CN104576290B - A kind of ion enrichment method of pulse-pressure - Google Patents
A kind of ion enrichment method of pulse-pressure Download PDFInfo
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- CN104576290B CN104576290B CN201410784348.4A CN201410784348A CN104576290B CN 104576290 B CN104576290 B CN 104576290B CN 201410784348 A CN201410784348 A CN 201410784348A CN 104576290 B CN104576290 B CN 104576290B
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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
- H01J49/34—Dynamic spectrometers
- H01J49/40—Time-of-flight spectrometers
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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
- H01J49/06—Electron- or ion-optical arrangements
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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
Abstract
The invention discloses a kind of ion enrichment method of pulse-pressure.Using ion enrichment segregation apparatuss, the method using applying pulse voltage on pulsed electrode, when making low level, ion is enriched with ionized region;During high level, the ion of enrichment moves downward in the presence of electric field, through ion transmission range and repulsion area, eventually arrives at mass analyzer.By controlling the time delay of the pulse voltage on ionized region and repulsion electrode, improve the efficiency that ion enters mass analyzer.The present invention effectively raises the ion utilization ratio using the vertical flight time mass spectrum accelerating, and improves the detection sensitivity of flight time mass spectrum.
Description
Technical field
The present invention relates to analytical technique of mass spectrum field, the ion enrichment method of specifically a kind of pulse-pressure.The method is led to
Spend the time delay controlling the pulse voltage on ionized region and repulsion electrode, to improve using the vertical flight time mass spectrum accelerating
Ion utilization ratio and detection sensitivity.
Background technology
1886, E.Goldstein observed positive charged particles in low pressure discharge experiment, and subsequent W.Wein finds positive electricity
Lotus particle beam deflects in magnetic field, and these observed results provide preparation for mass spectrographic birth.First mass spectrum in the world
Instrument is in 1912 by English physicist Joseph John Thomson (Nobel Prize in physics winner, Britain's sword in 1906
Bridge college professor) succeed in developing;To the twenties in 20th century, mass spectrum is increasingly becoming a kind of analysis means, is adopted by chemist;1948
Year, Cameron and Eggers was made for First time of-flight mass spectrometer, and this kind of mass spectrometer not only obtains on instrument design
Progress, widely available application, especially played an important role in terms of the combination with capillary gas chromatography simultaneously.1955
Year Wiley and Mclanren propose double fields and accelerate Focusing Theories, and accelerate focusing to make orthoscopic flight time matter by double fields
The resolution of spectrum has exceeded 100, and gives corresponding theoretical derivation.Vertical ion is introduced and reflection by Chen in 1999 etc.
Formula flight time mass spectrum combines and obtains the mass spectrum that resolution reaches 10000, and tool length is 1.3m.Traditional flight time
Mass spectrum is to be completed by Pulsed Sampling, does not enter into mass spectrographic ion and accounts for greatly.
Vertical boost-phase time mass spectrum drastically increases the resolution of instrument, but vertical boost-phase time is mass spectrographic
Ion utilization ratio is not high, and generally only 5% about, have impact on the detection sensitivity of instrument.Only sub-fraction ion warp
To in mass analyzer, most of ion does not enter into mass analyzer for extra pulse voltage repulsion.
In order to improve mass spectrographic ion utilization ratio of vertical boost-phase time and detection sensitivity, the present invention is in pulse electricity
It is applied with pulse voltage on extremely.When pulsed electrode applies low voltage pulse, the ion that ionized region produces vibrates in ionized region
And be enriched with;When pulsed electrode applies high voltage pulse, in the presence of electric field, the ion of enrichment moves downward, and finally enters
Enter mass analyzer.The applying of pulse voltage improves the utilization ratio of ion.
Content of the invention:
It is an object of the invention to provide a kind of ion enrichment method of pulse-pressure.
The technical scheme that the present invention solves above-mentioned technical problem is as follows:
1. a kind of ion enrichment device of pulse-pressure is by ionized region, ion transmission range, repulsion area and mass analyzer four
Individual region composition.
1) structure of each part of ion enrichment device:
1.1), in described ionized region, it is sequentially provided with light source incidence hole, pulsed electrode, focusing electrode and hole electricity from top to bottom
Pole;Described light source incidence hole is located at directly over ionized region pulsed electrode on wall or side wall;Described pulsed electrode is by circular hole gold
Belong to piece to constitute, centre bore is gradually increased from top to bottom, its function is to produce pulse voltage;Described focusing electrode, by justifying
Ring metal electrode is constituted, and its function is the ion focusing producing ionized region;Described pore electrode, is column or the mesa-shaped of hollow
Cylinder electrode, centre bore is gradually increased from top to bottom, its function be will focus on after ion shaping formed ion stream so as to
Enter ion transmission range.In pulsed electrode (1) upper applying pulse voltage, during low-voltage, ion is in pulsed electrode (1) and pore electrode
(3) the region enrichment between.
It is provided with capillary tube around ionized region, sample gas enters into ionized region by capillary tube;The capillary tube using
For surface through silanization treatment vitreous silica capillary tube, 50 μm of internal diameter, length 50cm.
1.2) it is provided with transmission electrode group in described ion transmission range, it is to be made up of one group of 2~10 electrode slice with holes,
It is spaced with insulating trip between electrode slice, for the transmission of ion stream.
1.3) described repulsion area, is inside provided with repulsion electrode and extraction electrode, and top is provided with slit.Described slit is a rectangle
Hole, for the shaping of ion stream.Described repulsion electrode, is a metal plate electrode, and its function is to produce repulsion voltage.Described
Extraction electrode, be perforated metal electrode, the extraction for repulsion area ion stream so as to enter mass analyzer.
1.4) described mass analyzer is that a kind of ion by different mass-to-charge ratioes carries out detached device.
2) spatial relation of each part of ion enrichment device:
Described pulsed electrode, focusing electrode, pore electrode, transmission electrode group and slit are in and are coaxially disposed.Described pushes away
Electrode and extraction electrode is scolded to be in and be coaxially disposed;Described transmission electrode group axial direction is hung down with the axial direction phase of repulsion electrode
Directly.
3) annexation between each region of ion enrichment device:
Ionized region is connected by the centre bore of the pore electrode of ionized region with ion transmission range, ion transmission range and repulsion area lead to
Cross the slit connection of ion transmission range, repulsion area is connected by the extraction electrode in repulsion area with mass analyzer.
2. a kind of ion enrichment method of pulse-pressure, using a kind of ion enrichment device of pulse-pressure, applies in arteries and veins
Rush the method that pulse voltage is applied on electrode, pulsed electrode apply pulse voltage, during low level, ion in pulsed electrode and
Region enrichment between pore electrode;During high voltage, the ion of enrichment moves downward in the presence of electric field, eventually arrives at ion matter
Contents analyzer.By controlling the time delay of the pulse voltage on ionized region and repulsion electrode, ion can be improved and enter quality
The efficiency of analyzer.The arrangement increases mass spectrographic ion utilization ratio of vertical boost-phase time.
Detailed process is as follows:
1) light enters ionized region by light source incidence hole, and sample gas reaches ionized region by capillary tube, and light is in ionized region
Interact with sample gas, so that sample gas molecule is ionized, produce ion.
2) when applying pulses low on pulsed electrode, the voltage on pulsed electrode and pore electrode is higher than on focusing electrode
Voltage, the ion that ionization produces is vibrated due to the ionized region that acts on of electric field, and enrichment in ionized region.
3) when pulse high level is applied on pulsed electrode, the downward warp successively of the ion in ionized region in the presence of electric field
Repulsion area is reached, now ion is pushed into by repulsion electrode applying pulse high level after crossing pore electrode, transmission electrode group and slit
Carry out in mass analyzer separating.
One pulse voltage is applied with above-mentioned pulsed electrode, focusing electrode and pore electrode are applied with DC voltage, arteries and veins
The low level rushing electrode is equal with the voltage of pore electrode, and the voltage of focusing electrode is less than the voltage of pore electrode.
Apply pulse voltage on above-mentioned pulsed electrode, repulsion electrode also applies a pulse voltage, both frequencies simultaneously
Identical, but there is certain time delay, time delay moves to the time in repulsion area for ion from ionized region.
Brief description
Fig. 1 is the ion enrichment apparatus structure schematic diagram of pulse-pressure of the present invention.
In figure, pulsed electrode 1, focusing electrode 2, pore electrode 3, transmission electrode group 4, slit 5, repulsion electrode 6, extraction electrode
7 and mass of ion analyzer 8 constitute, be divided into ionized region 9, ion transmission range 10, repulsion area 11, light source incidence mouth 12, capillary tube
13.
Fig. 2 is ion enrichment process simulation figure of the present invention.
Fig. 3 is pulse voltage waveform figure used herein.
Specific embodiment
The invention will be further described with enforcement below in conjunction with the accompanying drawings.
1. ion enrichment apparatus structure of the present invention as shown in figure 1, pulse-pressure ion enrichment device by ionized region 9, from
Sub- transmission range 10, repulsion area 11 and 8 four region compositions of mass analyzer.
1) structure of each part of ion enrichment device:
1.1), in described ionized region 9, it is sequentially provided with light source incidence hole 12, pulsed electrode 1, focusing electrode 2 and from top to bottom
Pore electrode 3;Described light source incidence hole 12 is located on ionized region pulsed electrode 1 surface wall or side wall;Described pulsed electrode 1 is
It is made up of circular hole sheet metal, centre bore is gradually increased from top to bottom, its function is to produce pulse voltage;Described focusing electricity
Pole 2, is made up of annulus metal electrode, and its function is the ion focusing producing ionized region;Described pore electrode 3, is hollow
Column or mesa-shaped cylinder electrode, centre bore is gradually increased from top to bottom, and its function is to form the ion shaping after focusing on
Ion stream is so as to enter ion transmission range.
It is provided with capillary tube 13 around ionized region 9, sample gas enters into ionized region 9 by capillary tube 13;Use
Capillary tube 13 is the vitreous silica capillary tube through silanization treatment for the surface, 50 μm of internal diameter, length 50cm.
1.2) it is provided with transmission electrode group 4 in described ion transmission range 10, it is the electrode slice structure with holes by a group 2~10
Become, be spaced with insulating trip between electrode slice, for the transmission of ion stream.
1.3) described repulsion area 11, is inside provided with repulsion electrode 6 and extraction electrode 7, and top is provided with slit 5.Described slit 5 is
One rectangular opening, for the shaping of ion stream.Described repulsion electrode 6, is a metal plate electrode, and its function is to produce repulsion electricity
Pressure.Described extraction electrode 7, is perforated metal electrode, and the extraction for repulsion area ion stream is so as to enter mass analyzer.
1.4) described mass analyzer 8 is that a kind of ion by different mass-to-charge ratioes carries out detached device.
2) spatial relation of each part of ion enrichment device:
Described pulsed electrode 1, focusing electrode 2, pore electrode 3, transmission electrode group 4 and slit 5 are in and are coaxially disposed.Described
Repulsion electrode 6 and extraction electrode 7 be in and be coaxially disposed;Described transmission electrode group 4 axial direction and the axial direction of repulsion electrode 6
Direction is perpendicular.
3) annexation between each region of ion enrichment device:
Ionized region 9 is connected by the centre bore of the pore electrode 3 of ionized region 9 with ion transmission range 10, ion transmission range 10 with
Repulsion area 11 is connected by the slit 5 of ion transmission range 10, repulsion area 11 and mass analyzer 8 extraction electrode by repulsion area
7 connections;
2. a kind of ion enrichment method of pulse-pressure, using the ion enrichment device of pulse-pressure, applies in pulse electricity
The extremely upper method applying pulse voltage, applies pulse voltage, during low level, ion is in pulsed electrode 1 and hole on pulsed electrode 1
Region enrichment between electrode 2;During high level, the ion of enrichment moves downward in the presence of electric field, eventually arrives at ion matter
Contents analyzer.By controlling the time delay of the pulse voltage on ionized region 9 and repulsion electrode 6, ion can be improved and enter matter
The efficiency of contents analyzer 8.The arrangement increases mass spectrographic ion utilization ratio of vertical boost-phase time.
Detailed process is as follows:
1) light enters ionized region 9 by light source incidence hole 12, and sample gas reaches ionized region 9 by capillary tube 13, and light exists
Ionized region 9 is interacted with sample gas, so that sample gas molecule is ionized, and produces ion.
2) when applying pulses low on pulsed electrode 1, the voltage on pulsed electrode 1 and pore electrode 3 is higher than to focus on electricity
Voltage on pole 2, the ion that ionization produces is vibrated due to the ionized region 9 that acts on of electric field, and is enriched with ionized region 9.
3) when applying pulse high level on pulsed electrode 1, the ion in ionized region 9 in the presence of electric field is downwards successively
Reach repulsion area 11 after pore electrode 3, transmission electrode group 4 and slit 5, now repulsion electrode 6 apply pulse high level will be from
Son is pushed in mass analyzer 8 and carries out separating.
One pulse voltage is applied with above-mentioned pulsed electrode 1, focusing electrode 2 and pore electrode 3 is applied with DC voltage,
The low level of pulsed electrode 1 is equal with the voltage of pore electrode 3, and the voltage of focusing electrode 2 is less than the voltage of pore electrode 3.
Apply pulse voltage on above-mentioned pulsed electrode 1, repulsion electrode 6 also applies a pulse voltage, Liang Zhepin simultaneously
Rate is identical, but has certain time delay, and time delay moves to the time in repulsion area 11 for ion from ionized region 9.
When the present invention is implemented:
Gas enters ionized region 9 by capillary tube 13, and ultraviolet light enters into ionized region by light source incidence mouth 12.In ionization
In area 9, gaseous sample molecule is interacted with ultraviolet light and ionizes.Applying frequency on pulsed electrode 1 is 10K, dutycycle
For 3%, high level and low level are respectively the pulse voltage of 18V and 14V;Focusing electrode 2 and 3 making alives of pore electrode are respectively
8V and 14V.Light source is the discharge lamp being filled with kr gas, and the ultraviolet photon of the 10.6eV producing during electric discharge passes through light source incidence hole 12
Enter ionized region to be radiated on pore electrode 3, pore electrode 3 surface occurs photoelectric effect to produce photoelectron.
As shown in Fig. 2 (a), when pulses low is applied on pulsed electrode 1, the voltage on pulsed electrode 1 and pore electrode 3
Higher than focusing electrode 2.The ion that ionization produces is vibrated due to the ionized region 9 that acts on of electric field, and rich in ionized region 9
Collection;When pulse high level is applied on pulsed electrode 1, shown in such as Fig. 2 (b), the ion in ionized region in the presence of electric field to
Under sequentially pass through and reach repulsion area 11 after pore electrode 3, transmission electrode group 4 and slit 5, now repulsion electrode 6 applies the high electricity of pulse
Flat ion is pushed in mass analyzer 8 carries out separating.
Pulsed electrode 1 is identical with the frequency of repulsion electrode 6, but has certain time delay.Time delay be ion from
Ionized region 9 moves to the time in repulsion area 11, as shown in Figure 3.
Claims (4)
1. a kind of ion enrichment device of pulse-pressure is it is characterised in that the ion enrichment device of described pulse-pressure is by ionizing
Area (9), ion transmission range (10), repulsion area (11) and (8) four region compositions of mass analyzer;
1) structure of each part of ion enrichment device:
1.1), in described ionized region (9), it is sequentially provided with light source incidence hole (12), pulsed electrode (1), focusing electrode from top to bottom
And pore electrode (3) (2);Described light source incidence hole (12) is located at directly over pulsed electrode (1) on wall or side wall;Described pulse electricity
Pole (1) is to be made up of circular hole sheet metal, and centre bore is gradually increased from top to bottom, and its function is to produce pulse voltage;Described
Focusing electrode (2), be made up of annulus metal electrode, its function is the ion focusing producing ionized region;Described pore electrode
(3), be hollow column or mesa-shaped cylinder electrode, centre bore is gradually increased from top to bottom, its function be will focus on after
Ion shaping forms ion stream so as to enter ion transmission range;In pulsed electrode (1) upper applying pulse voltage, during low-voltage, from
Region enrichment between pulsed electrode (1) and pore electrode (3) for the son;
It is provided with capillary tube (13) around ionized region (9), sample gas enters into ionized region (9) by capillary tube (13);Make
Capillary tube (13) is the vitreous silica capillary tube through silanization treatment for the surface, 50 μm of internal diameter, length 50cm;
1.2) it is provided with transmission electrode group (4) in described ion transmission range (10), it is the electrode slice structure with holes by a group 2~10
Become, be spaced with insulating trip between electrode slice, for the transmission of ion stream;
1.3) it is provided with repulsion electrode (6) and extraction electrode (7) in described repulsion area (11), top is provided with slit (5);Described slit
(5) it is a rectangular opening, for the shaping of ion stream;Described repulsion electrode (6), is a metal plate electrode, and its function is to produce
Raw repulsion voltage;Described extraction electrode (7), is perforated metal electrode, and the extraction for repulsion area ion stream is so as to enter matter
Contents analyzer;
1.4) described mass analyzer (8), is that a kind of ion by different mass-to-charge ratioes carries out detached device;
2) spatial relation of each part of ion enrichment device:
Described pulsed electrode (1), focusing electrode (2), pore electrode (3), transmission electrode group (4) and slit (5) are in and coaxially set
Put;Described repulsion electrode (6) and extraction electrode (7) are in and are coaxially disposed;Described transmission electrode group (4) axial direction with push away
Scold the axial direction of electrode (6) perpendicular;
3) annexation between each region of ion enrichment device
Ionized region (9) is connected by the centre bore of the pore electrode (3) of ionized region (9) with ion transmission range (10), ion transmission range
(10) it is connected by the slit (5) of ion transmission range (10) with repulsion area (11), repulsion area (11) are passed through with mass analyzer (8)
The extraction electrode (7) in repulsion area connects.
2. a kind of ion enrichment method of pulse-pressure is it is characterised in that adopt a kind of pulse-pressure described in claim 1
Ion enrichment device, applies the method applying pulse voltage on pulsed electrode, in pulsed electrode (1) upper applying pulse voltage,
During low-voltage, region enrichment between pulsed electrode (1) and pore electrode (3) for the ion;During high level, the ion of enrichment is in electric field
In the presence of move downward, eventually arrive at mass of ion analyzer;By controlling the arteries and veins on ionized region (9) and repulsion electrode (6)
Rush the time delay of voltage, improve the efficiency that ion enters mass analyzer (8), improve vertical boost-phase time mass spectrographic
Ion utilization ratio;
Detailed process is as follows:
1) light enters ionized region (9) by light source incidence hole (12), and sample gas reaches ionized region (9) by capillary tube (13),
Light is interacted with sample gas in ionized region (9), so that sample gas molecule is ionized, and produces ion;
2) when pulsed electrode (1) upper applying pulses low, the voltage on pulsed electrode (1) and pore electrode (3) is higher than to focus on
Voltage on electrode (2), the ion that ionization produces is vibrated due to the ionized region (9) that acts on of electric field, and in ionized region (9)
Middle enrichment;
3) when pulsed electrode (1) upper applying pulse high level, the ion in ionized region (9) in the presence of electric field is downwards successively
Reach repulsion area (11) after pore electrode (3), transmission electrode group (4) and slit (5), now repulsion electrode (6) applies pulse
High level ion is pushed in mass analyzer (8) and carries out separating.
3. a kind of ion enrichment method of pulse-pressure according to claim 2 is it is characterised in that on pulsed electrode (1)
It is applied with a pulse voltage, focusing electrode (2) and pore electrode (3) are applied with DC voltage, the low level of pulsed electrode 1 and hole
The voltage of electrode 3 is equal, and the voltage of focusing electrode (2) is less than the voltage of pore electrode (3).
4. a kind of ion enrichment method of pulse-pressure according to claim 2 is it is characterised in that on pulsed electrode (1)
Apply pulse voltage, repulsion electrode also applies a pulse voltage on (6) simultaneously, and both frequencies are identical, but have certain delay
Time, time delay moves to the time of repulsion area (11) for ion from ionized region (9).
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CN112951702B (en) * | 2019-12-10 | 2023-01-03 | 中国科学院大连化学物理研究所 | Ion control and transmission device for mass spectrometer |
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