CN108400080A - A kind of mass ions source device under the conditions of low vacuum - Google Patents
A kind of mass ions source device under the conditions of low vacuum Download PDFInfo
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- CN108400080A CN108400080A CN201810139214.5A CN201810139214A CN108400080A CN 108400080 A CN108400080 A CN 108400080A CN 201810139214 A CN201810139214 A CN 201810139214A CN 108400080 A CN108400080 A CN 108400080A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
- H01J49/142—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using a solid target which is not previously vapourised
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/24—Vacuum systems, e.g. maintaining desired pressures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
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- Electron Tubes For Measurement (AREA)
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Abstract
The invention belongs to mass spectral analysis technical field of measurement and test, specifically relate to as the mass ions source device under the conditions of a kind of low vacuum.The device includes：One vacuum system, and be set in the vacuum system ion source, example platform, ion Transmission system, mass of ion analyzer, ion detector；Multi-stage vacuum difference function may be implemented in the vacuum system；The ionic bombardment generated by ion source is to sample to be tested surface, and sample to be tested occurs to sputter and be desorbed after ion collision to generate gas phase sample ion, to realize sample to be tested ionization process；The sample to be tested ion of generation is entered by ion Transmission system in mass of ion analyzer；The use of vacuum system can improve ion-generating efficiencies, the loss in ion transmission process be reduced, to improve the detection sensitivity of ion transmission efficiency and whole system.
Description
Technical field
The invention belongs to mass spectral analysis technical field of measurement and test, and in particular to one kind generating sample ions under the conditions of low vacuum
With the sample ionization ion source device of transmission ion.
Background technology
Mass spectrograph is one of most important analysis science instrument in present analysis testing field, is widely used in modern science
It is each in life science, food security, environment pollution detection, national defense safety, aerospace, medicine etc. in research and production activity
Indispensable role is played in the micro or trace materials detection field of kind, it has also become in modern development in science and technology and daily life
Indispensable analysis tool.
In a mass spectrometer, ion source is most crucial one of critical component, and main function is to ionize sample to be tested
It is analyzed afterwards into mass analyzer, the fast development of ion source, decides that mass spectrograph obtains widely in many-sided field
Using with popularization.Therefore, electron spray ionisation ion source（Electrospray ionization, ESI）And ground substance assistant laser
Ion source is desorbed（Matrix-assisted laser desorption ionization, MALDI）Invention, mass spectrograph exists
The development of being used widely in bioprotein field.
However in conventional analytic process, the preprocessing process that needs to take much time before sample introduction system
In, to influence real-time, quick analysis of the analytical technique of mass spectrum in every field.In document《Science》Volume 306, page 471
（2004）In teach the spray droplet generated using electron spray ionisation technology and be applied directly to showing for sample under atmospheric pressure
It interacts with sample molecule and generates ion, here it is the Desorption Electrospray Ionizations under normal pressure（DESI）.Then also occur
The analytical technology of some other direct sample analysis, such as Direct Analysis in Real Time（DART）《Analytical Chemistry》77
Volume, page 2297（2005）；Desorb atmospheric pressure photoionization（DAPPI）《Analytical Chemistry》Volume 79, page 7867
（2007）Etc. a series of direct analytical technology of normal pressures, tentatively realizes sample and efficiently quickly analyze.
At present in biomolecule analysis, such as protein molecule, the macromoleculars domain analysis such as polypeptide, use be mostly
Ion source under normal pressure, such as ESI, DESI, DART plasma source, but since ion Transmission system and mass analyzer work all exist
Have under certain vacuum degree condition, ion source under normal pressure has a vacuum with ion Transmission system and mass of ion analyzer
Interface, due to ensureing that mass of ion analyzer reaches required vacuum degree, vacuum interface must be one, and there are one limitations
The micro hole of gas flow.This micropore one of is led to the problem of be exactly the ion that is generated by ion source under normal pressure enter vacuum it
Before, about 90% or more ion is blocked in outside vacuum and loses.In addition, since ion is in normal pressure and environmental molecules
The losses of ions that frequent impact will also result in；The impurity such as the solvent molecule that some are not removed are also admixed, can directly be reduced the later stage
Analysis detection sensitivity.
In over the years, people have invented the technology of the auxiliary desolvation of a variety of electron sprays to improve ionization effect
Rate, such as the heating capillary desolvation technology that United States Patent (USP) US4977320 is proposed, which adds one in the periphery of capillary
The heat conduction shielding cylinder of a metal reaches the temperature for improving capillary, realizes desolvation by the heating to heat conduction shielding cylinder
Effect, improves Ionization Efficiency, which is widely used in the commercial instrument of partial analysis instrument company at present.It is beautiful
The blowback sheath gas method desolvation technology that state patent US4861988 is proposed, testing sample solution are formed after electron spray ionisation
It during ion, while being diluted by sheath gas, forms Charged Droplet, it is most under the action of mass spectrum entrance negative direction air-flow
Solvent just volatilizees before reaching mass spectrum entrance, forms smaller electrification droplet lotus gaseous ion.Solvent is removed in order to improve sample
Effect, be blown into reversed air-flow before mass spectrum injection port, form a gas curtain, this gas curtain can make neutral structural constituent
Deviate the entrance of mass spectrum sample introduction, additionally it is possible to take away most solvent molecule, have the function of good desolvation.Use height
Pure N2 has the effect of allowing ionized gas to go solvent more preferable as auxiliary sheath gas, and the nitrogen of certain flow rate can be blown away
Most neutral particle and king-sized drop can significantly improve desolvation efficiency.
But above-mentioned method mainly uses in open type ion source under normal pressure, and complicated mixing sample is also needed
It wants cumbersome sample pretreatment process to be detached, the effect analyzed real-time described before is not achieved.Therefore, for mixed
High efficiency high sensitivity is quickly analyzed while being reached to the sample for closing object or complexity, is one of current problem to be solved.
Invention content
In view of many disadvantages and deficiency of existing ion source, to solve the above-mentioned problems, the purpose of the present invention is to propose to one
Mass ions source device under kind low vacuum improves the Ionization Efficiency of sample to realize that the real-time high-efficiency of sample is quickly analyzed
And ion transmission efficiency, loss of the ion in transmission process is reduced, the sensitivity of entire instrument system is improved.In addition, may be used also
To save cumbersome sample pretreatment process, analyze speed, Simplified analysis formality are improved.
Mass ions source device provided by the invention under the conditions of low vacuum, basic structure are as shown in Figure 1.Main packet
It includes：One vacuum system, and be set in the vacuum system ion source, example platform, ion Transmission system, mass of ion point
Parser, ion detector；Multi-stage vacuum difference function may be implemented in the vacuum system；The ion source is for generating ion；Institute
Example platform is stated for placing sample to be tested, example platform can carry out three dimensions adjusting；Ion source is with example platform at one
A angle, the angle are 0 ~ 90 degree；The ion Transmission system is used for transmission ion caused by ion source, is sent to ion
Detector, mass of ion analyzer.
In the present invention, the ionic bombardment generated by ion source to sample to be tested surface, after ion collision send out by sample to be tested
Raw sputtering and desorption generate gas phase sample ion, to realize sample to be tested ionization process；The sample to be tested ion of generation is logical
Ion Transmission system is crossed to enter in mass of ion analyzer；The use of vacuum system can improve ion-generating efficiencies, reduce
Loss in ion transmission process, to improve the detection sensitivity of ion transmission efficiency and whole system.
In the present invention, the ion source generates ion method and is：Desorption Electrospray Ionization generates the spray liquid of electrification
Drop and ion；Or for using metal capillary technology, such as using stainless steel capillary, helium is passed through in metal capillary
Or the gases such as argon gas, on the capillary table load ac high-voltage, between needle tip and sample generate electric discharge, generate sample to be tested from
Son.
In the present invention, the ion source, operating condition is low vacuum, and usually vacuum degree is 760Torr ~ 10- 3Torr。
In the present invention, adjustable three-dimensional mobile platform, according to the analysis demand during actual test, to institute
Sample to be measured carries out three-dimensional movement, obtains the detection demand of different location.
In the present invention, the ion source is in vacuum chamber, and there are one vacuum interfaces to design under normal pressure for ion, together
When the vacuum chamber there are one regulating valve control vacuum pumping speed, to adjust vacuum pressure.
In the present invention, the ion Transmission system, can be ion lens, quadrupole rod, sextupole bar, octupole bar and other
One or more combinations in multistage bar, ion funnel.
In the present invention, the mass of ion analyzer is the mass spectrometric mass analyzer of any type or Ion transfer
Spectrum.
In the present invention, the three-dimensional regulation platform also has and has heating and temperature controlling device, increases temperature for heating, improves
Sample to be tested gaseous ion.
In the present invention, the ion source have at vacuum interface auxiliary gas feed at, be mainly used for desolvation and
Assist sample to be tested gaseous ion.
In the present invention, the vacuum system is multi-level differential vacuum structure, according to ion source, ion Transmission system, matter
Vacuum degree required by contents analyzer carries out real-time control adjusting, reaches best operating condition.
In the present invention, the ion source and ion Transmission system can work under the same vacuum degree, different
It works under vacuum degree.
For example, vacuum system can be divided into primary vacuum chamber, rear class difference vacuum chamber；The ion source and ion pass
Defeated system is located in primary vacuum chamber, and the mass of ion analyzer and ion detector are located at rear class difference vacuum chamber
In；
In the present invention, one can be provided between the vacuum chamber where ion source and the vacuum chamber where ion Transmission system
A slide valve；It is arranged one between vacuum chamber where vacuum chamber and mass analyzer that can also be where ion Transmission system
A slide valve；When needing to replace detection sample in real time, slide valve can close, and the vacuum chamber where opening ion source is more
When varying product, will not have an impact to rear class vacuum, reach quick-replaceable determinand, play the effect analyzed real-time.
In the present invention, between the sample to be tested platform and ion Transmission system with an angle, the angle be 0 ~
90 degree controllable.
In the present invention, the ion Transmission system is provided with a thermostatically-controlled equipment and ventilation interface, is added with controlling gas
It is passed through after heat in the chamber where ion source and Transmission system；The gas can be one kind or two in nontoxic gas
Kind or more mixed gas, such as oxygen, carbon dioxide, sulfur hexafluoride, argon gas, xenon etc..
In the present invention, the ion source may be used as in the sample analysis of solid-state or liquid.
In the present invention, the mass of ion analyzer, Ke Yishi：Quadrupole rod mass analyzer, time of flight mass point
Parser, ion strap mass analyzer, magnetic substance contents analyzer, Fourier's cyclotron-resonance mass analyzer, orbitrap quality analyses
One kind or multiple combinations in device use.
In the present invention, the ion source and sampling device can be a kind of ion sources, can also be a variety of different ions
The arbitrary arrangement in source combines, and realizes that multiple ion sources are carried out while being analyzed to multiple similar samples or to different samples, realizes
High-throughput highly sensitive detection.
Therefore, according to the ion source device in the present invention under partial vacuum, by the ion source under open type normal pressure low true
Ion is generated under empty condition, in the case where keeping the ion source application field, improves Ionization Efficiency and ion transmission efficiency,
The sensitivity of entire analytical instrument is improved, especially in biomedical sector detection, high sensitivity plays trace detection
Important role, improve instrument uses field and efficiency, while also reducing the maintenance cost of the instrument.
Description of the drawings
Fig. 1 is the structural schematic diagram of mode device described in the embodiment of the present invention 1.
Fig. 2 is the first change schematic diagram of structure of mode device described in the embodiment of the present invention 1.
Fig. 3 is the second change schematic diagram of structure of mode device described in the embodiment of the present invention 1.
Fig. 4 is the structure third change schematic diagram of mode device described in the embodiment of the present invention 1.
Fig. 5 is the 4th change schematic diagram of structure of mode device described in the embodiment of the present invention 1.
Figure label：101 be electron spray ionisation source, and 102 be DC high-voltage power supply, and 103 be three-dimensional removable regulating platform
103,104 be ion Transmission system, and 105 be sample to be tested, and 106 for primary vacuum chamber 106,107 be throttle valve；After 108 are
Grade difference vacuum chamber, 109 be mass of ion analyzer, and 110 be slide valve；111 be vacuum interface, and 112 be heating device,
113 be ion detector, and 114 for vacuum chamber 114,115 be heating and temperature controlling device, and 116 be gas.
Specific implementation mode
Embodiment 1
Fig. 1 shows desorption ionization ion source and its schematic device under one embodiment of the invention low vacuum, in embodiment 1
In, the electron spray ionisation ion source selected under most common open type normal pressure generates the mixture of charged spray drop and ion,
Its structure contains electron spray ionisation source 101, and DC high-voltage power supply 102 of the load on the metal tube of electron spray tip waits for
The three-dimensional that sample 105 is put moves regulating platform 103, and ion Transmission system selects ion funnel 104, electron spray ionisation source
Capillary 101, sample to be tested 105, three-dimensional mobile platform 103, ion funnel 104 is all in a primary vacuum chamber 106.
The air pressure of vacuum chamber 106 is controlled there are one vacuum pump interface and throttle valves 107 106 side of vacuum chamber, according to specific
Experiment vacuum requirement is adjusted.Electron spray ionisation source capillary 101 can be 0 ~ 180 degree with 105 angle of sample to be tested, wait for test sample
At an angle with ion funnel 104, which is that 0 ~ 180 degree is controllable to product 105, in the present embodiment 1, electron spray ionisation source
Capillary 101 and 105 angle of sample to be tested are about 45 degree, and sample to be tested 105 and the angle of ion funnel 104 are about 0 degree.From
It can be fast when replacing sample to be tested 105 there are one slide valve 110 between sub- funnel 104 and rear class difference vacuum chamber 108
Speed closes slide valve 110, can protect the vacuum degree of entire rear class vacuum 108 rapidly.After replacing sample 105, it can also make
Obtain whole system rapid operation.
During 1 specific experiment of this implementation, in vacuum chamber 106, the band EFI that is generated by electron spray ionisation source 101
Spray film drop is splashed on sample to be tested 105, and sample to be tested 105 occurs sputtering after high speed drop collision and generates gaseous ion, waits for
Sample ion is analyzed by the mass analyzer 109 that ion funnel 104 enters in rear class difference vacuum chamber 108,
The ion of different mass-to-charge ratioes pops up from mass analyzer 109 detected by ion detector 113 successively.Wherein sample to be tested 105
By three-dimensional mobile platform 103 carry out angle and distance adjustment, during the experiment, can according to different samples to be tested from
The difference of sub-ization condition is observed specific signal strength to implement to adjust sample to be tested 105 and electron spray ionisation source in real time
101 and ion funnel 104 distance and angle so that experiment condition is optimal.
In cavity 106, in 104 course of work of ion funnel, in order to improve the efficiency of transmission of ion funnel, pass through vacuum
Interface 111 is passed through in the gases such as carbon dioxide or sulfur hexafluoride to the vacuum cavity 106 at 104 place of ion funnel, while at this
The heating device 112 that a temperature controllable is adjusted is connected at vacuum interface 111 to give when being passed through atmospheric carbon dioxide
The gas heats, and avoids the air pressure because of vacuum cavity 106 too low, causes the drop of 101 capillary tip of electron spray ionisation source solidifying
Gu and damaging.
It is found in the investigation of phase before this invention, after ion source generation ion under normal pressure, in the case where entering low vacuum
Ion Transmission system in, about 90% ion can be lost in this process, to directly influence whole system detection spirit
Phenomena such as sensitivity reduces, and ion signal is weak.In the content of the present invention and in specific embodiment, in low vacuum, test sample is waited for
After product 105 generate ion, ion Transmission system is entered directly into（Ion funnel 104）In, ion can be with almost 100% efficiency
It reaches in ion funnel 104, to improve Ionization Efficiency and ion transmission efficiency, further improves the spirit of whole device
Sensitivity.
Fig. 2 is a change case in 1 mode of the embodiment of the present invention, uses multistage bar as ion Transmission system 104,
The multistage bar is quadrupole rod, sextupole bar, octupole bar, ten pole bars, 12 pole bars, ten sextupole bars etc..In the vacuum where ion source
Chamber 106 is a differential configuration with the vacuum chamber 114 where ion Transmission system 104, and intermediate there are one slide valves 110.
When changing a sample, slide valve 110 is closed, it can be with quick-replaceable sample to be tested.
Fig. 3 is another change case in 1 mode of the embodiment of the present invention, and ion Transmission system 104 is ion funnel and more
The combination of grade bar improves ion transmission efficiency by different ion Transmission systems, removes neutral molecule, improves instrument system
Sensitivity.
Fig. 4 is another change case in 1 mode of the embodiment of the present invention, and one is installed in three-dimensional mobile platform 103 can
The device 115 of controllable temperature is heated, sample to be tested 105 is seated on heating device 115, for some complex samples, can pass through
Heating contributes to sample to volatilize, and improves Ionization Efficiency.
Fig. 5 is another change case in 1 mode of the embodiment of the present invention, and ion source is hollow stainless pin 101, in centre
The gases such as helium 116 or argon gas are passed through, generates and puts in load ac high-voltage 102, between needle tip and sample in stainless pin 101
Electricity generates sample to be tested ion.
In the present embodiment 1, mass analyzer 109 is specially ion strap mass analyzer, in the later stage implements change case,
Quadrupole rod mass analyzer, time-of-flight mass analyzer, ion strap mass analyzer, magnetic substance contents analyzer, Fu can be selected
In one or more in leaf cyclotron-resonance mass analyzer, orbitrap mass analyzers be applied in combination.
Claims (14)
1. the mass ions source device under the conditions of a kind of low vacuum, which is characterized in that including：One vacuum system, and be set to
Ion source, example platform, ion Transmission system in the vacuum system, mass of ion analyzer, ion detector；The vacuum system
Multi-stage vacuum difference function may be implemented in system；The ion source is for generating ion；The example platform waits for test sample for placing
Product, example platform can carry out three dimensions adjusting；At an angle with example platform, which is 0 ~ 90 degree to ion source；Institute
It states ion Transmission system and is used for transmission ion caused by ion source, be sent to ion detector, mass of ion analyzer；
Wherein, by ion source generate ionic bombardment arrive sample to be tested surface, sample to be tested occurs after ion collision sputter with
Desorption generates gas phase sample ion, to realize sample to be tested ionization process；The sample to be tested ion of generation is passed by ion
Defeated system enters in mass of ion analyzer；The use of vacuum system can improve ion-generating efficiencies, reduce ion transmission
Loss in the process, to improve the detection sensitivity of ion transmission efficiency and whole system.
2. the apparatus according to claim 1, which is characterized in that the ion source generates ion method and is：Desorption electrospray
Ionization technique generates the spray droplet and ion of electrification；Or using metal capillary technology, to be passed through in metal capillary
Helium or argon gas load ac high-voltage on the capillary, and electric discharge is generated between needle tip and sample, generate sample to be tested ion；
The ion source condition is low vacuum：Vacuum degree is 760Torr ~ 10-3Torr。
3. the apparatus according to claim 1, which is characterized in that the ion source is in vacuum chamber, and ion is derived from normal
There are one vacuum interfaces for pressure, while there are one regulating valves to control vacuum pumping speed for the vacuum chamber, to adjust vacuum pressure.
4. the apparatus according to claim 1, which is characterized in that the ion Transmission system be ion lens, quadrupole rod,
One or more combinations in sextupole bar, octupole bar and other multistage bar, ion funnels；
The mass of ion analyzer is mass spectrometric mass analyzer or ion mobility spectrometry.
5. the apparatus according to claim 1, which is characterized in that the example platform is equipped with heating and temperature controlling device, is used for
Heating increases temperature, improves sample to be tested gaseous ion.
6. the apparatus according to claim 1, which is characterized in that the ion source have at vacuum interface auxiliary gas into
Mouthful, for desolvation and auxiliary sample to be tested gaseous ion.
7. the apparatus according to claim 1, which is characterized in that the vacuum system is multi-level differential vacuum structure, root
Real-time control adjusting is carried out according to the vacuum degree required by ion source, ion Transmission system, mass analyzer, reaches best effort item
Part.
8. device according to claim 1 or claim 7, which is characterized in that the ion source and ion Transmission system is same
It works under a vacuum degree, or works under different vacuum degrees.
9. device according to claim 8, which is characterized in that the vacuum chamber where ion source and ion Transmission system institute
Vacuum chamber between setting there are one slide valve.
10. the device according to claim 1 or 9, which is characterized in that in the vacuum chamber and matter where ion Transmission system
There are one slide valves for setting between vacuum chamber where contents analyzer.
11. the apparatus according to claim 1, which is characterized in that have between the example platform and ion Transmission system
There are one angle, which is 0 ~ 90 degree controllable.
12. the apparatus according to claim 1, which is characterized in that the ion Transmission system is provided with thermostatic control dress
It sets and ventilates interface, to control in the chamber where being passed through ion source and Transmission system after gas heating；The gas be as
One or two or more kinds of mixed gas in lower gas：Oxygen, carbon dioxide, sulfur hexafluoride, argon gas, xenon.
13. the apparatus according to claim 1, which is characterized in that the mass of ion analyzer is：Quadrupole rod quality point
Parser, time-of-flight mass analyzer, ion strap mass analyzer, magnetic substance contents analyzer, the analysis of Fourier's cyclotron-resonance mass
Device, one kind in orbitrap mass analyzers or multiple combinations use.
14. the device according to one of claim 1-7,11-13, which is characterized in that the ion source is a variety of differences
The arbitrary arrangement of ion source combines, to realize that multiple ion sources carry out the same time-division to multiple similar samples or to different samples
High-throughput highly sensitive detection is realized in analysis.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810139214.5A CN108400080A (en) | 2018-02-11 | 2018-02-11 | A kind of mass ions source device under the conditions of low vacuum |
| PCT/CN2018/110778 WO2019153788A1 (en) | 2018-02-11 | 2018-10-18 | Ion source apparatus for mass spectrometry under low-vacuum condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810139214.5A CN108400080A (en) | 2018-02-11 | 2018-02-11 | A kind of mass ions source device under the conditions of low vacuum |
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| CN108400080A true CN108400080A (en) | 2018-08-14 |
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| CN201810139214.5A Pending CN108400080A (en) | 2018-02-11 | 2018-02-11 | A kind of mass ions source device under the conditions of low vacuum |
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| WO (1) | WO2019153788A1 (en) |
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| WO2019153788A1 (en) * | 2018-02-11 | 2019-08-15 | 复旦大学 | Ion source apparatus for mass spectrometry under low-vacuum condition |
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| WO2019153788A1 (en) * | 2018-02-11 | 2019-08-15 | 复旦大学 | Ion source apparatus for mass spectrometry under low-vacuum condition |
| CN109256321A (en) * | 2018-09-19 | 2019-01-22 | 清华大学 | It is a kind of to continue sample introduction atmospheric pressure interface secondary vacuum ion trap mass spectrometer |
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Application publication date: 20180814 |