CN202178233U - Atmospheric pressure interface ion source and mass spectrometer - Google Patents
Atmospheric pressure interface ion source and mass spectrometer Download PDFInfo
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- CN202178233U CN202178233U CN201120274625.9U CN201120274625U CN202178233U CN 202178233 U CN202178233 U CN 202178233U CN 201120274625 U CN201120274625 U CN 201120274625U CN 202178233 U CN202178233 U CN 202178233U
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- atmospheric pressure
- ion source
- pressure interface
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Abstract
The utility model provides an atmospheric pressure interface ion source and a mass spectrometer, wherein the atmospheric pressure interface ion source comprises a capillary tube and a repulsion electrode, the atmospheric pressure difference between the inside of the mass spectrometer and the atmosphere enables sample ions to form a sample ion flow, the sample ions are inhaled into the mass spectrometer through the capillary tube, the included angle alpha between the capillary tube and the mass analyzer of the mass spectrometer is from 80 DEG to 150 DEG, the repulsion electrode is mounted at the outer side of the included angle alpha, and the repulsion electrode is provided with a DC voltage from 110V-380V to change the flying direction of the sample ions with small kinetic energy in the sample ion flow of the capillary tube by the angle of 180 DEG-alpha and then to enable the sample ions with small kinetic energy to enter into the mass analyzer. The mass spectrometer comprises the atmospheric pressure interface ion source. In the utility model, only the stable sample ions with small kinetic energy can enter into the mass analyzer and the fogdrop remnants, etc., with large kinetic energy are effectively separated, and the atmospheric pressure interface ion source and the mass spectrometer are high in analyzing precision, excellent in sensitivity, and high in signal to noise ratio.
Description
Technical field
The utility model relates to a kind of atmospheric pressure interface ion source and mass spectrometer that is used for field of analytic instrument.
Background technology
The LC-MS system is widely used in scientific research and biological detection analysis field, and its structure mainly comprises liquid chromatograph and mass spectrometer.Wherein liquid chromatograph is used for preliminary treatment fluid sample to be detected, to form comparatively pure fluid sample.Mass spectrometer mainly comprises atmospheric pressure interface ion source and mass analyzer etc.The atmospheric pressure interface ion source comprises a charged nozzle needle, capillary and the heater that heats to capillary; Charged nozzle needle is arranged in the atmosphere; Be used to receive the purer fluid sample of handling through liquid chromatograph, and fluid sample ionization gasification is formed the charged ion of gaseous state; Capillary one end extend in the mass spectrometer, and the other end is arranged in the atmosphere, in the said mass spectrometer and the sample ions of the air pressure official post between the atmosphere after the ionization gasification form sample ions stream, and be drawn in the mass spectrometer through said capillary.In traditional atmospheric pressure interface ion source, the mass analyzer in capillary and the mass spectrometer is installed on the same center line, so ion flow flies into mass analyzer with form of straight lines.
As shown in Figure 1, voltage on the capillary 2 and nozzle needle 1 have a high-tension electricity potential difference, can utilize a high-voltage suppling power to make and keep this high-tension electricity potential difference between capillary 2 and the nozzle needle 1, can certainly between the two, keep the high-tension electricity potential difference through other modes.The spout place of nozzle needle 1 forms taylor cone by electric field action, makes fluid sample convert a large amount of drops that has electric charge to, and charged drop generation COULOMB EXPLOSION effect evaporates partial solvent, becomes littler charged droplet; These little droplets in the guiding of air-flow, wrap up in the effect taken down the formation sample ions flow into capillary 2; Solvent under the high temperature action of capillary 2 in the little droplet further is evaporated; Therefore little droplet gets in the mass analyzer through can be more and more littler in the process of capillary 2 at last.
Generally; When the fluid sample droplet changes ion flow into through capillary; Also can there be some unionized successful fluid samples,, also can have the charged droplet of some incomplete big mass-to-charge ratioes of desolvating like neutrophil granules such as impurity particle, solvent particles, solvent molecule groups.And in traditional atmospheric pressure interface ion source; All these ions, charged droplet and impurity particle, solvent particles, solvent molecule group etc. are because the inlet of the direct alignment quality analyzer of original motion direction; So can enter into mass analyzer in the lump, thereby pollute the parts such as electrode in the mass analyzer, cause the partial electrostatic accumulation; Destroy the inner ideal electric field of mass analyzer and distribute, thereby had a strong impact on mass spectrometric analysis precision and sensitivity; Droplet directly gets into mass analyzer and also can produce noise signal simultaneously, reduces mass spectrometric signal to noise ratio.In order to reduce neutrophil granules such as the impurity particle that gets into mass analyzer, solvent particles, solvent molecule group; Also be provided with blowning installation in traditional atmospheric pressure interface ion source; Sample ions stream is in the opposite direction in high temperature nitrogen direction that it blows out and the capillary; Purpose is to make the solvent in these neutrophil granules further to evaporate, and becomes the little particle of quality, to reduce the pollution to mass analyzer.Yet this can waste resources such as a large amount of nitrogen, electric energy.
The utility model content
The purpose of the utility model is to provide the atmospheric pressure interface ion source and the mass spectrometer of a kind of not impact analysis precision and sensitivity, to solve in the above-mentioned prior art owing to the ionogenic defective of atmospheric pressure interface causes analysis precision and the low technical problem of sensitivity.
For solving the problems of the technologies described above, the utility model adopts following technical scheme:
The atmospheric pressure interface ion source of the utility model; The atmospheric pressure interface ion source; Comprise that an end extend in the mass spectrometer, the other end is arranged on the capillary in the atmosphere; In the said mass spectrometer and the sample ions of the air pressure official post between the atmosphere after the ionization gasification form sample ions stream; And be drawn in the said mass spectrometer through said capillary; It is characterized in that: said atmospheric pressure interface ion source also comprises the repulsion electrode, and the angle between the center line of said center line capillaceous and mass spectrometric mass analyzer is 80 °～150 °, and said repulsion electrode is installed in the outside of said angle; Be added with 110～380 volts direct voltage on the said repulsion electrode, the electric field that this direct voltage produces gets into said mass analyzer after making 180 °-α of the heading change angle through the sample ions that kinetic energy is little in the said sample ions stream capillaceous.
Preferably, said angle is 90 °.
Said repulsion electrode surface is shaped as semi-cylindrical shape, spherical shape, ellipsoid shape, conical surface shape, frustum face shape or flat shape to said angle one side.
Have hole or slit on the said repulsion electrode, sample ions or the neutral particle big for kinetic energy pass through.
Said atmospheric pressure interface ion source also comprises the ion guides device that is installed between said repulsion electrode and the said mass analyzer.
Said ion guides device is a utmost point rod-type guiding device; Comprise being parallel to each other and that being added with voltage on the every electrode stem and being 100～400 volts, frequency is the radio-frequency current of 600 KHzs～2 megahertzes at equally distributed four of circumferencial direction, the six roots of sensation or eight electrode stems.Said ion guides device is an ion funnel; This ion funnel comprises some mutually insulateds and the battery lead plate that is arranged in parallel; The central authorities of every said battery lead plate have the through hole that supplies said sample ions to pass through, and the through hole on some electrode plate diminishes along the heading of sample ions successively; The vacuum degree in said ion funnel zone of living in is 65pa～650pa; Be added with 60～100 volts direct voltage on the battery lead plate near said repulsion electrode; Be added with 25～65 volts direct voltage on the battery lead plate near said mass analyzer; Voltage on some electrode plate successively decreases along the heading of sample ions successively, is added with alternating voltage on the said battery lead plate of each piece, and the phase difference of the alternating voltage between the adjacent two said battery lead plates in said some electrode plate is identical.
The vacuum degree in said ion funnel zone of living in is 110pa～150pa.
Direct voltage on said some electrode plate successively decreases with the mode of arithmetic progression along the heading of sample ions successively.
The mass spectrometer of the utility model comprises mass analyzer and atmospheric pressure interface ion source, and wherein, said atmospheric pressure interface ion source is the described atmospheric pressure interface ion source of the utility model.
Can know by technique scheme; Atmospheric pressure interface ion source of the utility model and mass spectrometric advantage and good effect are: owing to be provided with the repulsion electrode in the atmospheric pressure interface ion source; The electric field that the repulsion electrode produced can separate the big impurity of the little sample ions of kinetic energy and kinetic energy, micel, droplet particle etc.; Sample ions is the change of flight direction under the effect of repulsion Electrode Field, and can get into mass analyzer after changing; And impurity droplet or particle are big owing to kinetic energy, inertia is big, and the angle that heading changed under the effect of repulsion Electrode Field is littler than the angle that sample ions changed, thereby because powerful inertia can't get into mass analyzer.So in the atmospheric pressure interface ion source and mass spectrometer of the utility model; Have only stable sample ions can get into mass analyzer; And other droplet, micel, particle etc. all can't get into mass analyzer; Thereby avoided these droplets, micel, particle etc. to pollute the parts such as electrode in the mass analyzer effectively, therefore helped improving mass spectrometric analysis precision, sensitivity and signal to noise ratio.Meanwhile; In the utility model; Because the repulsion electrode just screened neutrophil granules such as the impurity particle in the sample ions stream, solvent particles, solvent molecule group before mass analyzer; Thereby blowning installation can be set, so this ability can be saved resources such as a large amount of nitrogen, electric energy.
With reference to the accompanying drawing description of a preferred embodiment, above-mentioned and other purpose of the utility model, feature and advantage will be more obvious through following.
Description of drawings
Fig. 1 representes the ionogenic structural representation of traditional atmospheric pressure interface, and it expresses fluid sample simultaneously by the change procedure in the flight course of ionization gasification back;
Fig. 2 representes the structural representation of ionogenic first embodiment of the atmospheric pressure interface of the utility model;
Fig. 3 representes the ionogenic mechanical structure sketch map of the atmospheric pressure interface of the utility model;
Fig. 4 representes the simulation drawing that sample ions is flown in the atmospheric pressure interface ion source of the utility model;
Fig. 5 representes the structural representation of ionogenic second embodiment of the atmospheric pressure interface of the utility model.
Embodiment
To combine accompanying drawing to describe the specific embodiment of the utility model in detail below.Should be noted that the embodiments described herein only is used to illustrate, be not limited to the utility model.
As shown in Figures 2 and 3, atmospheric pressure interface ion source first embodiment of the utility model mainly comprises charged nozzle needle 1, capillary 2, to the heater (not shown) and the repulsion electrode 3 of capillary heating.
Charged nozzle needle 1 can be with charged nozzle needle in the atmospheric pressure interface ion source of traditional structure identical.
Capillary 2 can be identical with the capillary 2 in the atmospheric pressure interface ion source of traditional structure, and it can be charged, also can be not charged.One end of capillary 2 is arranged in the atmosphere and is supported by porcelain bushing 8, and the other end extend in the mass spectrometer 10 and supported by the capillary pipe support in the mass spectrometer 10 6.In the mass spectrometer and the sample ions of the air pressure official post between the atmosphere after the ionization gasification form sample ions stream, and be drawn in the mass spectrometer through capillary 2.Angle between the center line of the mass analyzer 4 of the center line of capillary 2 and mass spectrometer 10 is 90 °; The angle of this angle is not limited to 90 °; Can confirm that the angle of this angle all is feasible usually in 80 °～150 ° scopes according to the factors such as electric field strength of mass spectrometric integral structure layout and repulsion electrode 3.Sample ions stream gets in the mass spectrometer through capillary 2, and under the high temperature action of capillary 2, the solvent in the sample ions stream is by further evaporation.The sample ions stream composition that is flown out by capillary 2 comprises ion or ion cluster bunch and unionized successful fluid sample molecule, like impurity particle, solvent particles, solvent molecule group etc., also has the charged droplet of some incomplete big mass-to-charge ratioes of desolvating.
In the utility model first embodiment optimized technical scheme; The atmospheric pressure interface ion source also comprises the ion guides device; This ion guides device is mounted in the ion funnel 50 between mass analyzer 4 and the repulsion electrode 3; This ion funnel 50 comprises the some battery lead plates that are arranged in parallel 51, and the central authorities of every electrode plate 51 have the through hole 511 that supplies sample ions to pass through, and the through hole 511 on some electrode plate 51 diminishes along the heading of sample ions successively; Be provided with insulating trip 52 between adjacent two electrode plate 51, every electrode plate 51 is provided with the electrical connection section 512 that is used to be connected to circuit board.The vacuum degree in ion funnel 50 zones of living in is 60pa～650pa; And near the direct voltage on the battery lead plate 51 of repulsion electrode 3 is 60～100 volts; Near the direct voltage on the battery lead plate 51 of mass analyzer 4 is 25～65 volts, and the direct voltage on some electrode plate 51 successively decreases with the mode of arithmetic progression along the heading of sample ions successively.Be added with alternating voltage on each electrode plate 51, preferably, the phase difference of the alternating voltage between adjacent two electrode plate 51 in some electrode plate 51 is identical, and the alternating voltage phase difference between the two for example whenever adjacent electrode plate is half period.Ion funnel 50 is under above-mentioned vacuum degree, direct voltage, alternating voltage condition, and sample ions can focus on better, thereby each ion primary power is different, deflection angle can be not in full accord even if make, and also can focus on effectively, concentrate.The collision of ion flow and background air can further reduce the temperature of sample ions; Be beneficial to sample ions with the proper speed ion funnel that flies out; Particularly the vacuum degree in ion funnel 50 zones of living in is 110pa～150pa, especially when the 130pa left and right sides, and the direct voltage on some electrode plate 51 with the mode of arithmetic progression when the sample ions heading successively decreases successively; The sample ions ion funnel 50 that can fly out is more swimmingly flown into mass analyzer 4.Direct voltage on certain some electrode plate 51 does not successively decrease with the arithmetic progression mode along the sample ions heading and exceeds, and other the mode of successively decreasing also is feasible; Be not limited to 60～100 volts near the direct voltage on the battery lead plate 51 of repulsion electrode 3, also be not limited to 25～65 volts near the voltage on the battery lead plate 51 of mass analyzer 4.
As shown in Figure 4, sample is a reserpine, and molecular weight is 609; The repulsion electrode is selected plane repulsion electrode 30 for use, and the voltage that puts on the repulsion electrode 30 is 180 volts, and the vacuum degree in ion funnel 50 zones of living in is 130pa; Voltage on first electrode plate 51 (near the battery lead plate of repulsion electrode 3) of sample ions heading is 100 volts; Voltage on second electrode plate 51 is 93 volts, and the voltage on the 3rd electrode plate 51 is 86 volts, and the voltage on the 4th electrode plate 51 is 79 volts; Voltage on the 5th electrode plate 51 is 72 volts; Voltage on the 6th electrode plate 51 is 65 volts, and the voltage on the 7th electrode plate 51 is 58 volts, and the voltage on the 8th electrode plate 51 is 51 volts.Can find out by Fig. 4, pass ion funnel 50 swimmingly, finally fly into mass analyzer from the sample ions that capillary 2 flies out.
As shown in Figure 5, atmospheric pressure interface ion source second embodiment and the first embodiment difference of the utility model only are: the ion guides device is mounted in the utmost point rod-type guiding device 60 between mass analyzer 4 and the repulsion electrode 3.Utmost point rod-type guiding device 60 comprises and being parallel to each other and at the electrode stem 61 of equally distributed four of circumferencial direction, the six roots of sensation or eight or other quantity, and the cross sectional shape of electrode stem 61 can be circular, rectangle or other shapes.Being added with voltage on the every electrode stem 61 and being 100～400 volts, frequency is the radio-frequency current of 600 KHzs～2 megahertzes.The utmost point rod-type guiding device of this second embodiment can do up the effect of good cooling, focusing equally to sample ions.
The mass spectrometer 10 of the utility model comprises mass analyzer 4 and atmospheric pressure interface ion source.Atmospheric pressure interface ion source wherein is the atmospheric pressure interface ion source of aforementioned the utility model, repeats no more here.
Though described the utility model with reference to several exemplary embodiments, should be appreciated that used term is explanation and exemplary and nonrestrictive term.Because the utility model practical implementation and do not break away from the spirit or the essence of utility model in a variety of forms; So be to be understood that; The foregoing description is not limited to any aforesaid details; And should in enclose spirit that claim limited and scope, explain widely, therefore fall into whole variations and remodeling in claim or its equivalent scope and all should be the claim of enclosing and contain.
Claims (10)
1. atmospheric pressure interface ion source; Comprise that an end extend in the mass spectrometer, the other end is arranged on the capillary (2) in the atmosphere; In the said mass spectrometer and the sample ions of the air pressure official post between the atmosphere after the ionization gasification form sample ions stream; And be drawn in the said mass spectrometer through said capillary (2); It is characterized in that: said atmospheric pressure interface ion source also comprises repulsion electrode (3); Angle between the center line of the center line of said capillary (2) and mass spectrometric mass analyzer (4) is 80 °～150 °; Said repulsion electrode (3) is installed in the outside of said angle, is added with 110～380 volts direct voltage on the said repulsion electrode (3), and the electric field that this direct voltage produces gets into said mass analyzer (4) after making 180 °-α of the heading change angle through the sample ions that kinetic energy is little in the sample ions stream of said capillary (2).
2. atmospheric pressure interface ion source as claimed in claim 1 is characterized in that: said angle is 90 °.
3. atmospheric pressure interface ion source as claimed in claim 1 is characterized in that: said repulsion electrode (3) is shaped as semi-cylindrical shape, spherical shape, ellipsoid shape, conical surface shape, frustum face shape or flat shape in the face of said angle one side.
4. atmospheric pressure interface ion source as claimed in claim 1 is characterized in that: have hole or slit on the said repulsion electrode (3), sample ions or the neutral particle big for kinetic energy pass through.
5. like each described atmospheric pressure interface ion source of claim 1-4, it is characterized in that: said atmospheric pressure interface ion source also comprises the ion guides device that is installed between said repulsion electrode (3) and the said mass analyzer (4).
6. atmospheric pressure interface ion source as claimed in claim 5; It is characterized in that: said ion guides device is a utmost point rod-type guiding device (60); Comprise being parallel to each other and that being added with voltage on the every electrode stem (61) and being 100～400 volts, frequency is the radio-frequency current of 600 KHzs～2 megahertzes at equally distributed four of circumferencial direction, the six roots of sensation or eight electrode stems (61).
7. atmospheric pressure interface ion source as claimed in claim 5; It is characterized in that: said ion guides device is ion funnel (50); The battery lead plate (51) that this ion funnel (50) comprises some mutually insulateds and is arranged in parallel; The central authorities of every said battery lead plate (51) have the through hole (511) that supplies said sample ions to pass through, and the through hole (511) on some electrode plate (51) diminishes along the heading of sample ions successively; The vacuum degree in said ion funnel (50) zone of living in is 65pa～650pa; Be added with 60～100 volts direct voltage on the battery lead plate (51) near said repulsion electrode (3); Be added with 25～65 volts direct voltage on the battery lead plate (51) near said mass analyzer (4); Voltage on some electrode plate (51) successively decreases along the heading of sample ions successively; Be added with alternating voltage on the said battery lead plate of each piece (51), and the phase difference of the alternating voltage between the adjacent two said battery lead plates (51) in said some electrode plate (51) is identical.
8. atmospheric pressure interface ion source as claimed in claim 7 is characterized in that: the vacuum degree in said ion funnel (50) zone of living in is 110pa～150pa.
9. atmospheric pressure interface ion source as claimed in claim 7 is characterized in that: the direct voltage on said some electrode plate (51) successively decreases with the mode of arithmetic progression along the heading of sample ions successively.
10. a mass spectrometer comprises mass analyzer (4) and atmospheric pressure interface ion source, it is characterized in that: each described atmospheric pressure interface ion source that said atmospheric pressure interface ion source is claim 1-9.
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| CN201120274625.9U CN202178233U (en) | 2011-07-29 | 2011-07-29 | Atmospheric pressure interface ion source and mass spectrometer |
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| CN201120274625.9U CN202178233U (en) | 2011-07-29 | 2011-07-29 | Atmospheric pressure interface ion source and mass spectrometer |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102903595A (en) * | 2011-07-29 | 2013-01-30 | 北京普析通用仪器有限责任公司 | Atmosphere interface ion source and mass spectrometer |
| WO2013016856A1 (en) * | 2011-07-29 | 2013-02-07 | 北京普析通用仪器有限责任公司 | Ion source and mass spectrometer with interface to atmospheric pressure |
| CN108648982A (en) * | 2018-04-28 | 2018-10-12 | 西北核技术研究所 | A kind of ion transmission method and time-of-flight mass spectrometer based on lock-out pulse |
| WO2022088373A1 (en) * | 2020-11-02 | 2022-05-05 | 昆山禾信质谱技术有限公司 | Ion valve device, mass spectrometer, and mass spectrometer dynamic range adjustment method |
-
2011
- 2011-07-29 CN CN201120274625.9U patent/CN202178233U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102903595A (en) * | 2011-07-29 | 2013-01-30 | 北京普析通用仪器有限责任公司 | Atmosphere interface ion source and mass spectrometer |
| WO2013016856A1 (en) * | 2011-07-29 | 2013-02-07 | 北京普析通用仪器有限责任公司 | Ion source and mass spectrometer with interface to atmospheric pressure |
| CN102903595B (en) * | 2011-07-29 | 2015-01-07 | 北京普析通用仪器有限责任公司 | Atmosphere interface ion source and mass spectrometer |
| CN108648982A (en) * | 2018-04-28 | 2018-10-12 | 西北核技术研究所 | A kind of ion transmission method and time-of-flight mass spectrometer based on lock-out pulse |
| WO2022088373A1 (en) * | 2020-11-02 | 2022-05-05 | 昆山禾信质谱技术有限公司 | Ion valve device, mass spectrometer, and mass spectrometer dynamic range adjustment method |
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| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120328 Termination date: 20150729 |
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| EXPY | Termination of patent right or utility model |