CN103903955B - Ion enrichment and lead-in device and method for atmospheric ion source time-of-flight mass spectrometer - Google Patents
Ion enrichment and lead-in device and method for atmospheric ion source time-of-flight mass spectrometer Download PDFInfo
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Abstract
The invention relates to an ion enrichment and lead-in device for an atmospheric ion source time-of-flight mass spectrometer. The ion enrichment and lead-in device comprises an enrichment device and a repelling device, wherein ions sequentially pass through the enrichment device and the repelling device. The enrichment device comprises a closed cavity, wherein a radio-frequency four-level rod, the two ends of the radio-frequency four-level rod are provided with a first electrode with an ion inlet and a second electrode with an ion outlet, the first electrode is connected with a direct current power supply, and the second electrode is connected with a high voltage pulse power supply. The invention further relates to an ion enrichment and lead-in method. A high voltage pulse power supply is led in the second electrode, release of ions is controlled through high level and low level switching of the high voltage pulse power supply, and therefore enrichment of ions is achieved, the enrichment time and the lead-out time of ions are regulated by adjusting the pulse width, the quality detection range of an instrument is widened, and the more the enriched ions are, the higher the sensitivity of the instrument is. The device and the method can be applied to ion enrichment and lead-in of the atmospheric ion source time-of-flight mass spectrometer.
Description
Technical field
The present invention relates to time of-flight mass spectrometer, more particularly to a kind of atmospheric pressure ionizationion time of-flight mass spectrometer from
Son enrichment introducing device and method.
Background technology
The ion transmission of atmospheric pressure ionizationion time of-flight mass spectrometer and introducing system are usually used quadrupole rod and multigroup quiet
Electric lens, refer to Fig. 1.Ion can enter molecular ion reactor 1(mir first), enter radio frequency quadrupole after preliminary focusing
Bar 2(rfq), after cooling down with background air molecular collision, ion kinetic energy is close to heat energy value, the acceleration of ions after then cooling down
Enter DC static quadrupole rod 3(dcq) and one-dimensional simple lens 4.Ion beam is modulated into flat by dcq3 and one-dimensional simple lens 4 system
Shape, effectively reduces ion energy dispersion, and can control the incident direction of ion beam, makes up ion to a certain extent and adjusts
Rigging error between transmission range processed and analyzer.This conventional ion transmission is with the system of introducing through development for many years, skill
Art is day by day ripe, and application is also more and more extensive.
Conventional atmospheric pressure ionizationion time of-flight mass spectrometer generally adopts continuous input mode, and that is, sample is successive
Be input to instrument, and adopt the TOF of pulse repulsion mode operationally can lose part ion, because
It is that ion is pushed into analyzer when repulsion pulse is high level, when repulsion pulse is low level, ion can pass through repulsion area,
Until next repulsion high level arrives.Add that conventional ion transmission and introducing system only play the effect of transmission ion again,
Ion can not be enriched with, instrument will seem insufficient sensitivity so when sample concentration is too low.
Content of the invention
In order to overcome above-mentioned technical problem, it is an object of the invention to provide one kind can be enriched with object ion, raising flies
The ion enrichment introducing device of atmospheric pressure ionizationion time of-flight mass spectrometer of row time mass spectrum instrument sensitivity and resolution and side
Method.
The technical solution adopted in the present invention is:
A kind of ion enrichment introducing device of atmospheric pressure ionizationion time of-flight mass spectrometer, the richness passing sequentially through including ion
Acquisition means and repulsion device, described enriching apparatus include closed cavity, are provided with radio frequency level Four bar in described closed cavity, described penetrate
The two ends of frequency level Four bar are the first electrode being provided with ion entrance and the second electrode being provided with ion outlet, in described first electrode
It is connected to DC source, described second electrode is connected to high-voltage pulse power source.
As the improvement further of technique scheme, described radio frequency level Four bar includes four round bars being parallel to each other, phase
It is provided with square bar, described square bar has angle relative to the axial direction of round bar, and described each square bar is connected to DC source between adjacent round bar.
As the improvement further of technique scheme, between described enriching apparatus and repulsion device, it is sequentially provided with electrostatic four
Pole bar and one-dimensional simple lens.
A kind of ion enrichment introducing method of atmospheric pressure ionizationion time of-flight mass spectrometer, applies unidirectional current in first electrode
Source, applies high-voltage pulse power source on the second electrode, makes to be formed direction transformation and electric field side between first electrode and second electrode
To cycle adjustable electric field, ion-beam cleaning is enriched in radiofrequency quadrupole by the cooling focusing principle by radiofrequency quadrupole simultaneously
In, enrichment time and the extraction time of ion is adjusted by the pulsewidth adjusting second electrode.
As the improvement further of technique scheme, after ion enters enriching apparatus, poly- in the presence of radio-frequency voltage
, near radio frequency level Four bar axis, when the current potential of second electrode is high level, ion is in the presence of reversed electric field power for Jiao
It is blocked in enriching apparatus end, the time that ion is enriched with enriching apparatus end is second electrode high level time, when the second electricity
When the current potential of pole is low level, the ion of enrichment enters repulsion device after being released.
As the improvement further of technique scheme, pulse signal is applied to the repeller plate of repulsion device, by adjustment
This pulse signal, with respect to the delay time of second electrode high-voltage pulse power source pulse signal, to select different object ions to enter
Enter TOF.
The invention has the beneficial effects as follows: the present invention passes through to introduce high-voltage pulse power source in second electrode, by high-voltage pulse
The release of the switching control ion of the high and low level of power supply, thus realizing the enrichment of ion, adjusts ion by the adjustment of pulsewidth
Enrichment time and the time of extraction, improve the detection mass range of instrument, and ion enrichment is more, the sensitivity of instrument is higher.
Brief description
The present invention is further described with embodiment below in conjunction with the accompanying drawings.
Fig. 1 is the schematic diagram of atmospheric pressure ionizationion time of-flight mass spectrometer in conventional art；
Fig. 2 is radio frequency level Four bar schematic diagram of the present invention；
Fig. 3 is that radio frequency level Four bar of the present invention powers up schematic diagram；
Fig. 4 is that first electrode of the present invention powers up schematic diagram with second electrode；
Fig. 5 is the time diagram of the present invention.
Specific embodiment
The present embodiment is the transformation based on conventional art, as shown in figure 1, include ion sequentially pass through ion reactor 1,
Radiofrequency quadrupole 2, DC static quadrupole rod 3, one-dimensional simple lens 4 and repulsion area.DC static quadrupole rod 3 and one-dimensional simple lens 4
Ion beam is modulated into flat pattern, effectively reduces ion energy dispersion.
As shown in Figures 2 and 3, radiofrequency quadrupole 2 is made up of four round bars 21 and four square bars 22, four round bars 21 and four
Root square bar 22 is fixed in three fixing round seats, and radiofrequency quadrupole 2 is integrally placed in the long cylinder of a cylindrical metal material,
Both sides are first electrode 5 and second electrode 6 respectively, are consequently formed a closed chamber, the intracavity air pressure of this closed chamber is in 10e- 3Torr about.The center of wherein first electrode 5 is provided with ion inlet orifice, and the center of second electrode 6 is provided with ion and goes out
Mouthful.Four axially in parallel and relative round bars 21 of round bar 21 are interconnected by wire, by applying radio-frequency voltage, ion is cold
But it is strapped within the chamber.The equal relative axis of four square bars 22 form an angle, then when DC voltage is applied on square bar 22, by
Different in distance between tie rods, different voltage influences will be produced on axis, such that it is able to form axial accelerating field.Four round bars
21st, four square bars 22, first electrode 5, second electrode 6 and cylinder mutual insulating, by the insulation peek pad of high pressure resistant high temperature
It is connected.
In order to obtain the effect of enrichment, as shown in figure 4, first electrode 5 is connected to fixing DC source 7, second electrode 6 connects
There is high-voltage pulse power source 8, this high-voltage pulse power source 8 forms the direct current applying on first via high-voltage pulse signal, and first electrode 5
Electric amplitude is higher than the low level of the high-voltage pulse applying in second electrode 6.First via high-voltage pulse signal frequency range be 1hz ~
20khz, pulsewidth is 50ns ~ 100us, and rising edge of a pulse is less than 100ns, and amplitude adjustable extent is 0 ~ 200v.
The repulsion area of the present embodiment is by the repeller plate 9 of ToF analyses instrument and the negative pulse electrode relative with repeller plate 9
10 composition, wherein repeller plate 9 is connected to the second road high-voltage pulse signal, its frequency range be 1hz ~ 20khz, pulsewidth be 1us ~
100us, rising edge of a pulse is less than 100ns, and amplitude adjustable extent is 0 ~ 1000v, and negative pulse electrode 10 is connected to the 3rd road high pressure
Pulse signal, anti-phase with the second road pulse signal.
The ion enrichment introducing method of the atmospheric pressure ionizationion time of-flight mass spectrometer of the present embodiment, method is as follows:
(1) apply radio-frequency voltage on the round bar 21 of radiofrequency quadrupole 2, adjacent round bar 21 applies amplitude identical, square
To contrary voltage, relative round bar 21 applies all the same voltage of amplitude phase.
(2) identical DC voltage is applied on four square bars 22.
(3) apply DC source 7 in first electrode 5, second electrode 6 applies first via high-voltage pulse signal, this
Sample first electrode 5 and second electrode 6 are just being axially formed electric field.
(4) ion enters closed chamber from first electrode 5, and is collided with the gas molecule in closed chamber, collision
Ion kinetic energy afterwards is less than 1ev, and all focuses near axis.When the pulse voltage in second electrode 6 is high level, the
Reversely, ion is collected at the exit of second electrode 6 to the electric field of one electrode 5 and second electrode 6 formation, in radiofrequency signal and side
Motion is shaken in second electrode 6 exit in the presence of bar electric field.When the pulse voltage in second electrode 6 is low level, rich
The ion beam of collection flies out from second electrode 6 outlet in the presence of electric field force, enters DC static quadrupole rod 3 and one-dimensional simple lens
In 4, then ion beam enters repulsion area, now applies the second road and the 3rd road high-voltage pulse signal, ion beam in repulsion area
Time-of flight analyzer is fully entered in the presence of pulse.
To sum up, the principle of the present embodiment is: by applying fixing DC source in first electrode 5, applies in second electrode 6
Add high pressure the pulse power, makes to form the electric field of a direction transformation between first electrode 5 and second electrode 6, and the direction of an electric field cycle
Adjustable, ion-beam cleaning is enriched in radiofrequency quadrupole 2 the cooling focusing principle by radiofrequency quadrupole 2 simultaneously, by adjusting
The pulsewidth of second electrode 6 can adjust enrichment time and the extraction time of ion.Calculate ion through DC static quadrupole rod 3
With the time of one-dimensional simple lens 4, this time be the second road pulse signal relative to first via pulse signal delay time.Time delay
After end, the second road high-voltage pulse signal being added on repeller plate 9 enters high level, and now ion beam is all arrived by repulsion and flies
In time analyser (TA).
As shown in figure 5, t1 is the cycle of first via high-voltage pulse signal, t2 is the pulsewidth of first via high-voltage pulse signal,
T3 is the delay time that the second road pulse signal is relative to first via pulse signal, and t4 is the second road pulse signal and the 3rd tunnel pulse
The pulsewidth of signal.
Through the modulation of DC static quadrupole rod and one-dimensional simple lens 4, the ion of enrichment according to mass number from small to large according to
Secondary entrance repulsion area, by adjusting the size of t3, can select different object ions to enter Time-of flight analyzer.Time delay t3
After end, the second road high-voltage pulse signal being applied on repeller plate 9 enters high level, is applied to the on negative pulse electrode 10
Three road pulse signals enter negative high level, and such ion is in the presence of the electric field that repeller plate 9 is formed with negative pulse electrode 10
Enter Time-of flight analyzer.
Further, by adjusting the size of t2, the enrichment time of ion can be adjusted, be less than the cycle in pulsewidth t2 in theory
On the premise of t1, t2 is bigger, ion enrichment more, the sensitivity of instrument will be better.
Further, t4 is controlled to change repulsion pulsewidth, i.e. the utilization rate to improve ion for the application time of control repulsion pulse,
Generally, in the range from 50us ~ 1ms.
The above is the preferred embodiment of the present invention, and it does not constitute limiting the scope of the invention.
Claims (4)
1. a kind of ion enrichment introducing device of atmospheric pressure ionizationion time of-flight mass spectrometer it is characterised in that: include ion according to
The secondary enriching apparatus passing through and repulsion device, described enriching apparatus include closed cavity, are provided with radio frequency four in described closed cavity
Level bar, the two ends of described radio frequency level Four bar are the first electrode being provided with ion entrance and the second electrode being provided with ion outlet, institute
State and be connected to DC source in first electrode, described second electrode is connected to high-voltage pulse power source, apply unidirectional current in first electrode
Source, applies high-voltage pulse power source on the second electrode, makes to be formed direction transformation and electric field side between first electrode and second electrode
To cycle adjustable electric field, ion-beam cleaning is enriched in radiofrequency quadrupole by the cooling focusing principle by radiofrequency quadrupole simultaneously
In, adjust enrichment time and the extraction time of ion by the pulsewidth adjusting second electrode, described radiofrequency quadrupole is integrally put
Put in the long cylinder of a cylindrical metal material, described radio frequency level Four bar includes four round bars being parallel to each other, adjacent circle
It is provided with square bar between bar, described square bar has angle relative to the axial direction of round bar, and described each square bar is connected to DC source, four circles
Bar, four square bars, first electrode, second electrode and long cylinder mutual insulating, and connected and long cylinder by the peek pad that insulate
Fixing.
2. the ion enrichment introducing device of atmospheric pressure ionizationion time of-flight mass spectrometer according to claim 1, its feature
It is: between described enriching apparatus and repulsion device, be sequentially provided with DC static quadrupole rod and one-dimensional simple lens.
3. the ion enrichment introducing device of atmospheric pressure ionizationion time of-flight mass spectrometer according to claim 1, its feature
It is: after ion enters enriching apparatus, focus in the presence of radio-frequency voltage near radio frequency level Four bar axis, when the second electricity
When the current potential of pole is high level, ion is blocked in enriching apparatus end in the presence of reversed electric field power, and ion is in enriching apparatus
The time of end enrichment is second electrode high level time, and when the current potential of second electrode is low level, the ion of enrichment is released
Repulsion device is entered after putting.
4. the ion enrichment introducing device of atmospheric pressure ionizationion time of-flight mass spectrometer according to claim 3, its feature
It is: pulse signal is applied to the repeller plate of repulsion device, by adjusting this pulse signal with respect to second electrode high-voltage pulse
The delay time of power pulse signal, to select different object ions to enter TOF.
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| CN201410108444.7A CN103903955B (en) | 2014-03-21 | 2014-03-21 | Ion enrichment and lead-in device and method for atmospheric ion source time-of-flight mass spectrometer |
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| CN106711009A (en) * | 2017-02-23 | 2017-05-24 | 昆山禾信质谱技术有限公司 | High-ion extraction efficiency ion trap flight time mass spectrometer and implementation method thereof |
| 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 |
| CN114334600A (en) * | 2021-12-25 | 2022-04-12 | 广州禾信仪器股份有限公司 | Mass spectrometer, ion source and ion transmission structure thereof |
| CN115172136B (en) * | 2022-07-12 | 2024-05-14 | 广东省麦思科学仪器创新研究院 | Method for adjusting initial state of ion group |
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Address after: 510530, A3 building, No. 11, Kaiyuan Avenue, Guangzhou Development Zone, Guangdong third, China Co-patentee after: Kunshan Hexin Zhipu Technology Co.,Ltd. Patentee after: Guangzhou Hexin Instruments Co., Ltd. Address before: 510530, A3 building, No. 11, Kaiyuan Avenue, Guangzhou Development Zone, Guangdong third, China Co-patentee before: Kunshan Hexin Zhipu Technology Co.,Ltd. Patentee before: Guangzhou Hexin Analytical Instrument Co., Ltd. |
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