connected with the sample to be detected by aperture.
Preferably, the aperture selects graphene aperture, is in molecular flow condition in sampling process always, and conductance value is protected
It holds constant.
The conductance value of the aperture is designed according to gas sampled pressure, so that conductance value is constant in sampling process, it is full simultaneously
Sufficient mass spectrograph working vacuum degree requirement.
The conductance of aperture and the required gross area are determining in the following way:
The effective pumping speed of vacuum pump is Se, and it is Pv that vacuum chamber, which mentions internal pressure, and the pressure atmosphere of sample to be tested is Po, small
The conductance C in hole.When system reaches it is stable when, due to entered by aperture gas flow inside vacuum cavity with by vacuum pumping
Gas flow out is equal:
C (Po-Pv)=SePv (1)
By measuring the numerical value of other three parameters, orifice conductance value required for can obtaining.
When fluidised form is molecular flow, the conductance C of aperture are as follows:
R is ideal gas constant in formula, and T is temperature, and M is gas molecule relative molecular mass, by bring into conductance value with
And other known parameters, the gross area A of aperture required for can obtainingO。
Vacuum ionic source system be electron impact ion source, plasma discharge ionization source, glow discharge electronics Hong
Hit ion source or ultraviolet lamp discharge ionization source.
Miniaturization mass spectrograph provided by the invention includes vacuum ionic source, vacuum cavity and extract system, wherein described
Vacuum ionic source uses described in any item vacuum ionic sources system of above technical scheme.
In above-mentioned mass spectrograph, the vacuum ionic source is set in the mass spectrometric vacuum cavity.
In-situ sampling interface ion source system provided by the invention and corresponding miniaturization mass spectrograph utilize aperture for the first time
As in-situ sampling interface, conductance is kept constant at work, can be determined the mass discrimination in sampling process
Amount calibration, sampling transmission path is short, therefore can increase the number of ions in detection device using internal ionization with quick response
Amount.
In mass spectrograph of the invention, since the conductance of aperture can be met with very little, the vacuum pump of small pumping speed
The requirement of vacuum, and the stability that continuous sample introduction guarantees vacuum degree may be implemented, improve mass spectrometric scanning speed.
Miniaturization mass spectrograph of the invention is on the basis of existing, it is only necessary to which doing a small amount of adjustment can be obtained by, and be easy to
Processing and manufacturing, has broad application prospects.
Detailed description of the invention
Fig. 1 is that second of embodiment provided by the invention minimizes mass spectrometric structural schematic diagram；
Wherein, label is described as follows in attached drawing: 1- graphene in-situ sampling interface, 2- vacuum cavity, 3- detector, 4- are true
Empty pump, 5- mass analyzer, 6- vacuum ionic source.
Specific embodiment
To keep the purpose of the present invention, technical solution and advantage more clear, the present invention is described below in conjunction with attached drawing
Embodiment technical solution.By reading the following detailed description of the preferred embodiment, various other advantages and benefits
It will become apparent to those of ordinary skill in the art.Described embodiment is a part of embodiment party of the invention
Formula, rather than whole embodiments.Described embodiment is used only for being illustrated diagram, rather than to the present invention
Range limitation.Based on embodiments of the present invention, those skilled in the art are not being made the creative labor
Under the premise of all other embodiments for being obtained, shall fall within the protection scope of the present invention.
The first embodiment of the invention provides a kind of ion source system of in-situ sampling interface, the ion source system
For vacuum ionic source, sample connection downstream vacuum inside cavity in situ is arranged in vacuum ionic source.
When using the ion source system, sample to be tested is directly sampled in situ, enters vacuum from in-situ sampling interface
Inside cavity is ionized in vacuum ionic source subsequently into vacuum ionic source, the sample of available ionization.So
Analysis detection is carried out to sample composition afterwards.
Other possess fixed stream by graphene aperture etc. for vacuum ionic source and sample to be tested as a preferred technical solution,
The aperture led is attached.
The conductance of aperture and the required gross area are determining in the following way:
The effective pumping speed of vacuum pump is Se, and it is Pv that vacuum chamber, which mentions internal pressure, and the pressure atmosphere of sample to be tested is Po, small
The conductance C in hole.When system reaches it is stable when, due to entered by aperture gas flow inside vacuum cavity with by vacuum pumping
Gas flow out is equal:
C (Po-Pv)=SePv (1)
By measuring the numerical value of other three parameters, orifice conductance value required for can obtaining.
When fluidised form is molecular flow, the conductance C of aperture are as follows:
R is ideal gas constant in formula, and T is temperature, and M is gas molecule relative molecular mass, by bringing conductance value into
And other known parameters, the gross area A of aperture required for can obtainingO.Graphene is small as a preferred technical solution,
Hole element can choose the graphene with 2nm uniform pore, and the thickness magnitude of graphene, can be from vacuum to big in an angstrom magnitude
Molecular flow region is always worked under air pressure conditions.
As a preferred technical solution, vacuum ionic source can be existing vacuum ionic source any one, vacuum from
Component system includes but is not limited to electron impact ion source, plasma discharge ionization source, glow discharge electron impact ion source
Or ultraviolet lamp discharge ionization source.
Second of embodiment of the invention provides a kind of miniaturization mass spectrograph, as shown in Figure 1, should be in situ based on aperture
The miniaturization mass spectrograph of the vacuum ionic source system of sample connection includes vacuum cavity 2, and vacuum cavity 2 is internally provided with detector
3 and mass analyzer 5, mass analyzer 5 is internally provided with vacuum ionic source 6 equal conventional analytical equipment and detection device, very
Vacuum degree required for inside cavity body is provided by the vacuum pump 4 of small pumping speed, and vacuum ionic source 6 and sample to be tested pass through AAO original
Position sample connection 1 is connected.
Graphene pinhole element can choose with 2nm uniform pore, the thickness of graphene as a preferred technical solution,
Measurement level in an angstrom magnitude, can from vacuum to atmospheric pressure under always work at molecular flow region.
As a preferred technical solution, vacuum ionic source can be existing vacuum ionic source any one, vacuum from
Component system includes but is not limited to electron impact ion source, plasma discharge ionization source, glow discharge electron impact ion source
Or ultraviolet lamp discharge ionization source.
When carrying out test sample using above-mentioned miniaturization mass spectrograph, sample to be tested passes through graphene aperture in-situ sampling interface
1 enters inside vacuum cavity 2, ionizes subsequently into vacuum ionic source 6 to sample to be tested, and the ion ionized is first
It is introduced into mass analyzer 5, is analyzed subsequently into detector 3, is detected.
Claims (7)
1. a kind of ion source system of the in-situ sampling interface based on aperture, including vacuum ionic source, which is characterized in that described true
Empty ion source is connected by in-situ sampling interface with sample to be tested.
2. ion source system according to claim 1, which is characterized in that the vacuum ionic source and the sample to be tested are logical
Small holes are connected.
3. ion source system according to claim 2, which is characterized in that the aperture selection includes but is not limited to aperture
For the graphene pinhole element of 2nm, the thickness magnitude of graphene is constant from vacuum to atmospheric pressure conductance value in an angstrom magnitude.
4. ion source system according to claim 1-3, which is characterized in that the vacuum ionic source is banged for electronics
Hit ion source, plasma discharge ionization source, glow discharge electron impact ion source or ultraviolet lamp discharge ionization source.
5. a kind of miniaturization mass spectrograph, including ion source, vacuum cavity, which is characterized in that the ion source is wanted using right
Seek the described in any item ion source systems of 1-4.
6. miniaturization mass spectrograph according to claim 5, which is characterized in that vacuum ionic source in the ion source system
It is connected with sample to be tested by aperture.
7. miniaturization mass spectrograph according to claim 5, which is characterized in that the aperture selection includes but is not limited to hole
Diameter is the graphene pinhole element of 2nm, and the thickness magnitude of graphene is constant from vacuum to atmospheric pressure conductance value in an angstrom magnitude.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910383449.3A CN110085504B (en) | 2019-05-09 | 2019-05-09 | Ion source system based on small-hole in-situ sampling interface and miniaturized mass spectrometer |
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| CN201910383449.3A CN110085504B (en) | 2019-05-09 | 2019-05-09 | Ion source system based on small-hole in-situ sampling interface and miniaturized mass spectrometer |
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| CN110085504B CN110085504B (en) | 2022-02-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111665102A (en) * | 2020-05-13 | 2020-09-15 | 中国科学院微电子研究所 | Quick nondestructive sampling device and sampling method for low-vacuum gas |
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| EP0962958A1 (en) * | 1998-06-01 | 1999-12-08 | The Institute Of Physical & Chemical Research | Ion scattering spectrometer |
| EP2378539A2 (en) * | 2010-04-19 | 2011-10-19 | Hitachi High-Technologies Corporation | Mass spectrometer |
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| CN104465296A (en) * | 2013-09-13 | 2015-03-25 | 岛津分析技术研发（上海）有限公司 | Ion transmission apparatus and ion transmission method |
| CN104576287A (en) * | 2013-10-16 | 2015-04-29 | 北京理工大学 | Ion source system and mass spectrometer for atmospheric pressure interface |
| CN104637774A (en) * | 2013-11-08 | 2015-05-20 | 中国科学院大连化学物理研究所 | Electrospray ion leading-in device |
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| US20170263427A1 (en) * | 2014-05-22 | 2017-09-14 | W. Henry Benner | Instruments for measuring ion size distribution and concentration |
| CN108439377A (en) * | 2018-05-18 | 2018-08-24 | 浙江大学 | It is a kind of to cooperate with processing organic liquid waste using non-thermal plasma trap and prepare the device and method of graphene |
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2019
- 2019-05-09 CN CN201910383449.3A patent/CN110085504B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0962958A1 (en) * | 1998-06-01 | 1999-12-08 | The Institute Of Physical & Chemical Research | Ion scattering spectrometer |
| EP2378539A2 (en) * | 2010-04-19 | 2011-10-19 | Hitachi High-Technologies Corporation | Mass spectrometer |
| CN102800554A (en) * | 2012-09-02 | 2012-11-28 | 王利兵 | Multimode ionization method |
| CN104465296A (en) * | 2013-09-13 | 2015-03-25 | 岛津分析技术研发（上海）有限公司 | Ion transmission apparatus and ion transmission method |
| CN104576287A (en) * | 2013-10-16 | 2015-04-29 | 北京理工大学 | Ion source system and mass spectrometer for atmospheric pressure interface |
| CN104637774A (en) * | 2013-11-08 | 2015-05-20 | 中国科学院大连化学物理研究所 | Electrospray ion leading-in device |
| US20170263427A1 (en) * | 2014-05-22 | 2017-09-14 | W. Henry Benner | Instruments for measuring ion size distribution and concentration |
| CN106340437A (en) * | 2015-07-09 | 2017-01-18 | 株式会社岛津制作所 | Mass spectrometer and method used to reduce ion loss and post-stage vacuum load |
| CN105702553A (en) * | 2016-04-19 | 2016-06-22 | 东华理工大学 | Ion mobility spectrometer and carrier gas flow control method thereof |
| CN108439377A (en) * | 2018-05-18 | 2018-08-24 | 浙江大学 | It is a kind of to cooperate with processing organic liquid waste using non-thermal plasma trap and prepare the device and method of graphene |
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| CN111665102A (en) * | 2020-05-13 | 2020-09-15 | 中国科学院微电子研究所 | Quick nondestructive sampling device and sampling method for low-vacuum gas |
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