CN101750265B - Time-of-flight mass spectrometer for measuring ratio of nano-particle component elements in real time - Google Patents
Time-of-flight mass spectrometer for measuring ratio of nano-particle component elements in real time Download PDFInfo
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- CN101750265B CN101750265B CN2008102298819A CN200810229881A CN101750265B CN 101750265 B CN101750265 B CN 101750265B CN 2008102298819 A CN2008102298819 A CN 2008102298819A CN 200810229881 A CN200810229881 A CN 200810229881A CN 101750265 B CN101750265 B CN 101750265B
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Abstract
The invention relates to a time-of-flight mass spectrograph, in particular to a time-of-flight mass spectrometer for measuring ratio of nano-particle component elements in real time, comprising a pulse sampling device, a beam source chamber and a time-of-flight mass spectrum mass analyzer provided with an ionization chamber. The time-of-flight mass spectrometer is characterized in that the ionization chamber is positioned in the time-of-flight mass spectrum mass analyzer, the front end of the pulse sampling device is connected with a pulse valve, the pulse sampling device is inserted into the beam source chamber, the beam source chamber is positioned directly above the laser ionization chamber, the outlet of the beam source chamber is connected with the laser ionization chamber through a nozzle, a nanosecond long wavelength high-energy laser is installed at the outer side of the time-of-flight mass spectrum mass analyzer, the high-energy laser beams emitted by the laser pass through the ionization chamber vertically so as to ionize nano-particles completely into univalent and high valence ions, the ratio of the high valence ions can accurately reflect the ratio of nano-particle component elements, and the ions produced by ionization can be recorded by the time-of-flight mass spectrograph. The invention can measure the ratio of nano-particle component elements rapidly, and the measurement is not influenced by ionization laser energy.
Description
Technical field
The invention belongs to mass spectrometer; Relate in particular to and a kind ofly measure the time of-flight mass spectrometer of nano particle component ratio, can carry out real-time measurement less than the nano particle component ratio of 10nm to particle diameter through this technology with the laser ionization method.
Background technology
Gasoloid is solid-state or liquid particles is scattered in formed disperse phase system in the gas phase media, is the important component part of earth atmosphere.Gasoloid can be divided into primary gas colloidal sol and secondary gasoloid according to the source.Primary gas colloidal sol comes from the direct shattering process of solid, liquid substance, bursts and volcanic explosion etc. like airborne dust, spindrift, ocean bubble.Secondary aerocolloidal main source is that gas-grain transforms, and pollution course that some are important such as acid rain, photo-chemical smog are all relevant therewith.Gas-grain transforms and forms new particle is a very complex physicochemical process, is that the scholar of representative proposes nucleating growth process neodoxy (Atomos.Chem.Phys., 2004,4:2553 with Kulmala; J.Aerosol Sci.2004 35:143-176), thinks possibly exist a large amount of thermodynamically stable inferior nano particles in the atmosphere; These inferior nano particles are sources of nucleation process; But because the particle diameter of these particles is too little, do not have suitable instrument that its chemical composition is measured at present, therefore how to measure (0.5～5nm) the particle of nano-scale in the atmosphere; And knowing their chemical composition and structure, is the key of understanding atmosphere new particle mechanism of production and differentiation.
Because the collection efficiency of nano particle is low, reactive strong, poor stability, when using traditional off-line technology to measure, the chemical composition of nano particle possibly change or be contaminated.The online gasoloid mass-spectrometric technique of development in recent years; As with Prather being laser ionization single-particle gasoloid mass spectrum (the Aerosol Time-of-flight Mass Spectrometry of representative; ATOFMS) with electron impact ionization gasoloid mass spectrum (the Aerosol Mass Spectrometer of Aerodyne company; AMS); In aerocolloidal source resolution and heterogeneous phase chemical reaction research, obtained success; But these two kinds of gasoloid mass-spectrometric techniques adopt aerodynamics lens continuous sample introductions, and are low less than the particulate transfer efficiency of 50nm to particle diameter. and AMS need earlier with after the particulate thermal desorption through electron impact ionization, the difficulty volatilization inorganic component in can't the measurement of gas sol particles.Laser almost can be with the effective ionization of all elements; But used laser power is lower among the ATOFMS, and particulate ectomesoderm element is easy to ionization than inner layer elements, has the incomplete phenomenon of ionization; The qualitative information that particle is formed can only be obtained, quantitative information can not be obtained.
Summary of the invention
The purpose of this invention is to provide a kind of time of-flight mass spectrometer that is used for the on-line measurement size less than the nano particle element ratios of 10nm, can obtain the quantitative information of nanosecond particle composition, measurement result is accurate.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is:
A kind of time of-flight mass spectrometer of real-time measurement nano particle component ratio; Comprise pulse sampling device, electron gun chamber and have the flight time mass spectrum mass analyzer of ionization chamber, it is characterized in that: it is inner that ionization chamber is positioned at the time of flight mass analyzer, and the front end of pulse sampling device stretches into the electron gun chamber interior; The electron gun chamber is positioned at directly over the ionization chamber; The exit of electron gun chamber be provided with one have a center micropore nozzle, the electron gun chamber is connected with ionization chamber through nozzle, a nanosecond laser is arranged at the outside of flight time mass spectrum mass analyzer; The high energy laser beam that laser instrument sends vertically passes ionization chamber; With the complete ionization of nano particle is the monovalence and the high valence ion of its component, can accurately obtain the ratio of nano particle component from its high valence ion ratio, the ion that is produced by the ionization of time of-flight mass spectrometer record.
The sample introduction end of pulse sampling device is provided with a pulse valve; The center micropore of pulse valve and the center micropore of nozzle are on the same axis; It can improve the nano particle transfer efficiency producing the difference vacuum between electron gun chamber and the pulse sampling device, between electron gun chamber and the laser ionization chamber, and nozzle center's micro-pore diameter is 1～3mm.Can be according to the requirement of sample size and vacuum, the distance between regulating impulse valve and the nozzle, its distance can be 2～10mm.
Be provided with a difference molecular pump in the outside of said electron gun chamber, the difference molecular pump links to each other with opening on the side wall surface of electron gun chamber through pipeline; Be provided with a part pump in the said flight time mass spectrum mass analyzer outside, molecular pump links to each other with opening on the flight time mass spectrum mass analyzer side wall surface through pipeline.Electron gun chamber and flight time mass spectrum mass analyzer respectively by 110, the 600L/s molecular pump bleeds, and keeps the mass spectrum vacuum.
Said ionization chamber is made up of the repulsion electrode, extraction electrode and the accelerating electrode that laterally arrange successively; High energy laser beam passes from repulsion electrode and extraction electrode central vertical, on the central axis of repulsion electrode, extraction electrode and accelerating electrode, in the accelerating electrode outboard shafts to being provided with a field-free flight pipe; The nano particle bundle that forms through regulating impulse valve, electron gun chamber, nozzle from the pulse sampling device gets into ionization chamber and crossing with high energy laser beam; And high energy laser beam is vertical in twos with nano particle bundle and field-free flight pipe three; The light path of the superlaser that laser instrument sends is provided with condenser lens, and the intersection point that the focus of condenser lens and high energy laser beam and nano particle bundle intersect coincides.
Be provided with a detecting device at said field-free flight Guan Weiduan, detecting device is connected with the data acquisition card signal through lead; One pulse producer is connected with data collecting card, pulse valve and laser signal respectively.Through the sequential that pulse producer control data capture card, pulse valve and laser instrument are opened, pass through the width of pulse producer gating pulse opening of valves simultaneously, to reach effective transmission to nano particle.
Said laser instrument can produce high power long wavelength pulse laser, and laser wavelength range 532～1064nm, laser pulse width are nanosecond, laser power density scope 10
9～10
11W/cm
2
Nano particle component provided by the invention compares value measurement mechanism; Adopt pulse mode that nano particle is introduced the electron gun chamber; The electron gun chamber is adopted the molecule pump side to take out and is formed the difference vacuum; Can in time unnecessary carrier gas be taken away, utilize the pressure reduction of pulse valve moment unlatching effectively nano particle to be formed particle beams introducing mass spectrum simultaneously.Select the size of the nano particle of surveying through changing time delay that ionization laser and pulse valve open, raising laser is to the efficient of hitting of nano particle.Package unit can carry out on-line measurement less than the nano particle of 10nm to particle diameter, in the generation of atmosphere new particle and Evolution Mechanism research, important effect is arranged.
Description of drawings
Fig. 1 is a nano particle element ratios measurement mechanism synoptic diagram of the present invention.
Fig. 2 is the mass signal figure of ether nano particle among the embodiment 1.
When Fig. 3 is 532nm for optical maser wavelength among the embodiment 1, the C of ether nano particle
2+/ O
2+High valence ion ratio is with the variation diagram of laser energy.
When Fig. 4 is 1064nm for optical maser wavelength among the embodiment 1, the C of ether nano particle
2+/ O
2+High valence ion ratio is with the variation diagram of laser energy.
When Fig. 5 is 532nm for optical maser wavelength among the embodiment 2, the C of ethanol nano particle
2+/ O
2+High valence ion ratio is with the variation diagram of laser energy.
Embodiment
See also Fig. 1, a kind of time of-flight mass spectrometer of real-time measurement nano particle component ratio comprises pulse sampling device 1, electron gun chamber 2 and has the flight time mass spectrum mass analyzer 4 of ionization chamber 3; Ionization chamber 3 is positioned at time of flight mass analyzer 4 inside; 2 inside, electron gun chamber are stretched in holding of pulse sampling device 1, and electron gun chamber 2 is positioned at directly over the ionization chamber 3, the exit of electron gun chamber 2 be provided with one have a center micropore nozzle 6; Electron gun chamber 2 is connected with ionization chamber 3 through nozzle 6; Nozzle center's micro-pore diameter is 1～3mm, between electron gun chamber 2 and laser ionization chamber 3, forms pressure reduction, is beneficial to nano particle is introduced ionization chamber; One laser instrument 16 is arranged at the outside of flight time mass spectrum mass analyzer 4; The high energy laser beam 12 that laser instrument 16 sends vertically passes ionization chamber 3; With the complete ionization of nano particle is the monovalence and the high valence ion of its component; Can accurately obtain the ratio of nano particle component from its high valence ion ratio, the ion that produces by time of-flight mass spectrometer 4 record ionization.
The sample introduction end of pulse sampling device 1 is provided with a pulse valve 5; The center micropore of pulse valve 5 and the aperture of nozzle 6 are on the same axis; Can be according to the requirement of sample size and vacuum, the distance between regulating impulse valve 5 and the nozzle 6, its distance can be 2～10mm; The molecular pump pumping speed is 110L/s, and electron gun chamber vacuum tightness maintains 10 during sample introduction
-2～10
-1About Pa;
Be provided with a difference molecular pump 7 in the outside of said electron gun chamber 2, difference molecular pump 7 links to each other with opening on 2 side wall surfaces of electron gun chamber through pipeline, is used to form the difference vacuum, removes unnecessary carrier gas.
Said ionization chamber 3 is made up of the repulsion electrode 8 that laterally arranges, extraction electrode 9 and accelerating electrode 10 successively; High energy laser beam 12 passes from repulsion electrode 8 and extraction electrode 9 central vertical, on the central axis of repulsion electrode 8, extraction electrode 9 and accelerating electrode 10, in accelerating electrode 10 outboard shafts to being provided with a field-free flight pipe 13; The nano particle bundle 11 that forms through regulating impulse valve 5, electron gun chamber 2, nozzle 6 from pulse sampling device 1 gets into ionization chamber 3 and crossing with high energy laser beam 12; And high energy laser beam 12 is vertical in twos with nano particle bundle 11 and field-free flight pipe 13 threes.Repulsion electrode, extraction electrode and accelerating electrode, distance is 20mm between repulsion electrode and the extraction electrode, and distance is 10mm between extraction electrode and the accelerating electrode, and it is 2800,1680 that three pole plates add high pressure, 0V.
Do not hold at said field-free flight pipe 13 to be provided with a detecting device 14, detecting device 14 is connected with data collecting card 15 signals through lead.
One pulse producer 17 is connected with data collecting card 15, pulse valve 5 and laser instrument 16 signals respectively.
The light path of the superlaser that laser instrument 16 sends is provided with condenser lens 19, and a focus of condenser lens 19 coincides with the intersection points that high energy laser beam 12 and nano particle bundle 11 intersect.
Said laser instrument 16 can produce high power long wavelength pulse laser, and laser wavelength range 532～1064nm, laser pulse width are nanosecond, and line focus lens 19 focus on back laser power density scope 10
9～10
11W/cm
2
Be provided with a part pump 18 in said flight time mass spectrum mass analyzer 4 outsides, molecular pump 18 links to each other with opening on flight time mass spectrum mass analyzer 4 side wall surfaces through pipeline.
High energy laser beam 12 is from repelling pole plate 8 and drawing pole plate 9 centers and pass, and is orthogonal with group's bunch particle beams 11 and time of flight mass analyzer 13.High energy long wavelength nanosecond laser can be the monovalence and the high valence ion of corresponding component with the complete ionization of nano particle, by the ion of time of flight mass analyzer 4 record ionization generations.Can select to measure the nano particle of different-grain diameter through changing the sequential relationship between pulse laser and pulse valve 5 unlatchings.
During application, the time of flight mass analyzer keeps the mass spectrum high vacuum by 600L/s molecular pump 18.Come the sequential relationship between gating pulse valve, laser instrument and the data acquisition through pulse producer.According to the difference of nano-particles size, through changing the size of selecting the nano particle of surveying time delay that pulse valve and laser instrument are opened, this time is generally 300～1000us.
Ionization laser is long wavelength's nanosecond laser, wavelength coverage 532nm～1064nm, and the laser spot power density is 10
9～10
11W/cm
2All can, laser pulse frequency is identical with the pulse valve frequency, by the unlatching of pulse producer gating pulse valve and the sequential relationship between the laser, thereby selects the particle diameter of the nano particle of surveying.Used superlaser can be with the complete ionization of nano particle, the measuring error that does not exist ionization not exclusively to cause, and the nano particle element ratio is only relevant with the component of particle, and irrelevant with selected optical maser wavelength and energy, the result is accurate.
The present invention can measure the nano particle element ratios fast, measures the influence that not changed by the ionization laser energy.
Embodiment 1
Embodiment 1
In order to investigate the ionizing efficiency of laser energy, under low laser energy, the ether nano particle of particle diameter less than 10nm detected cluster molecule.The ether nano particle is produced by Bubbling method; Be specially ether liquid is placed in the container; The argon gas of certain pressure imports under the liquid level through stainless-steel tube; The argon gas that overflows under the liquid level carries ether liquid and introduces the pulse sampling device from another stainless-steel tube, after pulse valve, forms the ether nano particle of particle diameter less than 10nm.Fig. 2 is the flight time mass spectrum figure of ether nano particle in apparatus of the present invention, and used laser energy is 7.6 * 10
9W/cm
2, optical maser wavelength is 532nm, and the opening time of laser relative pulse valve is 700us, and the frequency of laser and pulse valve is 5Hz.The molion that does not have ether in the spectrogram, appearance be ether component C
+, H
+, O
+And high valence ion C
Q+(q=2～4), O
Q+(q=2～4).Strong interaction has taken place in explanation between laser under this laser energy and ether nano particle, the ether molecule is monovalence and corresponding high valence ion by ionization fully.
Change influence in order to investigate laser energy, change laser energy and measure measurement result.Fig. 3 is under the same experimental conditions, C in the ether nano particle ionization spectrogram
2+/ O
2+Ratio is with the variation tendency of laser energy.Can see, although laser energy is by 7.6 * 10
9Increase to 1.4 * 10
11W/cm
2, change about 20 times, C
2+/ O
2+Ratio is always about 4; Basically do not change with laser energy; This with the ether molecule in C, O element ratio consistent, explain with this kind method and can accurately measure, and the measurement result influence that not changed by the ionization laser energy the element ratio of ether nano particle.
For investigating the influence of optical maser wavelength, be to measure under the 1064nm condition in optical maser wavelength to measurement result.C in ether nano particle ionization spectrogram when Fig. 4 is 1064nm for optical maser wavelength
2+/ O
2+Ratio is with the variation tendency of laser energy, and other experiment condition is identical with Fig. 2.C
2+/ O
2+Ratio can reflect C, O element ratios in the ether equally between 3.5～4.
Fig. 5 is under the different laser energy, C in the ethanol nano particle ionization spectrogram
2+/ O
2+Ratio is with the variation tendency of laser energy.Used optical maser wavelength is 532nm, and range of laser energy is 9.0 * 10
9～1.3 * 10
11W/cm
2The opening time of laser relative pulse valve is 900us, and the frequency of laser and pulse valve is 10Hz.Can see C
2+/ O
2+Ratio range is 1.5～2.0, and this is near C, O element ratio 2 in the ethanol molecule.Embodiment 1 and 2 result explain with this kind method and can carry out quantitative measurment to the element ratio of nano particle, and measurement result do not receive the influence of ionization laser energy, wavelength change.
Claims (10)
1. time of-flight mass spectrometer of measuring in real time nano particle component ratio; Comprise pulse sampling device (1), electron gun chamber (2) and have the flight time mass spectrum mass analyzer (4) of ionization chamber (3); It is characterized in that: ionization chamber (3) is positioned at flight time mass spectrum mass analyzer (4) inside; The front end of pulse sampling device (1) stretches into inside, electron gun chamber (2), and electron gun chamber (2) are positioned at directly over the ionization chamber (3), the exit of electron gun chamber (2) be provided with one have a center micropore nozzle (6); Electron gun chamber (2) is connected with ionization chamber (3) through nozzle (6); Laser instrument (16) is arranged at the outside of flight time mass spectrum mass analyzer (4), and the high energy laser beam (12) that laser instrument (16) sends vertically passes ionization chamber (3), is the monovalence and the high valence ion of its component with the complete ionization of nano particle; Can accurately obtain the ratio of nano particle component from its high valence ion ratio, the ion that produces by the ionization of flight time mass spectrum mass analyzer (4) record.
2. time of-flight mass spectrometer according to claim 1 is characterized in that: the sample introduction end of pulse sampling device (1) is provided with a pulse valve (5); The center micropore of the center micropore of pulse valve (5) and nozzle (6) is on the same axis.
3. time of-flight mass spectrometer according to claim 2 is characterized in that: can be according to the requirement of sample size and vacuum, and the distance between regulating impulse valve (5) and the nozzle (6), its distance can be 2～10mm.
4. time of-flight mass spectrometer according to claim 1 is characterized in that: be provided with a difference molecular pump (7) in the outside of said electron gun chamber (2), difference molecular pump (7) links to each other with opening on the side wall surface of electron gun chamber (2) through pipeline.
5. time of-flight mass spectrometer according to claim 1; It is characterized in that: said ionization chamber (3) is made up of the repulsion electrode (8) that laterally arranges, extraction electrode (9) and accelerating electrode (10) successively; High energy laser beam (12) passes from repulsion electrode (8) and extraction electrode (9) central vertical, on the central axis of repulsion electrode (8), extraction electrode (9) and accelerating electrode (10), in accelerating electrode (10) outboard shafts to being provided with a field-free flight pipe (13); The nano particle bundle (11) that forms through regulating impulse valve (5), electron gun chamber (2), nozzle (6) from pulse sampling device (1) gets into ionization chamber (3) and crossing with high energy laser beam (12); And high energy laser beam (12) is vertical in twos with nano particle bundle (11) and field-free flight pipe (13) three.
6. time of-flight mass spectrometer according to claim 5 is characterized in that: do not hold at said field-free flight pipe (13) to be provided with a detecting device (14), detecting device (14) is connected with data collecting card (15) signal through lead.
7. time of-flight mass spectrometer according to claim 1; It is characterized in that: a pulse producer (17) is connected with data collecting card (15), pulse valve (5) and laser instrument (16) signal respectively; Sequential through pulse producer (17) control data capture card (15), pulse valve (5) and laser instrument (16) unlatching; The width of opening through pulse producer (17) gating pulse valve (5) simultaneously is to reach the effective transmission to nano particle.
8. time of-flight mass spectrometer according to claim 1; It is characterized in that: the light path of the superlaser that laser instrument (16) sends is provided with condenser lens (19), and the intersection point that the focus of condenser lens (19) and high energy laser beam (12) and nano particle bundle (11) intersect coincides.
9. time of-flight mass spectrometer according to claim 1 is characterized in that: said laser instrument (16) can produce high power long wavelength pulse laser, laser wavelength range 532～1064nm, and laser pulse width is a nanosecond, the laser power density scope 10 after the focusing
9～10
11W/cm
2
10. time of-flight mass spectrometer according to claim 1; It is characterized in that: be provided with a part pump (18) in said flight time mass spectrum mass analyzer (4) outside, molecular pump (18) links to each other with opening on flight time mass spectrum mass analyzer (4) side wall surface through pipeline.
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| CN115020188B (en) * | 2022-07-15 | 2022-10-11 | 广东省麦思科学仪器创新研究院 | Single-particle mass spectrometer, laser ionization device and laser ionization method thereof |
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