CN105185688A - Mass spectrograph for automatically regulating air pressure inside ion trap and operation method of mass spectrograph - Google Patents
Mass spectrograph for automatically regulating air pressure inside ion trap and operation method of mass spectrograph Download PDFInfo
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Abstract
The invention discloses a mass spectrograph for automatically regulating the air pressure inside an ion trap. The mass spectrograph comprises an ion trap, a detector used for detecting ion separation inside the ion trap, a buffer gas flow controller, a vacuum gauge inside the ion trap, and an operation function module used for automatically adjusting the vacuum degree inside the ion trap. The buffer gas flow controller is connected with the rear end of the ion trap by a gas conduit. The vacuum gauge inside the ion trap is connected with the front end of the ion trap by a gas conduit. The operation function module is respectively in communication connection with the vacuum gauge inside the ion trap and the buffer gas flow controller. During the ion implantation and storage stage, the buffer gas flow is increased to realize the high pressure inside the ion trap, so that the kinetic energy of implanted ions is effectively reduced. After that, the buffer gas flow is orderly lowered to realize the low pressure inside the ion trap. In this way, during the ion separation and detection stage, the pressure inside the ion trap is ensured to be low, so that the optimal detection environment is realized. The mass spectrograph is better in ion storage efficiency and better in analysis performance.
Description
Technical field
The present invention relates to ion trap mass spectrometry apparatus system, relate to the mass spectrometric apparatus system automatically regulating ion trap internal gas pressure especially.
Background technology
In the prior art, mass spectrometric analysis method is that material particle (atom, molecule) is ionized into ion, and by the electric field of suitable stable or change or magnetic field by they spatially position, time sequencing etc. realize karyoplasmic ratio and be separated, and detect its intensity to make the analytical method of qualitative and quantitative analysis.Due to the direct measurement of species particle of mass spectrometric analysis method, and mass spectrometric analysis method has the characteristic of highly sensitive, high-resolution, high flux and high applicability, makes mass spectrometer and analytical technique of mass spectrum very important in modern science and technology.Along with the development of the subjects such as life science, environmental science, medical science, and food security, national security, International Terrorism needs, mass spectrometricly become one of the fastest analytical instrument of demand growth rate, especially the appearance of Chromatography/Mass Spectrometry multiple techniques and pertinent instruments, because of its high separation function to complicated substrate and the high sensitivity of detection, gain great popularity in above-mentioned each field especially, even indispensable.
Mass analyzer is, in mass spectrometer, ion is isolated the parts that can detect according to karyoplasmic ratio, ion trap is important a kind of mass analyzer, its principle is by after many ion storage are in trap, be separated detection again, the mass analyzer of ion trap is not comprised relative to other, the mass analyzer comprising ion trap can ion storage, therefore can be MSn operation (mass spectrum operation) in the mass analyzer comprising ion trap.
The structure of ion trap has multiple, traditional 3D ion trap, the linear ion trap of company of the U.S., and the rectilinear ion trap of U.S. doctor invention, wherein can to overcome traditional 3D ion trap storage of ions few for rectilinear ion trap, and linear ion trap is difficult to the problems such as processing.
The operating mode of ion trap divides two stages: ion implantation memory phase, ion isolation detection-phase.
At ion implantation memory phase, in ion trap, be usually filled with cushion gas (often high-purity He gas), allow cushion gas and the ion entered in trap carry out colliding thus to reduce the initial kinetic energy of ion, reduce the probability escaped from after ion enters ion trap.When cushion gas is few, the probability that ion and cushion gas collide is just few, is not enough to the kinetic energy reducing ion, therefore needs relatively many cushion gases.
At ion isolation detection-phase, require that buffering tolerance is few, avoid too much cushion gas impact force to affect the control of radio frequency electrical field force to ion and mass resolution is deteriorated, the signal to noise ratio that detector works at low pressure simultaneously can be better.
These two different stages, cushion gas is had to the requirement of complete contradiction.Therefore, often adopt the strategy of compromise, be namely filled with the cushion gas of compromise flow, take into account ion implantation and ion detection, but, no matter ion implantation or the equal difficulty of ion detection reach best performance.
Patent No. US8198580B2, devise the ion trap of two series connection, realize high-low pressure, (cushion large-minded at hyperbar, air pressure is high) realize ion implantation in ion trap and store, in low pressure (buffering tolerance is few, and air pressure is low) ion trap, realize ion isolation detect, obtain higher detection perform (high sensitivity and high-resolution).
But, this pair of pressure dual ion trap mass spectrometer system, need 2 cover ion traps and 2 cover rf power system, ion enters low-voltage ion trap from hyperbar ion trap after " cooling " (kinetic energy minimizing), have certain loss, and Control timing sequence is responsible for, the overall difficulty realized is excessive, high cost.And once high-low pressure ion trap interface is fixed, in two pressure trap, vacuum gradient relation is fixed, be difficult to adjust flexibly according to being made by measured ion.These problems hinder ideal and the realization of the ion trap mass spectrometry device of low cost.
Therefore, the mass spectrometric apparatus of ion trap internal gas pressure can be so automatically regulated may to be a kind of comparatively ideal solution.But, realize automatically regulating the mass spectrometric apparatus of ion trap internal gas pressure to there is the technical barrier of three aspects:
One, in ion trap, vacuum degree is not easy direct measurement, indirectly estimates vacuum degree in ion trap (ion trap internal gas pressure than in cavity slightly high) often by the vacuum degree measured in vacuum cavity.
Two, in ion trap, input buffer gas, form vacuum gradient religion easily, but the vacuum gradient that formation is specified then not easily.Ion trap has 1 air inlet, 4 gas delivery outlets, and the geometric parameter in hole and locus can have a strong impact on the formation of vacuum degree in ion trap.
Three, in the short period of time (in the scan period), at ion implantation demands hyperbar, require low gas at ion isolation detection-phase, and require that stable gas pressure is very difficult, otherwise the reappearance of impact analysis.
Summary of the invention
For above-mentioned shortcoming and defect of the prior art, the object of the present invention is to provide a kind of mass spectrometric apparatus and method of operation thereof of automatic adjustment ion trap internal gas pressure.
For achieving the above object, the present invention proposes a kind of mass spectrometric apparatus of automatic adjustment ion trap internal gas pressure, comprise ion trap, for detecting the detector that in ion trap, ion isolation detects, buffer gas flow amount controller, vacuum measurement meter and the automatic calculation function module regulating vacuum degree in trap in ion trap, described buffer gas flow amount controller is communicated with by gas conduit with ion trap rear end, in described ion trap, vacuum measurement meter is communicated with by gas conduit with ion trap front end, described calculation function module communicates to connect with vacuum measurement meter in ion trap and cushion gas flow controller respectively.
Preferably, described ion trap comprises the two arrays of electrodes be provided at its inner portion, the front end housing being arranged on its two ends, rear end cap and air guide cover plate, and often organize electrode and comprise two electrodes arranged in opposite directions, two arrays of electrodes Rotational Symmetry is arranged, described front end housing center has ion guide hand-hole, circularizes uniform multiple cushion gas leadout hole around ion guide hand-hole, described rear end cap center has ion guide and portals, uniform multiple cushion gas entrance hole is circularized around described ion guide is portalled, described air guide cover plate is annular cover plate, described annular cover plate is arranged on the outside of front end housing and rear end cap, annular chamber is formed between front end housing and close annular cover plate and between rear end cap and close annular cover plate, the ion guide of ion guide hand-hole and rear end cap that the intermediate throughholes of described annular slab is more than or equal to front end housing is portalled, cushion gas leadout hole on described front end housing and the cushion gas entrance hole on rear end cap all with corresponding annular chamber conducting.
Preferably, described air guide cover plate is conductive insulation, and described front end housing and rear end cap are conductive electrode film, and the thickness of described conductive electrode film is 0.8 ~ 1.2mm.
Preferably, the ion guide hand-hole ion guide of easing up on qi of chong channel ascending adversely leadout hole and rear end cap on described front end housing is portalled and the equal one_to_one corresponding of cushion gas entrance hole is arranged, the diameter that described ion guide hand-hole and ion guide are portalled is 1mm, the diameter of cushion gas leadout hole and cushion gas entrance hole is 0.5mm, the distance of center circle that described ion guide hand-hole eases up between qi of chong channel ascending adversely leadout hole is 1.5mm, and ion guide is portalled and distance of center circle between cushion gas entrance hole is 1.5mm.
Preferably, also comprise the vaccum interval that Pyatyi air pressure reduces successively, by through hole conducting between described vaccum interval, in one-level vaccum interval, ion source is set, electro-ionic osmosis pipeline is set in secondary vacuum interval, in three grades of vaccum intervals to Pyatyi vaccum interval, ion guides pipeline is all set, through hole that is interval at secondary vacuum and three grades of vaccum intervals arranges ion extractuin device, described ion source outlet, ion guides pipeline and electro-ionic osmosis line ports are all just to the through hole that vaccum interval at different levels is interconnected, air pressure in described one-level vaccum interval is standard atmospheric pressure, air pressure in secondary vacuum interval is 0.8 ~ 1.2Torr, air pressure in Pyatyi vaccum interval is 1 × 10
-5torr, in secondary vacuum interval, three grades of vaccum intervals, level Four vaccum interval and Pyatyi vaccum intervals, the molecular pump being responsible for vacuumizing all is set, be arranged on ion guides pipeline in final stage vaccum interval just to ion trap, described ion trap is arranged in Pyatyi vaccum interval.
A full scan method of operation for the mass spectrometric apparatus of automatic adjustment ion trap internal gas pressure, in turn includes the following steps:
S1, regulates the calculation function module controls buffer gas flow amount controller of vacuum degree in trap automatically, increases cushion gas flow, realizes ion trap air pressure by 1 × 10
-5torr rises to 5 × 10
-3torr, obtains hyperbar in ion trap, is convenient to the injection of ion;
S2, opens the ion gate of ion trap, injects ion to ion trap;
S3, closes the ion gate of ion trap, carries out shaping in trap, ion and cushion gas collide ion, reduces the initial kinetic energy of ion;
S4, regulates the calculation function module controls buffer gas flow amount controller of vacuum degree in trap automatically, reduces cushion gas flow, realizes ion trap air pressure by 5 × 10
-3torr is reduced to 1 × 10
-5torr, obtains low pressure in ion trap, is convenient to the injection that ion isolation detects, in the process, carries out ion shaping, increases ion trap end caps voltage, cluster ion is extruded to ion trap center;
S5, automatically regulates the calculation function module controls detector of vacuum degree in trap to carry out separation to the ion in ion trap and detects operation, obtain the signal strength signal intensity of different mass-to-charge ratio ion.
Preferably, twice air pressure adjustment required time of step S1 and step S4 is the shortest time when ensureing that target air pressure stability is less than 10%.
A multi-stage ms analysis operation method for the mass spectrometric apparatus of automatic adjustment ion trap internal gas pressure, in turn includes the following steps:
S1, regulates the calculation function module controls buffer gas flow amount controller of vacuum degree in trap automatically, increases cushion gas, realizes ion trap air pressure by 1 × 10
-5torr rise to 5 × 10
-3torr, obtains hyperbar in ion trap, is convenient to the injection of ion;
S2, opens the ion gate of ion trap, injects ion to ion trap;
S3, closes the ion gate of ion trap, carries out shaping in trap, allows ion and cushion gas collide to ion, reduces the initial kinetic energy of ion;
S4, according to the motion frequency F_special of target parent ion in trap, ion trap applies do not have the full range of F_special frequency sinusoidal wave, sine wave freuqency scope is 10KHz ~ 500MHz, retain target parent ion, other ions are portalled by ion guide and evicts ion trap from;
S5, drops to the Q point that target parent ion is suitable, ion trap applies the sine wave of same frequency by a small margin by the radio-frequency voltage RF in ion trap, make target parent ion and cushion gas carry out colliding and cracked;
S6, regulates the calculation function module controls buffer gas flow amount controller of vacuum degree in trap automatically, reduces cushion gas, realizes ion trap air pressure by 5 × 10
-3torr is reduced to stable 1 × 10 fast
-5torr, obtains low pressure in ion trap, is convenient to the injection that ion isolation detects; In the process, carry out ion shaping, increase ion trap end caps voltage, cluster ion is extruded to ion trap center;
S7, automatically regulates the calculation function module controls detector of vacuum degree in trap to carry out separation to the ion in trap and detects operation, obtain the signal strength signal intensity of different mass-to-charge ratio ion.
Preferably, also comprise and collide the cracked further of the cracked arbitrary daughter ion obtained to target parent ion in step S5 and cushion gas, described fragmentation is for repeating step S4 and S5.
Preferably, twice air pressure adjustment required time of step S1 and step S6 is the shortest time when ensureing that target air pressure stability is less than 10%.
Compared with prior art, the embodiment of the present invention at least has the following advantages:
The present invention regulates the mass spectrometric apparatus of ion trap internal gas pressure at ion implantation memory phase automatically, increase cushion gas flow and realize hyperbar in trap, effective kinetic energy reducing injection ion, reduce cushion gas flow afterwards in order and realize low pressure, ensure that having low pressure at ion isolation detection-phase obtains best testing environment.The mass spectrometric apparatus system of automatic adjustment ion trap internal gas pressure has better ion storage efficiency, better analytical performance, this system have realize cost low, control the features such as simple, can as the mass spectrometer system of a extensive use.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention regulates the mass spectrometric apparatus of ion trap internal gas pressure automatically;
Fig. 2 is that the present invention regulates the front end housing of the mass spectrometric apparatus of ion trap internal gas pressure and the structural representation of rear end cap automatically;
Fig. 3 is the structural representation that the present invention regulates the air guide cover plate of the mass spectrometric apparatus of ion trap internal gas pressure automatically;
Fig. 4 is the flow chart that the present invention regulates the full scan method of operation of the mass spectrometric apparatus of ion trap internal gas pressure automatically;
Fig. 5 is the flow chart that the present invention regulates the multi-stage ms analysis operation method of the mass spectrometric apparatus of ion trap internal gas pressure automatically.
Embodiment
Below in conjunction with Fig. 1-Fig. 5 and embodiment, the invention will be further described, and following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
A mass spectrometric apparatus for automatic adjustment ion trap 150 internal gas pressure, comprises the vaccum interval (100 that multistage air pressure reduces successively, 110, 120, 130, 140), described vaccum interval (100, 110, 120, 130, 140) by through hole (111 between, 112, 122, 132) conducting, ion source 101 is set in one-level vaccum interval 100, electro-ionic osmosis pipeline 111 is set in secondary vacuum interval 110, in three grades of vaccum interval 120 to final stage vaccum intervals, ion guides pipeline is all set, arrange ion extractuin device 112 at through hole 112 place of secondary vacuum interval 110 and three grades of vaccum intervals 120, described ion source 101 exports, ion guides pipeline (121, 131, 141) and electro-ionic osmosis pipeline 111 port all just to the through hole (111 that vaccum interval at different levels is interconnected, 112, 122, 132), ion trap 150 and the detector 190 for detecting ion isolation detection in ion trap 150 is also provided with in described final stage vaccum interval, be arranged on ion guides pipeline 141 in final stage vaccum interval just to ion trap 150, also comprise buffer gas flow amount controller 160, vacuum measurement meter 170 and the automatic calculation function module 180 regulating vacuum degree in trap in ion trap 150, described buffer gas flow amount controller 160 is communicated with by gas conduit 161 with ion trap 150 rear end, in described ion trap 150, vacuum measurement meter 170 is communicated with by gas conduit 171 with ion trap 150 front end, and described calculation function module 180 communicates to connect with vacuum measurement meter 170 in ion trap 150 and cushion gas flow controller 160 respectively.
Ion trap 150 comprises the two arrays of electrodes be provided at its inner portion, the front end housing 152 being arranged on its two ends, rear end cap 153 and air guide cover plate (151,154), and often organize electrode and comprise two electrodes arranged in opposite directions, two arrays of electrodes Rotational Symmetry is arranged, described front end housing 152 center has ion guide hand-hole, circularizes uniform multiple cushion gas leadout hole around ion guide hand-hole, described rear end cap 153 center has ion guide and portals, uniform multiple cushion gas entrance hole is circularized around described ion guide is portalled, described air guide cover plate (151, 154) be annular cover plate, described annular cover plate is arranged on the outside of front end housing 152 and rear end cap 153, annular chamber is formed between front end housing 152 and close annular cover plate and between rear end cap 153 and close annular cover plate, the ion guide of ion guide hand-hole and rear end cap 153 that the intermediate throughholes of described annular slab is more than or equal to front end housing 152 is portalled, cushion gas leadout hole on described front end housing 152 and the cushion gas entrance hole on rear end cap 153 all with corresponding annular chamber conducting.The front end housing 152 of ion trap 150, rear end cap 153 realize the constrained electric field in ion trap 150Z direction.In order to ensure the symmetry of ion trap 150 internal electric field.
The air guide cover plate (151,154) of ion trap 150 is conductive insulation, and described front end housing 152 and rear end cap 153 are conductive electrode film, and the thickness of described conductive electrode film is 0.8 ~ 1.2mm.
The multi-stage vacuum interval of essential spectrum device is Pyatyi vaccum interval, and the air pressure in described one-level vaccum interval 100 is standard atmospheric pressure, and the air pressure in secondary vacuum interval 110 is 0.8 ~ 1.2Torr, and the air pressure in Pyatyi vaccum interval 140 is 1 × 10
-5torr, in secondary vacuum interval, 110, three grades of vaccum intervals 120, level Four vaccum interval 130 and Pyatyi vaccum intervals 140 all arrange the molecular pump (119,129,139,149) being responsible for vacuumizing.
Ion guide hand-hole on ion trap 150 front end housing 152 ion guide of easing up on qi of chong channel ascending adversely leadout hole and rear end cap 153 is portalled and the equal one_to_one corresponding of cushion gas entrance hole is arranged, the diameter that described ion guide hand-hole and ion guide are portalled is 1mm, the diameter of cushion gas leadout hole and cushion gas entrance hole is 0.5mm, the distance of center circle that described ion guide hand-hole eases up between qi of chong channel ascending adversely leadout hole is 1.5mm, and ion guide is portalled and distance of center circle between cushion gas entrance hole is 1.5mm.
Before carrying out multi-stage ms analysis operation and full scan operation, first to carry out necessary preparation, the size of through hole (111,112,122,132) between the size of foundation multi-stage vacuum interval (100,110,120,130,140) and vaccum interval, and the actual conditions of the actual pumping speed size of multiple molecular pump (119,129,139,149), adopt closed-loop automatic control technology, by repeatedly testing, obtain 2 bare flow parameter regulating parameter curves: 1, ion trap 150 internal gas pressure is by 1 × 10
-5torr is climbed to 5 × 10
-3the buffer gas flow discharge curve of Torr, 2, ion trap 150 internal gas pressure is by 5 × 10
-3torr rapidly drops to 1 × 10
-5the buffer gas flow discharge curve of Torr, automatically regulates the calculation function module 180 of vacuum degree in trap to adopt closed-loop automatic control to finely tune according to fundamental curve in actual conditions, ensures within the shortest time, obtain stable target air pressure.
A full scan method of operation for the mass spectrometric apparatus of automatic adjustment ion trap 150 internal gas pressure, in turn includes the following steps:
S1, automatically regulates the calculation function module 180 of vacuum degree in trap to control buffer gas flow amount controller 160, increases cushion gas flow, realize ion trap 150 air pressure by 1 × 10
-5torr rises to 5 × 10
-3torr, obtains hyperbar in ion trap 150, is convenient to the injection of ion;
S2, opens the ion gate of ion trap 150, injects ion to ion trap 150;
S3, closes the ion gate of ion trap 150, carries out shaping in trap, ion and cushion gas collide ion, reduces the initial kinetic energy of ion;
S4, automatically regulates the calculation function module 180 of vacuum degree in trap to control buffer gas flow amount controller 160, reduces cushion gas flow, realize ion trap 150 air pressure by 5 × 10
-3torr is reduced to 1 × 10
-5torr, obtains low pressure in ion trap 150, is convenient to the injection that ion isolation detects, in the process, carries out ion shaping, increases ion trap 150 end cap voltage, cluster ion is extruded to ion trap 150 center;
S5, automatically regulates the calculation function module 180 of vacuum degree in trap to control detector and carries out separation detection operation to the ion in ion trap 150, obtain the signal strength signal intensity of different mass-to-charge ratio ion.
In the shortest time that the step S1 of this control method and twice air pressure adjustment required time of step S4 are when ensureing that target air pressure stability is less than 10%.
A multi-stage ms analysis operation method for the mass spectrometric apparatus of automatic adjustment ion trap 150 internal gas pressure, in turn includes the following steps:
S1, automatically regulates the calculation function module 180 of vacuum degree in trap to control buffer gas flow amount controller 160, increases cushion gas, realize ion trap 150 air pressure by 1 × 10
-5torr rise to 5 × 10
-3torr, obtains hyperbar in ion trap 150, is convenient to the injection of ion;
S2, opens the ion gate of ion trap 150, injects ion to ion trap 150;
S3, closes the ion gate of ion trap 150, carries out shaping in trap, allows ion and cushion gas collide to ion, reduces the initial kinetic energy of ion;
S4, according to the motion frequency F_special of target parent ion in trap, ion trap 150 applies do not have the full range of F_special frequency sinusoidal wave, sine wave freuqency scope is 10KHz ~ 500MHz, retain target parent ion, other ions are portalled by ion guide and evicts ion trap 150 from;
S5, drops to the Q point that target parent ion is suitable, ion trap 150 applies the sine wave of same frequency by a small margin by the radio-frequency voltage RF in ion trap 150, make target parent ion and cushion gas carry out colliding and cracked;
S6, automatically regulates the calculation function module 180 of vacuum degree in trap to control buffer gas flow amount controller 160, reduces cushion gas, realize ion trap 150 air pressure by 5 × 10
-3torr is reduced to stable 1 × 10 fast
-5torr, obtains low pressure in ion trap 150, is convenient to the injection that ion isolation detects; In the process, carry out ion shaping, increase ion trap 150 end cap voltage, cluster ion is extruded to ion trap 150 center;
S7, automatically regulates the calculation function module 180 of vacuum degree in trap to control detector and carries out separation detection operation to the ion in trap, obtain the signal strength signal intensity of different mass-to-charge ratio ion.
This control method also comprises collides the cracked further of the cracked arbitrary daughter ion obtained to target parent ion in step S5 and cushion gas, and described fragmentation is for repeating step S4 and S5.
In the shortest time that the step S1 of this control method and twice air pressure adjustment required time of step S6 are when ensureing that target air pressure stability is less than 10%.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claims.
Claims (9)
1. one kind regulates the mass spectrometric apparatus of ion trap internal gas pressure automatically, it is characterized in that, comprise ion trap, for detecting vacuum measurement meter in detector that ion isolation in ion trap detects, buffer gas flow amount controller, ion trap and automatically regulating the calculation function module of vacuum degree in trap, described buffer gas flow amount controller is communicated with by gas conduit with ion trap rear end, in described ion trap, vacuum measurement meter is communicated with by gas conduit with ion trap front end, and described calculation function module communicates to connect with vacuum measurement meter in ion trap and cushion gas flow controller respectively.
2. the mass spectrometric apparatus of automatic adjustment ion trap internal gas pressure according to claim 1, it is characterized in that, described ion trap comprises the two arrays of electrodes be provided at its inner portion, the front end housing being arranged on its two ends, rear end cap and air guide cover plate, often organize electrode and comprise two electrodes arranged in opposite directions, two arrays of electrodes Rotational Symmetry is arranged, described front end housing center has ion guide hand-hole, circularizes uniform multiple cushion gas leadout hole around ion guide hand-hole, described rear end cap center has ion guide and portals, uniform multiple cushion gas entrance hole is circularized around described ion guide is portalled, described air guide cover plate is annular cover plate, described annular cover plate is arranged on the outside of front end housing and rear end cap, annular chamber is formed between front end housing and close annular cover plate and between rear end cap and close annular cover plate, the ion guide of ion guide hand-hole and rear end cap that the intermediate throughholes of described annular slab is more than or equal to front end housing is portalled, cushion gas leadout hole on described front end housing and the cushion gas entrance hole on rear end cap all with corresponding annular chamber conducting.
3. the mass spectrometric apparatus of automatic adjustment ion trap internal gas pressure according to claim 2, it is characterized in that, described air guide cover plate is conductive insulation, and described front end housing and rear end cap are conductive electrode film, and the thickness of described conductive electrode film is 0.8 ~ 1.2mm.
4. the mass spectrometric apparatus of the automatic adjustment ion trap internal gas pressure according to Claims 2 or 3, it is characterized in that, the ion guide hand-hole ion guide of easing up on qi of chong channel ascending adversely leadout hole and rear end cap on described front end housing is portalled and the equal one_to_one corresponding of cushion gas entrance hole is arranged, the diameter that described ion guide hand-hole and ion guide are portalled is 1mm, the diameter of cushion gas leadout hole and cushion gas entrance hole is 0.5mm, the distance of center circle that described ion guide hand-hole eases up between qi of chong channel ascending adversely leadout hole is 1.5mm, and ion guide is portalled and distance of center circle between cushion gas entrance hole is 1.5mm.
5. automatically regulate a full scan method of operation for the mass spectrometric apparatus of ion trap internal gas pressure, it is characterized in that, in turn include the following steps:
S1, regulates the calculation function module controls buffer gas flow amount controller of vacuum degree in trap automatically, increases cushion gas flow, realizes ion trap air pressure by 1 × 10
-5torr rises to 5 × 10
-3torr, obtains hyperbar in ion trap, is convenient to the injection of ion;
S2, opens the ion gate of ion trap, injects ion to ion trap;
S3, closes the ion gate of ion trap, carries out shaping in trap, ion and cushion gas collide ion, reduces the initial kinetic energy of ion;
S4, regulates the calculation function module controls buffer gas flow amount controller of vacuum degree in trap automatically, reduces cushion gas flow, realizes ion trap air pressure by 5 × 10
-3torr is reduced to 1 × 10
-5torr, obtains low pressure in ion trap, is convenient to the injection that ion isolation detects, in the process, carries out ion shaping, increases ion trap end caps voltage, cluster ion is extruded to ion trap center;
S5, automatically regulates the calculation function module controls detector of vacuum degree in trap to carry out separation to the ion in ion trap and detects operation, obtain the signal strength signal intensity of different mass-to-charge ratio ion.
6. the full scan method of operation of the mass spectrometric apparatus of automatic adjustment ion trap internal gas pressure according to claim 5, is characterized in that ground, and twice air pressure adjustment required time of step S1 and step S4 is the short time when ensureing that target air pressure stability is less than 10%.
7. automatically regulate a multi-stage ms analysis operation method for the mass spectrometric apparatus of ion trap internal gas pressure, it is characterized in that, in turn include the following steps:
S1, regulates the calculation function module controls buffer gas flow amount controller of vacuum degree in trap automatically, increases cushion gas, realizes ion trap air pressure by 1 × 10
-5torr rise to 5 × 10
-3torr, obtains hyperbar in ion trap, is convenient to the injection of ion;
S2, opens the ion gate of ion trap, injects ion to ion trap;
S3, closes the ion gate of ion trap, carries out shaping in trap, allows ion and cushion gas collide to ion, reduces the initial kinetic energy of ion;
S4, according to the motion frequency F_special of target parent ion in trap, ion trap applies do not have the full range of F_special frequency sinusoidal wave, sine wave freuqency scope is 10KHz ~ 500MHz, retain target parent ion, other ions are portalled by ion guide and evicts ion trap from;
S5, drops to the Q point that target parent ion is suitable, ion trap applies the sine wave of same frequency by a small margin by the radio-frequency voltage RF in ion trap, make target parent ion and cushion gas carry out colliding and cracked;
S6, regulates the calculation function module controls buffer gas flow amount controller of vacuum degree in trap automatically, reduces cushion gas, realizes ion trap air pressure by 5 × 10
-3torr is reduced to stable 1 × 10 fast
-5torr, obtains low pressure in ion trap, is convenient to the injection that ion isolation detects; In the process, carry out ion shaping, increase ion trap end caps voltage, cluster ion is extruded to ion trap center;
S7, automatically regulates the calculation function module controls detector of vacuum degree in trap to carry out separation to the ion in trap and detects operation, obtain the signal strength signal intensity of different mass-to-charge ratio ion.
8. the multi-stage ms analysis operation method of the mass spectrometric apparatus of automatic adjustment ion trap internal gas pressure according to claim 7, it is characterized in that, also comprise and collide the cracked further of the cracked arbitrary daughter ion obtained to target parent ion in step S5 and cushion gas, described fragmentation is for repeating step S4 and S5.
9. the multi-stage ms analysis operation method of the mass spectrometric apparatus of automatic adjustment ion trap internal gas pressure according to claim 7, it is characterized in that, twice air pressure adjustment required time of step S1 and step S6 is the shortest time when ensureing that target air pressure stability is less than 10%.
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| CN106356275A (en) * | 2016-08-08 | 2017-01-25 | 复旦大学 | Uniform air supply device for overlaying ring ionic mobility drift tube |
| CN107799384A (en) * | 2017-10-09 | 2018-03-13 | 清华大学 | Mass spectrograph |
| CN110277301A (en) * | 2019-06-28 | 2019-09-24 | 清华大学深圳研究生院 | A kind of air pressure inside ion trap unevenly distributed and its working method |
| CN111899909A (en) * | 2020-08-10 | 2020-11-06 | 中国科学技术大学 | Device for cooling and trapping ions |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105390364A (en) * | 2015-12-28 | 2016-03-09 | 中国计量科学研究院 | Mass spectrum apparatus capable of detecting neutral molecule products and ion products, and operating method thereof |
| CN105551928A (en) * | 2015-12-28 | 2016-05-04 | 中国计量科学研究院 | Efficient simple molecules/ions reaction mass spectrometry apparatus and operation method therefor |
| CN106356275A (en) * | 2016-08-08 | 2017-01-25 | 复旦大学 | Uniform air supply device for overlaying ring ionic mobility drift tube |
| CN107799384A (en) * | 2017-10-09 | 2018-03-13 | 清华大学 | Mass spectrograph |
| CN110277301A (en) * | 2019-06-28 | 2019-09-24 | 清华大学深圳研究生院 | A kind of air pressure inside ion trap unevenly distributed and its working method |
| CN111899909A (en) * | 2020-08-10 | 2020-11-06 | 中国科学技术大学 | Device for cooling and trapping ions |
| CN111899909B (en) * | 2020-08-10 | 2023-03-24 | 中国科学技术大学 | Device for cooling and trapping ions |
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