CN100454477C - Single particle aerosol on-line ionization source and its realization method - Google Patents
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Abstract
本发明提供一种单颗粒气溶胶在线电离源，设置于飞行时间质量分析器的加速区之外，包括电离激光器、低压射频四极杆，所述电离激光器发射的激光束垂直于低压射频四极杆入射至其内切圆心。一种利用前述电离源实现的方法，主要是对单颗粒气溶胶利用空气动力学测径后，在其进入飞行时间质量分析器之前，利用电离激光将其电离成等离子体，所产生的正负离子利用低压射频四极杆聚焦成相空间很小的离子束再送入飞行时间质量分析器中。本发明将电离区与空气动力学测径区连为一体，测径结束的同时气溶胶电离，最大程度缩小了气溶胶的漂移距离，明显提高了传输效率；低压射频四极杆的聚焦作用明显提高了飞行时间质量分析器的分辨率。
The invention provides a single-particle aerosol on-line ionization source, which is arranged outside the acceleration zone of a time-of-flight mass analyzer, and includes an ionization laser and a low-voltage radio frequency quadrupole. The laser beam emitted by the ionization laser is perpendicular to the low-voltage radio frequency quadrupole The rod is incident on its inscribed circle center. A method realized by using the aforementioned ionization source, which mainly uses an ionization laser to ionize the single-particle aerosol into plasma after using aerodynamic diameter measurement before it enters the time-of-flight mass analyzer, and the positive and negative ions generated A low-voltage RF quadrupole is used to focus an ion beam with a small phase space and then send it to a time-of-flight mass analyzer. The invention integrates the ionization area and the aerodynamic diameter measurement area, and the aerosol is ionized at the same time as the end of the diameter measurement, which greatly reduces the drift distance of the aerosol and significantly improves the transmission efficiency; the focusing effect of the low-voltage radio frequency quadrupole is obvious Improved the resolution of the time-of-flight mass analyzer.
Description
Technical field
The present invention relates to the aerosol particle line Measurement Technique, particularly a kind of single-particle aerosol online ionization source and its implementation.
Background technology
Aerocolloidal size and chemical composition thereof cause significant impact to global climate, air quality, environmental health.Individual particle aerosol on-line monitoring time-of-flight mass spectrometer (Aerosol Time-of-flightMass Spectrometer, ATOFMS) be a kind of new technology that developed recently gets up, can real time on-line monitoring individual particle aerosol air kinetic diameter and air pollution composition thereof, be to judge that aerosol forms and the important means in source, its basic principle is to measure the aerosol diameter by the aerodynamics method, with aerosol ionization, the ion that ionization forms detects with mass spectrometer again.The method of concrete aerodynamic measurement aerosol particle diameter and time of flight mass analyzer detect the method for ion and consult document Mass Spectrometry of Aerosols, David T.Suess and Kimberly A.Prather, Chem.Rev.1999,99,3007-3035.Laser ionization source is adopted in the aerocolloidal online ionization of individual particle usually, and with the time of flight mass analyzer as the ion signal detector, in order to monitor a negative ions in the particle simultaneously, need two time of flight mass analyzers.
Because aerosol is the electric neutrality particle, and the transmission in a vacuum of electric neutrality particle can't be modulated with the electronic and ionic optical system, transmission range aerocolloidal detection efficiency far away more is just low more.In the existing device, aerocolloidal aerodynamics is calibrated distance and is generally 5～10 centimetres at present, and ion source also has other 10～20 centimetres from diameter measuring zone, and therefore aerocolloidal transmission range generally reaches 15～30 centimetres.This is because in existing device, ionization source (laser ionization source) is arranged in the time of flight mass analyzer, aerosol need enter in the time of flight mass analyzer and just can be ionized, so its transmission range is far away relatively, has produced the lower problem of aerosol detection efficiency thus.Simultaneously since in existing device laser ionization directly occur in the time of flight mass analyzer, the ion that ionization produces has bigger initial kinetic energy to be disperseed, and causes the mass resolution of time of flight mass analyzer on the low side, only about 500.
Summary of the invention
The shortcoming that the objective of the invention is to overcome prior art provides a kind of rational in infrastructure with not enough, can improve aerosol efficiency of transmission and ionization hit rate, and can improve the single-particle aerosol online ionization source of the mass resolution of time of flight mass analyzer.
Another object of the present invention is to provide a kind of implementation method of above-mentioned single-particle aerosol online ionization source.
Purpose of the present invention is achieved through the following technical solutions: a kind of single-particle aerosol online ionization source, be arranged at outside the accelerating region of time of flight mass analyzer, comprise ionization laser, low pressure radiofrequency quadrupole, described ionization laser emitted laser bundle is incident to the incenter of low pressure radiofrequency quadrupole perpendicular to the low pressure radiofrequency quadrupole, will arrive the aerosol ionization of incenter position.
Described ionization laser emitted laser bundle is perpendicular to the low pressure radiofrequency quadrupole and in the axial center incident of low pressure radiofrequency quadrupole.
Described low pressure radiofrequency quadrupole is meant the quadrupole rod ion transfer device under certain air pressure.
Described low pressure radiofrequency quadrupole has the gap of four direction, is respectively the secondary ionization laser entrance port of calibrating laser entrance port, secondary scattered light exit portal and laser ionization system of aerocolloidal intake, laser diameter measurement system.
Described ionization laser is connected with the secondary photomultiplier of calibrating of laser diameter measurement system, and the trigger impulse of ionization laser is provided by secondary output signal of calibrating photomultiplier.
Every bar of described low pressure radiofrequency quadrupole mechanically is made up of more piece bar section, is provided with the gap between each pole section to guarantee electric insulation, and the gap between the adjacent two pole sections is less than 0.3mm.
Described low pressure radiofrequency quadrupole is provided with the axial DC electric field; The DC potential of the low pressure radiofrequency quadrupole position that described laser beam vertical incidence point is corresponding is set to 0V, increase respectively and reduce toward the opposite two ends DC potential of low pressure radiofrequency quadrupole direction, form the axial DC electric field to guarantee cation toward the negative voltage side migration, anion is toward the positive voltage terminal migration.
Each pole section of described low pressure radiofrequency quadrupole applies identical radio-frequency voltage with focused ion, and described radio-frequency voltage is in the same place by inductance, resistance and capacitive coupling with direct voltage.
Described low pressure radiofrequency quadrupole is positioned at a cavity, and the gas in the described cavity is generally the good gas of chemical stability, as: helium, nitrogen, argon gas etc.; The size that the air pressure of described gas is looked ion to be tested is arranged on the scope between 0.1Pa～100Pa.
The time of flight mass analyzer of this single-particle aerosol online ionization source is vertical introduction-type time of flight mass analyzer, and described vertical introduction-type time of flight mass analyzer is provided with two, detects negative ions respectively.In addition, if interested in the molecular structure of aerosol composition, can connect cascade mass spectrometer behind the low pressure radiofrequency quadrupole promptly can provide the tandem analysis.
This single-particle aerosol online ionization source and aerodynamics diameter measuring zone are connected as a single entity, and the secondary laser of calibrating is identical with the position of ionization laser action, promptly when finishing aerodynamics and calibrating, carry out ionization.It is same as the prior art that the aerosol air dynamics that the present invention relates to is calibrated technology.
In order to make all ions obtain detecting, negative ions can be sent into vertical introduction-type time of flight mass analyzer in low pressure radiofrequency quadrupole two ends tens microseconds of accumulation respectively again.The low pressure radiofrequency quadrupole principle of band axial field is identical with existing technology, and ion is also identical with prior art in the accumulation technology at quadrupole rod two ends.
A kind of method of utilizing above-mentioned single-particle aerosol online ionization source to realize, it is characterized in that: after utilizing aerodynamics to calibrate to the individual particle aerosol, before it enters the accelerating region of time of flight mass analyzer, utilize laser that it is ionized into plasma, the negative ions that is produced utilizes the low pressure radiofrequency quadrupole to be focused into the very little ion beam of phase space and sends in the time of flight mass analyzer again and detect.
Utilize the axial DC electric field of low pressure radiofrequency quadrupole setting to make the negative ions that produces after the ionization separately and respectively move (the past electronegative potential direction migration of cation wherein to the two ends of low pressure radiofrequency quadrupole, and anion is simultaneously toward the migration of high potential direction), detected by different time of flight mass analyzers respectively then.
The pulse that utilizes second photomultiplier of aerodynamics measurement diameter system to produce triggers the ionization laser immediately and sends laser pulse, utilizes this laser pulse that the individual particle aerosol is ionized into plasma; Owing to calibrate ionization take place when finishing immediately, can improve the ionization hit rate like this.
Action principle of the present invention is: establish m
i/ q, U
Rf, ω, r
0Be respectively radio-frequency voltage, rf frequency, the quadrupole rod inscribed circle radius of ion mass-to-charge ratio, quadrupole rod, quadrupole rod is to leaving effective potential trough U of ion formation that inscribed circle centre distance is r
Eff, its size is
Select suitable parameter, can be so that this effective potential trough reaches several even tens electron-volts.Therefore the present invention moves on to traditional aerosol ionized region the aerosol transmission range of low vacuum from the time of flight mass analyzer of high vacuum, and ionization is occurred in the center of low pressure radiofrequency quadrupole, utilize constraint and the aggtegation of the potential trough of low pressure radiofrequency quadrupole to ion, collect all ions that ionization obtains from aerosol, and be focused into the very little ion beam of phase space and deliver to again in the time of flight mass analyzer.Owing to have axial electric field, migration is separated negative ions to low pressure radiofrequency quadrupole two ends respectively, because grain diameter measurement and ionization take place in the same space position, improved the ionization hit rate, owing to detecting with mass of ion, aerocolloidal ionization separates fully again, ion source reduces to minimum to the influence of analyzer, has obviously improved the mass resolution of time of flight mass analyzer.
The relative prior art of the present invention has following advantage and effect: (1) the present invention is connected as a single entity ionized region and aerodynamics diameter measuring zone, aerodynamics is calibrated when finishing aerosol ionization, farthest dwindle aerocolloidal drift distance, obviously improved efficiency of transmission and ionization hit rate.(2) along with the increase of tested component molecules amount in the aerosol, structural analysis is more and more important, carry out structural analysis and need use the tandem mass spectrometry technology, and traditional individual particle aerosol on-line monitoring mass-spectrometric technique can not reach this purpose.Since the technology of the present invention earlier with ion collection in radiofrequency quadrupole, thereby can with the coupling of cascade mass spectrometry device, the ion that is produced can be detected by tandem mass spectrometry, for the structural analysis of molecular ion provides may.(3) utilize the present invention can make measurement of aerosol particle diameter and ionization take place in the same space position, and detect with mass of ion and to separate fully, utilize the low pressure radiofrequency quadrupole to reduce the phase space of ion beam in advance simultaneously, can improve the mass resolution of time of flight mass analyzer.
Description of drawings
Fig. 1 is the structural representation of apparatus of the present invention.
Fig. 2 is the dc offset voltage of low pressure radiofrequency quadrupole of device shown in Figure 1 and the coupling schematic diagram of radio-frequency voltage.
Fig. 3 is the schematic diagram and the pulse sequence figure of the inventive method.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment
Fig. 1～Fig. 3 shows the concrete structure of apparatus of the present invention, as seen from Figure 1, this single-particle aerosol online ionization source vertical introduction-type time of flight mass analyzer 5,6 of comprising instrument vacuum cavity 1, aerosol injector 2, low pressure radiofrequency quadrupole 3 and quadrupole rod cavity 4, laser diameter measurement and laser ionization system and detecting positive and negative ion simultaneously; 7 is the aerosol of being introduced by aerosol injector 2; Low pressure radiofrequency quadrupole 3 is positioned at quadrupole rod cavity 4, and the gas in the described quadrupole rod cavity is generally purity and is higher than 99.99% the good gas of chemical stability, as: gas or other inert gases such as helium, nitrogen, argon gas; The size that the air pressure of described gas is looked ion to be tested is arranged on the scope between 0.1Pa～100Pa.
As shown in Figure 3, low pressure radiofrequency quadrupole 3 has the gap of four direction, and wherein two of horizontal direction gaps are respectively the intake of aerosol 7 and the intake of ionization laser beam 19; The gap of the upper and lower both direction of vertical direction is respectively the secondary entrance port of laser 17 and the measurement mouth of secondary scattered light 21 calibrated of laser diameter measurement system; The ionization laser beam 19 of ionization laser 18 emissions is perpendicular to low pressure radiofrequency quadrupole 3, and be incident to the incenter of low pressure radiofrequency quadrupole 3 in low pressure radiofrequency quadrupole 3 axial centers, ionization laser 18 is connected with the secondary photomultiplier 20 of calibrating, by its pulse-triggered that provides; The two ends of low pressure radiofrequency quadrupole 3 are connected with vertical introduction-type time of flight mass analyzer 5,6 respectively.
Every bar of described low pressure radiofrequency quadrupole 3 mechanically is made up of more piece bar section 8, and concrete structure is provided with the gap to guarantee electric insulation between each pole section 8 shown in Fig. 2 (a), and the gap between the adjacent two pole sections 8 is less than 0.3mm; Between adjacent two pole sections 8, resistance 9 and electric capacity 10 have been arranged in parallel; Each pole section 8 added radio-frequency voltage and dc offset voltage are coupled by resistance 9 and electric capacity 10, the direct current biasing negative voltage is added on the node 11, the direct current biasing positive voltage is added on the node 12, other respectively saves dc offset voltage and is formed by resistance 9 dividing potential drops, and radio-frequency voltage is added on the node 13, and pass to each pole section by electric capacity 10, thereby the added radio-frequency voltage of each pole section is identical.Fig. 2 (b) is depicted as low pressure radiofrequency quadrupole 3 direct current biasing Potential distribution vertically, center voltage is 0V, left end node 12 is provided with positive potential to attract anion, right-hand member node 11 is provided with negative potential to attract cation, increase respectively and reduce toward the opposite two ends DC potential of low pressure radiofrequency quadrupole direction, form the axial DC electric field, the potential difference Δ v at two ends can control the migration rate of ion.
Fig. 3 (a) calibrates and the ionization process schematic diagram for aerosol particle, and shown in Fig. 3 (a), the laser 14,16 of calibrating of laser diameter measurement and laser ionization system is in normally open and gives off laser beam 15,17.Aerosol 7 process laser beams 15,17 scattered beams of being introduced by aerosol injector 2 from atmosphere that produced 21,23 are respectively by photomultiplier 20,22 records, and produce two the at interval electric pulses 24,25 of t of certain hour are arranged, shown in Fig. 3 (b), aerocolloidal drift velocity v=l/t can be calculated according to the time interval t of two pulses and the space length l of two bundle laser 15,17, aerocolloidal aerodynamic diameter can be measured by the relation of proofreading and correct aerocolloidal drift velocity and particle diameter.The aerosol that photomultiplier 20 records arrives the trigger impulse 26 of pulse 25 as ionization laser 18, promptly when aerosol arrives low pressure radiofrequency quadrupole 3 incenter positions, applies ionization laser pulse 19, with aerosol ionization.Under the effect of ionization laser pulse 19, aerosol is ionized the generation plasma, cation wherein moves toward electronegative potential direction (node 11 ends among Fig. 2 (a)), and anion is detected by vertical introduction-type time of flight mass analyzer 5,6 respectively at last simultaneously toward high potential direction (node 12 ends among Fig. 2 (a)) migration.
Because in apparatus of the present invention, the generation of ion separates fully with the quality testing of ion, the ion that is produced can be delivered in any mass spectrometer and analyze.With apparatus of the present invention and the coupling of cascade mass spectrometry device, can carry out the structural analysis of aerosol component.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1, a kind of single-particle aerosol online ionization source, it is characterized in that: be arranged at outside the accelerating region of time of flight mass analyzer, comprise ionization laser, low pressure radiofrequency quadrupole, described ionization laser emitted laser bundle is incident to the incenter of low pressure radiofrequency quadrupole perpendicular to the low pressure radiofrequency quadrupole.
2, single-particle aerosol online ionization source according to claim 1 is characterized in that: described ionization laser emitted laser bundle is perpendicular to the low pressure radiofrequency quadrupole and in the axial center incident of low pressure radiofrequency quadrupole.
3, single-particle aerosol online ionization source according to claim 1 and 2, it is characterized in that: described low pressure radiofrequency quadrupole has the gap of four direction, wherein the horizontal direction gap is respectively the intake of aerocolloidal intake and ionization laser beam, and the gap of vertical direction is respectively the secondary intake of laser beam and the outlet of secondary scattering laser bundle calibrated of laser diameter measurement system.
4, single-particle aerosol online ionization source according to claim 1 and 2 is characterized in that: described ionization laser is connected with the secondary photomultiplier of calibrating of laser diameter measurement system, by its pulse-triggered that provides.
5, single-particle aerosol online ionization source according to claim 1 and 2, it is characterized in that: every bar of described low pressure radiofrequency quadrupole is made up of more piece bar section, be provided with clearance for insulation between each pole section, the clearance for insulation between the adjacent two pole sections is less than 0.3mm.
6, single-particle aerosol online ionization source according to claim 1 and 2 is characterized in that: described low pressure radiofrequency quadrupole is provided with the axial DC electric field; The DC potential of the low pressure radiofrequency quadrupole position that described laser beam vertical incidence point is corresponding is set to 0V, increases respectively and reduces toward the opposite two ends DC potential of low pressure radiofrequency quadrupole direction, forms the axial DC electric field; Each pole section of described low pressure radiofrequency quadrupole applies identical radio-frequency voltage, and described radio-frequency voltage is in the same place by resistance and capacitive coupling with direct voltage.
7, single-particle aerosol online ionization source according to claim 1 and 2 is characterized in that: described time of flight mass analyzer is vertical introduction-type time of flight mass analyzer or cascade mass spectrometry device.
8, a kind of method of utilizing each described single-particle aerosol online ionization source of claim 1～7 to realize, it is characterized in that: after utilizing aerodynamics to calibrate to the individual particle aerosol, before it enters the accelerating region of time of flight mass analyzer, utilize ionization laser that it is ionized into plasma, the negative ions that is produced utilizes the low pressure radiofrequency quadrupole to be focused into the very little ion beam of phase space and sends in the time of flight mass analyzer again.
9, the method for utilizing single-particle aerosol online ionization source to realize according to claim 8, it is characterized in that: utilize the axial DC electric field of low pressure radiofrequency quadrupole setting that the negative ions that produces after the ionization separately and is respectively moved to the two ends of low pressure radiofrequency quadrupole, detected by the time of flight mass analyzer of opposed polarity respectively then.
10, a kind of method of utilizing the described single-particle aerosol online ionization source of claim 4 to realize, it is characterized in that: after utilizing aerodynamics to calibrate to the individual particle aerosol, before it enters the accelerating region of time of flight mass analyzer, utilize ionization laser that it is ionized into plasma, the negative ions that is produced utilizes the low pressure radiofrequency quadrupole to be focused into the very little ion beam of phase space and sends in the time of flight mass analyzer again; The pulse that utilizes the secondary photomultiplier of aerodynamics measurement diameter system to produce triggers the ionization laser immediately and produces the ionization laser pulse individual particle aerosol is ionized into plasma.
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| CN104596900A (en) * | 2015-01-05 | 2015-05-06 | 暨南大学 | Method and system for automatically realizing grain size correction of atmosphere particles |
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| FI20080182A0 (en) * | 2008-03-04 | 2008-03-04 | Navaro 245 Oy | Measurement method and apparatus |
| CN101581698B (en) * | 2009-06-23 | 2012-08-22 | 中国科学院安徽光学精密机械研究所 | Aerosol field ionization electric charge source device |
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| EP3389080A1 (en) * | 2017-04-10 | 2018-10-17 | Tofwerk AG | Ion source and method for generating elemental ions from aerosol particles |
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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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Effective date of registration: 20120316 Address after: 215311, 3F, building 2, Pudong Software Park, Kunshan, Xueyuan Road, Kunshan, Jiangsu, Suzhou 828, China Co-patentee after: Guangzhou Hexin Analytical Instrument Co., Ltd. Patentee after: Kunshan Hexin Zhipu Technology Co.,Ltd. Address before: Science City Moon road 510530 Guangzhou high tech Industrial Development Zone, No. 80 Guangzhou science and technology innovation base in F District 3 building 301, 302 Patentee before: Guangzhou Hexin Analytical Instrument Co., Ltd. |
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Address after: 215311, 3F, building 2, Pudong Software Park, Kunshan, Xueyuan Road, Kunshan, Jiangsu, Suzhou 828, China Patentee after: Kunshan Hexin Zhipu Technology Co.,Ltd. Patentee after: Guangzhou Hexin Instruments Co., Ltd. Address before: 215311, 3F, building 2, Pudong Software Park, Kunshan, Xueyuan Road, Kunshan, Jiangsu, Suzhou 828, China Patentee before: Kunshan Hexin Zhipu Technology Co.,Ltd. Patentee before: Guangzhou Hexin Analytical Instrument Co., Ltd. |