CN102176403B - Ionic focusing method for high-field asymmetric waveform ion mobility spectrometer with flat plate structure - Google Patents
Ionic focusing method for high-field asymmetric waveform ion mobility spectrometer with flat plate structure Download PDFInfo
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Abstract
The invention provides an ionic focusing method for a high-field asymmetric waveform ion mobility spectrometer with a flat plate structure, and belongs to the field of biochemical substance field analysis and detection. In the mobility spectrometer, an upper substrate and a lower substrate form a gas path in a mobility area; an upper mobility area electrode and a lower mobility area electrode are arranged on the upper substrate and the lower substrate respectively; high-field asymmetric waveform radio frequency voltage and direct current scanning compensation voltage are applied to the upper mobility area electrode; and direct current voltage is applied to the lower mobility area electrode. When ions are sent into the mobility area by carrier gas, different ions are separated from one another under the action of the asymmetric waveform radio frequency voltage; the irons is subjected to ion selection under the action of the direct current scanning compensation voltage; and the irons are focused under the action of the direct current voltage of the lower mobility area electrode and are detected finally by a detection unit at the tail end of the gas path. By the method, different ions are separated and focused, so that loss of ions in the mobility area is reduced, the signal strength is increased, and the sensitivity of the mobility spectrometer is improved.
Description
Technical field
The present invention relates to biochemical substances is carried out Fast Measurement, belong to the field assay detection field, be specially a kind of ion focusing method of slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer.
Background technology
High-Field asymmetric waveform ion mobility spectrometry (FAIMS, High-field Asymmetric Waveform Ion MobilitySpectrometry) is a kind of biochemical substances detection technique that the nineties progressively grows up last century.It mainly utilizes the mobility of ion under the high electric field different characteristics to separate the different types of biochemical substances of detection with the variation of electric field strength.Its basic principle is as follows: under low current field condition, the mobility coefficients of ion and electric field strength are irrelevant; (after the E/N＞40Td), the mobility coefficients K of ion will change with electric field strength in a kind of nonlinear mode to certain value when electric field strength is high.Mobility and the relation of electric field strength of ion under High-Field is available as shown in the formula subrepresentation:
K=K
0[1+ α
1(E/N)
2+ α
2(E/N)
4+ ... ], wherein K is the mobility of ion under high electric field, K
0Be the mobility of ion under low electric field, E is electric field strength, and N is gas density, α
1, α
2Be the ionic mobility decomposition coefficient.Make α (E)=[α
1(E/N)
2+ α
2(E/N)
4+ ... ], K=K then
0[1+ α (E)].When α (E)＞0, K＞K
0, then K increases with E; When α (E)＜0, K＜K
0, then K reduces along with the increase of E; When α (E) ≈ 0, K ≈ K
0As seen from the above analysis, under the effect of high electric field, the mobility of ion can present different separately nonlinear trends, this just so that the ion that ionic mobility is identical or close under low electric field strength condition can be under high electric field strength condition separated opening.
At present, High-Field asymmetric waveform ion mobility spectrometry mainly contains plate and two kinds of structures of cylinder type, than cylinder type, plate High-Field Asymmetric Waveform Ion Mobility Spectrometer be easier to micro electro mechanical system (MEMS) technology (MEMS,
Micro-Electro-Mechanical System) carries out process, be convenient to microminiaturization, therefore have larger advantage aspect the portable biochemical detecting instrument device.
University and Sionex company are found in the New Mexico that mainly contains that plate High-Field Asymmetric Waveform Ion Mobility Spectrometer is furtherd investigate, its main core chip architecture adopts MEMS process technology design processing, and ion source adopts vacuum UV lamp ion source or 63Ni ion source.This plate High-Field Asymmetric Waveform Ion Mobility Spectrometer has two kinds of versions, and as shown in Figure 1 carrier gas is perpendicular to ion source and the mode that enters facing to ion source shown in Figure 2 respectively.These two kinds of frame modes all exist deficiency: owing to adopt plate armature, and only be added with asymmetric waveform radio-frequency voltage and direct current scan compensation voltage at upper migration area electrode, namely only have and be added with voltage on the upper migration area electrode and lower migration area electrode does not have voltage, ion after the ion source ionization spreads in the whole migration area, under the driving of asymmetric electric field, produce up-down vibration, having considerable ion meeting impinge upon because Oscillation Amplitude is excessive to produce on the pole plate buries in oblivion, the loss of ion in the migration area is very big, greatly affected the intensity of detection signal, so that detect the difficult that becomes.
Summary of the invention
The objective of the invention is to overcome the deficiency of existing plate High-Field asymmetric waveform ion mobility spectrometry, provide a kind of so that the sample ions in the slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer is strapped in the center, migration area, reduce the ion focusing method that causes losses of ions because of bump migration area pole plate and diffusion.
Technical scheme of the present invention is as follows:
A kind of ion focusing method of slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer, described slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer comprises ion source, migration area and detecting unit; Described migration area comprises upper substrate and the subtegulum of parallel placement, migration area electrode and lower migration area electrode are being set respectively on upper substrate and the subtegulum, be added with asymmetric waveform radio-frequency voltage and direct current scan compensation voltage at upper migration area electrode, ion in the migration area is carried out isolation and selection, the method is characterized in that: add a direct voltage at lower migration area electrode, ion is assembled to the center, migration area when separating, sample ions is realized focusing on.The field strength range that described direct voltage produces between upper migration area electrode and lower migration area electrode is less than 5000V/cm greater than zero.
The present invention compared with prior art, have the following advantages and the high-lighting effect: 1. the present invention adopts and adds direct voltage at lower migration area electrode, ion can be subject to the repulsive force of the electrode identical with ion polarity between migration area electrode and the lower migration area electrode on entering, thereby in the middle of gas channels, assemble, reduce the losses of ions of bringing because of factors such as diffusion, carrier gas disturbances; 2. the present invention is totally based on slab construction, and the structure of separate mesh electrode, migration area and ion detection unit all is convenient to adopt the MEMS process technology to process, and is easy to integratedly, and it is microminiaturized to be convenient to the FAIMS system.
Description of drawings:
Fig. 1 is the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer schematic diagram that carrier gas enters perpendicular to ion source.
Fig. 2 is that carrier gas faces toward the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer schematic diagram that ion source enters.
Fig. 3 is the apparatus structure schematic diagram of the ion focusing method of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer provided by the invention.
Fig. 4 is the focusing principle figure of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer.
Fig. 5 is the added direct voltage schematic diagram of lower migration area electrode.
Fig. 6 is asymmetric waveform radio-frequency voltage schematic diagram.
Fig. 7 is direct current scan compensation voltage schematic diagram.
Fig. 8 is that lower migration area electrode does not add and adds the signal contrast figure that gathers behind the direct voltage, the contrasts of focus voltages (the voltage max 240V flow velocity 0.6L/min different) wherein: (a) focus voltage 0.00V, (b) focus voltage 2.51V (c), focus voltage 4.94V, (d) focus voltage 7.80V, (e) focus voltage 11.90V, (f) focus voltage 15.30V.
Among the figure: the 1-carrier gas; The 2-ion source; The 3-migration area; The upper substrate of 4-; The 5-subtegulum; The upper migration area of 6-electrode; Migration area electrode under the 7-; The 8-detecting unit; 9-direct current scan compensation voltage; 10-asymmetric waveform radio-frequency voltage; The 11-direct voltage.
Embodiment
Below in conjunction with accompanying drawing the concrete structure of ion focusing type slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer provided by the invention and the action principle of ion focusing method are described further.
Fig. 3 is the apparatus structure schematic diagram of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer ion focusing method provided by the invention.The asymmetric ionic migration spectrometer of described slab construction High-Field comprises ion source 2, migration area 3 and detecting unit 8.Wherein migration area 3 comprises substrate 4, subtegulum 5, upper migration area electrode 6, lower migration area electrode 7; Upper substrate 4 and subtegulum 5 parallel placements, the gas channels of formation migration area 3, upper migration area electrode 6 and lower migration area electrode 7 lay respectively on substrate 4 and the subtegulum 5; The end of 3 rear portion, gas channels is the detecting unit 8 that can detect faint ion current in the migration area; Upper migration area electrode 6 is added with asymmetric waveform radio-frequency voltage 10 and direct current scan compensation voltage 9, and 7 at lower migration area electrode is added with direct voltage 11.
The action principle of slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer ion focusing method shown in the present is as follows:
When ion carried by carrier gas enter migration area 3 interior after, if upper migration area electrode 6 all is added with identical direct voltage 11 (as shown in Figure 4) with lower migration area electrode 7, its value is CV0 (direct voltage 11 is less than 5000V/cm greater than zero in the field strength range of upper migration area electrode 6 and 7 generations of lower migration area electrode) (as shown in Figure 5).Under the effect of CV0 on upper migration area electrode 6 and the lower migration area electrode 7, depart from the repulsive force that ion between the migration area center lines of electrodes can be subject to the electrode identical with ion polarity, thereby in the middle of the migration area, assemble, the losses of ions that minimizing brings because of factors such as diffusion, carrier gas disturbances, realize and the similar ion focusing function in cylinder type migration area, the signal that detects is enhanced.The basic principle of ion focusing that Here it is.
In the design of reality, upper migration area electrode 6 is added with direct current scan compensation voltage 9 and asymmetric waveform radio-frequency voltage 10, is added with direct voltage 11 (as shown in Figure 3) at lower migration area electrode 7.Wherein asymmetric waveform radio-frequency voltage 10 is the High-Field asymmetric waveform (as shown in Figure 6) that equates of area up and down; Direct current scan compensation voltage 9 scans (as shown in Figure 7) with specific scanning frequency and scanning step between certain voltage range CV1～CV2; The magnitude of voltage of direct voltage 11 is CV0 (as shown in Figure 5).This moment, system as shown in Figure 3 can see so so: asymmetric waveform radio-frequency voltage, direct current scan compensation voltage (sweep limits CV1-CV0～CV2-CV0) mutually superpose with three voltages of direct voltage CV0 are arranged on the upper migration area electrode 6; Only has direct voltage CV0 on the lower migration area electrode 7.Go up like this direct voltage CV0 that migration area electrode 6 and lower migration area electrode 7 have simultaneously so that such migration area design has the focusing to ion.And for ion not of the same race, under the effect of asymmetric waveform radio-frequency voltage 10, make progress migration area electrode 6 or lower migration area electrode 7 of certain ion produces a clean displacement and (depends on the kinetic characteristic of ion under high field action, the clean displacement of different ions is different), if there is not the effect of direct current scan compensation voltage 9, ion will produce deflection and strike on migration area electrode 6 or the lower migration area electrode 7 and be neutralized.When if direct current scan compensation voltage 9 is a certain desired value, the clean displacement energy that ion is produced under 10 effects of asymmetric waveform radio-frequency voltage accesses compensation, and then ion can pass through the migration area.The ion of so corresponding certain direct current scan compensation voltage can pass through the migration area, and other ion then strikes on the metal electrode and is neutralized.Therefore the corresponding different types of ion of the direct current scan compensation voltages of different sizes just can determine the kind of sample according to the value of direct current scan compensation voltage.
The ion that filters after selecting through migration area 3 continues to move right under the effect of carrier gas, enters detecting unit 8, and ion signal is converted into current signal, measures the value of current signal.By recording the related data of the electric current that the corresponding detecting unit of each direct current scan compensation voltage detects, and draw in real time both corresponding relation curves by software.Noise and image through microprocessor are processed, and determine direct current scan compensation magnitude of voltage corresponding to current signal maximum in each waveform.High-Field asymmetric waveform radio-frequency voltage and the relevant parameter (voltage max, frequency, duty ratio, waveform etc.) of direct current scan compensation voltage, size (length, width, spacing), air pressure, flow velocity, temperature and the kind (High Purity Nitrogen, the air that purified, carbon dioxide etc.) of pure carrier gas and the data in direct current scan compensation magnitude of voltage and the database of migration area of this moment are compared, thereby determine entrained sample material kind in the sample carrier gas.
Embodiment 1:
Utilize ion focusing type High-Field Asymmetric Waveform Ion Mobility Spectrometer that 2 pentanone is detected.Carrier gas 1 is carried 2 pentanone and is entered migration area 3.According to the ionization property of ion source 2, carrier gas 1 is 99.999% High Purity Nitrogen, and flow velocity is defined as 0.6L/min.Lower migration area electrode 7 is added with direct voltage 11, loading frequency 2MHz on the upper migration area electrode 6, the asymmetric waveform radio-frequency voltage 10 of duty ratio 30%.The focusing of ion of the same race occurs in the 2 pentanone ion of ionization under direct voltage 11 effects, signal strength signal intensity increases, and radio-frequency voltage so that the 2 pentanone ion separate with foreign ion in the carrier gas in the migration area, obtain at last the real-time curve of 2 pentanone bucking voltage and current signal corresponding relation by the scanning of control direct current scan compensation voltage 9 voltages, determine the bucking voltage that 2 pentanone is corresponding, determine the substance classes of 2 pentanone by comparing.From the experimental results (as shown in Figure 8), when asymmetric waveform radio-frequency voltage amplitude is 240V, behind the loading focus voltage, the 2 pentanone ion signal strength increase that detects, detection sensitivity improves greatly.
Embodiment 2:
Adopt MEMS technique that ion focusing type High-Field Asymmetric Waveform Ion Mobility Spectrometer is carried out the system integration.Ion source 2 adopts the corona discharge ion source of cylinder type, and detecting unit 8 adopts the microarray formula Faraday cup of column structure.Ion source 2 and detecting unit 8 all can form by ICP technique etching conductive silicon chip.Upper substrate 4 and subtegulum 5 adopt Pyrex.On-chip upper migration area electrode 6, lower migration area electrode 7 by sputtered with Ti on Pyrex/Pt/Au metal form (thickness T i:
Pt:
Au:
).Substrate assembles by bonding technology.Adopt the discharge mode of negative corona, acetic acid sample entrained in the carrier gas is ionized.According to the operating characteristic of cylinder type corona discharge ion source, the gas flow rate of carrier gas is adjusted to 100ml/min.Under certain High-Field asymmetric waveform radio-frequency voltage parameter, select suitable lower migration electrode focus voltage that signal is strengthened, by scanning direct current scan compensation voltage, obtain corresponding signal curve, by the comparison of acetic acid direct current scan compensation voltage being determined the substance classes of acetic acid.
Claims (1)
1. the ion focusing method of a slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer, described slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer comprises ion source (2), migration area (3) and detecting unit (8); Described migration area (3) comprises upper substrate (4) and the subtegulum (5) of parallel placement, upper migration area electrode (6) and lower migration area electrode (7) are set respectively on upper substrate (4) and subtegulum (5), be added with asymmetric waveform radio-frequency voltage (10) and direct current scan compensation voltage (9) at upper migration area electrode (6), ion in migration area (3) is carried out isolation and selection, the method is characterized in that: add a direct voltage (11) at lower migration area electrode (7), make ion (3) center gathering to the migration area when separating, sample ions is realized focusing on; The field strength range that described direct voltage produces between upper migration area electrode (6) and lower migration area electrode (7) is less than 5000V/cm greater than zero.
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| CN102683151B (en) * | 2012-05-15 | 2015-01-28 | 中国科学院合肥物质科学研究院 | Chemical ionization mass spectrometer for selectively controlling reaction ions |
| CN102723254B (en) * | 2012-06-20 | 2015-07-22 | 清华大学 | Focusing device and method of flat high-field asymmetric waveform ion mobility spectrometer |
| DE112013003813T5 (en) * | 2012-07-31 | 2015-05-13 | Leco Corporation | Ion mobility spectrometer with high throughput |
| CN102945786B (en) * | 2012-11-09 | 2015-06-17 | 清华大学 | Flat-plate type high-field asymmetric waveform ion mobility spectrometer with noise reduction function |
| CN104538274B (en) * | 2014-12-31 | 2017-02-01 | 清华大学 | Separation voltage applying method for high-field asymmetric waveform ion mobility spectrometer |
| CN108088888A (en) * | 2016-11-23 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of real-time, quick, on-line monitoring sample differential mobility spectral method |
| CN108091538B (en) * | 2016-11-23 | 2020-01-14 | 中国科学院大连化学物理研究所 | Integrated vacuum ultraviolet lamp ionization source differential ion mobility spectrometer |
| CN113035686B (en) * | 2021-03-03 | 2023-06-16 | 桂林电子科技大学 | Ion source, FAIMS device and method for improving resolution and sensitivity of FAIMS device |
| CN116230487B (en) * | 2022-11-18 | 2024-03-12 | 中船重工安谱（湖北）仪器有限公司 | Ion migration tube and ion migration spectrometer |
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| CN101853771A (en) * | 2009-04-03 | 2010-10-06 | 中国科学院上海应用物理研究所 | Ionic migration spectrometer with inspiratory condenser structure |
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| CN101853771A (en) * | 2009-04-03 | 2010-10-06 | 中国科学院上海应用物理研究所 | Ionic migration spectrometer with inspiratory condenser structure |
| CN101571508A (en) * | 2009-06-16 | 2009-11-04 | 清华大学 | High-field asymmetric waveform ion mobility spectrometer with multi-layer plate structure |
| CN101881752A (en) * | 2010-06-21 | 2010-11-10 | 中国科学院合肥物质科学研究院 | Micro two-dimensional ionic migration spectrometer |
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