CN104483378B - Reverse expansion HADAMARD transform ion mobility spectrometer - Google Patents
Reverse expansion HADAMARD transform ion mobility spectrometer Download PDFInfo
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Abstract
The invention relates to a reverse expansion HADAMARD transform ion mobility spectrometer. The reverse expansion HADAMARD transform ion mobility spectrometer comprises an ionization region, a curtain gas region, a reaction region, a reverse expansion HADAMARD transform ion gate control module, a migration area, a charge detection region and an inverted HADAMARD transform signal processing module, wherein the ionization region is provided with an ionization source, the curtain gas region is used for preventing a sample from entering the ionization region, an ion gate is arranged between the reaction region and the migration area, the ion gate is connected with the reverse expansion HADAMARD transform ion gate control module, the reverse expansion HADAMARD transform ion gate control module is used for controlling a high-speed switch of the ion gate periodically to achieve multiplexing of ion flows, the charge detection region is connected with the inverted HADAMARD transform signal processing module, and the signal processing module is mainly used for carrying out acquisition of a multipath superposed spectrum signal, A/D conversion, inverted HADAMARD transform treatment and display of restoring spectrums.
Description
Technical field
The present invention relates to a kind of ionic migration spectrometer, convert ion mobility spectrometry particularly to a kind of inverse expansion HADAMARD
Instrument.
Background technology
In recent years, either external or domestic, various terrorist activities aggravate continuous, in order to more effectively ensure citizen
Property and life security, people increase the Innovation Input of the rapid detection apparatus to explosive, chemical warfare agent, drugs etc., ion
Mobility spectrometer is fought agent testing equipment as a kind of quick trace chemistry, also in development like a raging fire.
Ion mobility spectrometry compared to other anti-riot anti-terrorism survey meters, mainly can enter to some trace toxic gas by its advantage
Row quick detection, has different migration velocities under Weak Uniform Electromagnetic field condition using different ions and distinguishes measured object, have
The features such as detection speed is fast, sensitivity is high.Ion mobility spectrometry detection device occurs in the sixties in 20th century earliest, and early stage mainly should
Used in military aspect, it is substantially carried out the detection of trace chemistry war agent etc., currently, cruelly fear being becoming increasingly rampant of activity with various,
Also ionic migration spectrometer has been put in a large number, to assist security staff in the safety check department in the places such as airport, railway station, customs port
Complete the quick detection of trace explosive, drugs and chemical warfare agent etc..
The working mechanism of corona discharge ionization mobility spectrometer：In region of discharge, first by high-pressure modular to high-purity N2Or air
Electric discharge, reaction of formation thing ion, following reaction thing ion enters into reaction zone；In reaction zone, reactant ion with by carrier gas
There is a series of ion-molecule reaction, thus neutral sample molecule ionizing is formed in the sample molecule entering reaction zone
Product ion.The ion gate of coupled reaction area and migration area is periodically to open and close, when ion gate is opened, product ion
Enter into migration area, migration area has uniform and stable weak electric field, it makes it carry out lateral drift product ion effect, in drift
Collide with oncoming migration gas neutral molecule during shifting, because different product ions has different matter
Amount, electric charge and collision cross-section structure, therefore it forms different migration rates in the presence of migration and collision, and this is also just certainly
Determine the time difference that different product ions reach detector end, finally achieve efficiently separating of different ions.
With the continuous lifting of detection performance requirement, high-resolution and high s/n ratio have become as measurement ion mobility spectrometry inspection
Survey the important technology index of performance.In order to improve the detection performance of ion mobility spectrometry, forefathers have done substantial amounts of research, 21 century
Just, people attempt HADAMARD multiplexing technique is incorporated in ion mobility spectrometry, successfully construct HADAMARD convert from
Sub- mobility spectrometer, the signal utilization rate that improve ion mobility spectrometry to a certain extent is dutycycle, and then improves ion and move
Move the signal to noise ratio of spectrum.Chinese patent CN200910051783.5 discloses a kind of ion migration of use HADAMARD alternative approach
Spectrometer, its ionization source adopts63Ni radioactive ionization gauge source, controls ion gate using conventional pseudo-random sequence, improves ion
, there is more ghost peak using the HADAMARD conversion ion mobility spectrometry that the method generates in flux and signal to noise ratio, and the method life
The ion mobility spectrometry becoming can not effectively improve the resolution of ion mobility spectrometry.
Therefore, under conditions of not changed ion mobility spectrometry hardware configuration on a large scale, signal to noise ratio can be improved and energy
The resolution effectively improving ion mobility spectrometry then becomes the inexorable trend of ionic migration spectrometer research and development.Associated at present
Document report less.
Content of the invention
The technology of the present invention solve problem：Low for traditional signal averaging ion migration spectral resolution and signal to noise ratio, often
The HADAMARD conversion ion mobility spectrometry of rule is only capable of raising signal to noise ratio and can not put forward high-resolution problem, proposes a kind of inverse expansion
HADAMARD converts ionic migration spectrometer, and this invention improves signal to noise ratio and the resolution of ion mobility spectrometry simultaneously, improve from
The comprehensive detection performance of sub- mobility spectrometer.
The technology of the present invention solution：A kind of inverse expansion HADAMARD converts ionic migration spectrometer, it include ionized region,
Lian Qi area, reaction zone, inverse expansion HADAMARD conversion ion gating module, migration area, charge detection area, inverse HADAMARD become
Change signal processing module, in described ionized region, have ionization source, between described ionized region and described reaction zone, be provided with Lian Qi area, institute
The curtain gas being passed through in Shu Lianqi area can intercept sample gas and enter described ionized region, the interval setting with described migration of described reaction zone
There is ion gate, be characterised by, described ion gate is connected with described inverse expansion HADAMARD conversion ion gating module, by described
Ion gating module completes the High-speed on-off control of ion gate, and described charge detection area is converted at signal with described inverse HADAMARD
Reason module is connected, and described signal processing module mainly completes the collection of stack spectral, A/D conversion, inverse HADAMARD conversion process, goes back
The display of former spectrum.
In one embodiment of the invention, described ionized region adopts negative high voltage to be directed to board-like discharge mode, and ionization source is
One negative high voltage module, the negative high voltage of its output is -10000V.
In one embodiment of the invention, described reaction zone and migration area pass through the isolation of BN type ion gate, described ion
Door is connected with described inverse expansion HADAMARD gating module；In one embodiment of the invention, described inverse expansion
HADAMARD conversion ion gating module is by pseudo-random sequence generator, extended coding device, phase-reversal coding device and boost module group
Become, generate 255 pseudo-random binary sequences by 8 rank pseudo-random sequence generators first, wherein contain 128 1,127 0；
The pseudo-random sequence of described 255 is converted into the extension pseudo random sequence code of 255*4 (1020) position by described extended coding device；Institute
State phase-reversal coding device and described extension pseudo noise code is converted into inverse expansion pseudo random sequence code, thus obtain ion gate numeral
Sequence；Described boost module, this Serial No. (Transistor-Transistor Logic level) is converted into the ion gate voltage signal of 0～220V, this signal
It is directly connected to described ion gate two ends.The modulation resolution (pulsewidth) of described ion gate is 200 μ s.
In one embodiment of the invention, described migration area is uniformly composed in series by the valued resistor such as a group, is ion
Motion provides a uniform weak electric field, and migration area electric field obtains the Weak Uniform Electromagnetic field of 400V/cm by partial pressure mode.
In one embodiment of the invention, described charge detection area is by charge detection plate and Signal Pretreatment unit structure
Become, ion signal is mainly converted into current signal by described charge detection plate, and described Signal Pretreatment unit is to utilize amplifier
The current signal characterizing ionic strength is amplified and converted to voltage signal.
Further, described inverse HADAMARD converts the collection that signal processing module completes HADAMARD conversion superposition modal data
Inverse HADAMARD conversion process with high-speed a/d conversion and migration spectrum.Data acquisition is controlled by periodically pulsing synchronous letter
Number, this synchronizing signal is in the same size with the inverse expansion pseudo-random sequence cycle, by inverse expansion HADAMARD ion gating module
Output control, the sample frequency of described signal processing module is 20KHz, and data acquisition adopts continuous acquisition pattern, and subchannel connects
Receive the data collecting.
In one embodiment of the invention, described ion mobility spectrometry is in room temperature, operated at atmospheric pressure, need not adjust ion
The temperature and humidity of migration area.
Present invention advantage compared with prior art is：A kind of inverse expansion HADAMARD of the present invention converts ion migration
Spectrometer, can not only effectively improve ionic flux, improve signal to noise ratio, and can make full use of interionic diffusion repulsive interaction compression
The halfwidth of quasi-molecular ions, thus be effectively improved the resolution of ion mobility spectrometry.The present invention does not need to existing ion migration
Spectrum does larger hardware modifications；In detection aspect of performance, with respect to traditional signal averaging ion mobility spectrometry, apparatus of the present invention will
Detection signal-to-noise ratio improves about 6.5 times, resolution is improve about 33% about, and conventional H ADAMARD alternative approach can not change
The resolution of kind ion mobility spectrometry, this shows that the present invention is better than classical signal averaging method and routine in comprehensive detection aspect of performance
HADAMARD converter technique ion mobility spectrometry.In addition the technology of the present invention achievement can be additionally used in other similar analytical technologies, application
Have a extensive future.
Brief description
Fig. 1 is that a kind of inverse expansion HADAMARD of the present invention converts ion mobility spectrometer configuration；
Fig. 2 is that inverse expansion HADAMARD of the present invention converts ion gating module control schematic diagram；
Fig. 3 is signal averaging ion mobility spectrometry testing result；
Fig. 4 is conventional H ADAMARD conversion ion mobility spectrometry and inverse expansion HADAMARD conversion ion mobility spectrometry detection property
Energy comparison diagram).
Wherein, 1- ionized region, 2- Lian Qi area, 3- reaction zone, 4- inverse expansion HADAMARD converts ion gating module, 5-
Migration area, 6- charge detection area, 7- converts signal processing module, 8- negative high voltage module against HADAMARD, and 9- first gas export,
10- curtain gas, 11- second gas export, 12- carrier gas inlet, 13- ion gate, and 14- uniformly migrates electric field, and 15- migrates gas entrance,
16- faraday's plate, 17- Signal Pretreatment unit, 18- longest linear feedback shift register, 19- extended coding device, 20- is reverse
Encoder, 21- boost module.
Specific embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.
As shown in figure 1, a kind of inverse expansion HADAMARD converts ionic migration spectrometer, it include ionized region 1, Lian Qi area 2,
Reaction zone 3, inverse expansion HADAMARD conversion ion gating module 4, migration area 5, charge detection area 6, inverse HADAMARD conversion
Signal processing module 7.Described ionized region adopts negative corona discharge pattern, and the negative high voltage module 8 using 10000V exports to high pressure
Spray point, by for board-like discharge mode, the gas ionization being passed through, reaction of formation thing ion being provided with first in ionized region
Gas outlet 9；Described Lian Qi area stops sample gas from entering ionized region using the curtain gas 10 being blown into；Described reaction zone is provided with
Two gas outlets 11 and carrier gas inlet 12；It is provided with BN type ion gate 13, described ion gate between described reaction zone and migration area
Convert ion gating module 4 with described inverse expansion HADAMARD to be connected, to realize the High-speed on-off control of ion gate；Described move
Alternately placement forms by a series of beckets and polytetrafluoroethylene ring to move area, is connected each becket by even resistance and is formed
Uniformly migration electric field 14, described migration area end has migration gas entrance 15 to be used for neutral molecule blow-back, stops its arrival
Faraday's plate；Described charge detection area detects charge signal by faraday's plate 16, and signal is accessed Signal Pretreatment unit
17, complete signal and be amplified and converted to 0～10V voltage signal；Described inverse HADAMARD conversion signal processing module and described electricity
Lotus detecting area is connected, and realizes the collection of stack spectral, A/D conversion, inverse HADAMARD conversion process, the display of reduction spectrum.
In place of inverse expansion HADAMARD conversion gating module is the main innovation of the present invention.Early in 2006, external
Person has begun to seek multiplexing ion mobility spectrometry (IMS), and HADAMARD multiplexing technique is thus introduced into IMS, relatively
For signal averaging, the HADAMARD using multiplexing technique converts the noise that IMS considerably enhances analytical tool
Than, but shortcoming is cannot to improve the resolution of ion mobility spectrometry simultaneously, and there is ghost peak phenomenon in exchanging cards with personal and family details when becoming sworn brothers in its inversion.For this reason,
The present invention done two aspects process, be on the one hand that pseudo random sequence code is isolated, that is, be extended process, formed extension puppet with
Machine sequence code (is realized by adding extended code after every pseudo random sequence code), is on the other hand by the pseudorandom sequence of extension
Row are made phase-reversal coding and are processed, and this process is primarily to improve the resolution of ion mobility spectrometry.
The inverse expansion HADAMARD conversion ion gating module complete structure of the present invention is as shown in Figure 2.In embodiment, first
First pass through FPGA fabric 8 rank longest linear feedback shift register 18, its linear feedback logical expression is x8=x4+x3+x2+
1, the pseudo random sequence length of generation is 255 (128 1,127 0), and dutycycle is about 50%, by extended coding device 19
This pseudo-random sequence is converted to the pseudo-random sequence of extension, adds 30 after every pseudo random sequence code, the duty of this sequence
Ratio then drops to 12.5% about, then by phase-reversal coding device 20 by this pseudo-random sequence extending be transformed to inverse expansion pseudo- with
Machine sequence, dutycycle rises to 87.5% about again, and finally inverse expansion pseudo-random sequence is converted into out by boosted module 21
Gate voltage be 0V, close gate voltage be 180V ion gate pulse signals, be finally driven by ion gate switch (with described from
Cervical orifice of uterus 13 two ends are connected).
The pulsewidth (modulation resolution) of intermediate ion door 13 of the present invention is chosen as 200 μ s.
In the present invention, the ion current that faraday's plate detects is put by charge detection area using Signal Pretreatment unit
Big and current/voltage conversion process, obtains the voltage signal of 0～10V；Inverse HADAMARD conversion signal processing module first passes through
The A/D ALT-CH alternate channel that it carries completes to be superimposed the collection of modal data, conversion, storage, then carries out against HADAMARD conversion process,
And reduction spectrum is shown.Finally to signal averaging ion mobility spectrometry, conventional H ADAMARD conversion ion mobility spectrometry and anti-
The testing result converting ion mobility spectrometry to extension HADAMARD has carried out relative analyses, spectrogram such as Fig. 3 institute of signal averaging
Show, conventional HADAMARD conversion ion mobility spectrometry and inverse expansion HADAMARD conversion ion mobility spectrometry are as shown in Figure 4.Experiment
Result shows, taking the pseudo-random sequence of 255 as a example, conventional H ADAMARD converts ion mobility spectrometry, and the raising of its signal to noise ratio is about
1.58 times of signal averaging ion mobility spectrometry, but its resolution is slightly less than signal averaging ion mobility spectrometry；This
Compared to signal averaging, its signal to noise ratio is about signal averaging to bright inverse expansion HADAMARD conversion ion mobility spectrometry
6.5 times, resolution ratio signal averaging improves 33% about, and contrast can obtain, inverse expansion HADAMARD proposed by the present invention
Alternative approach ion mobility spectrometry combination property is substantially better than the comprehensive detection performance that conventional H ADAMARD converts ion mobility spectrometry.
There is provided above example to be used for the purpose of the description purpose of the present invention, and be not intended to limit the scope of the present invention.This
The scope of invention is defined by the following claims.Various equivalents made without departing from spirit and principles of the present invention and repairing
Change, all should cover within the scope of the present invention.
Claims (8)
1. a kind of inverse expansion HADAMARD converts ionic migration spectrometer, and it includes ionized region (1), Lian Qi area (2), reaction zone
(3), inverse expansion HADAMARD conversion ion gating module (4), migration area (5), charge detection area (6), inverse HADAMARD become
Change signal processing module (7)；There is ionization source in described ionized region, between described ionized region and described reaction zone, be provided with curtain gas
Area, described Lian Qi area can intercept sample gas and enter described ionized region, and described reaction zone and described migration interval are provided with a BN
Type ion gate (13) it is characterised in that：Described ion gate is connected with described inverse expansion HADAMARD conversion ion gating module,
Described ion gating module is used for periodically controlling described ion door trip, completes the multiplexing of current ion signal, described electricity
Lotus detecting area converts signal processing module with described inverse HADAMARD and is connected, and described signal processing module mainly completes stack spectral
Inverse HADAMARD conversion process, obtains reduction spectrum；
Described inverse expansion HADAMARD conversion ion gating module (4) is by pseudo-random sequence generator (18), extended coding device
(19), phase-reversal coding device (20) and boost module (21) composition, construct a n rank linear feedback by pseudo-random sequence generator first
Shift register, obtains 2n- 1 pseudo-random sequence；Using extended coding device, this pseudo-random sequence is converted into extending pseudorandom
Sequence code；Recycle phase-reversal coding device that this extension pseudo noise code is converted into inverse expansion pseudo random sequence code, resulting in
Periodically ion gate Serial No.；Using boost module, ion gate Serial No. is converted into being suitable for ion gate control
Voltage signal is simultaneously linked into described ion gate two ends, to control ion door trip.
2. a kind of inverse expansion HADAMARD conversion ionic migration spectrometer according to claim 1 it is characterised in that：Described
Ionized region (1) adopts negative corona discharge pattern, and ionization source is the height being exported 8700V～14000V by a negative high voltage module (8)
It is pressed onto corona discharge needle, by obtaining reactant ion for plate discharge mode, ionization source also can adopt light ionization source, radioactivity
Ionization source, electron spray ionisation source.
3. a kind of inverse expansion HADAMARD conversion ionic migration spectrometer according to claim 2 it is characterised in that：Described
Radioactive ionization gauge source is63Ni.
4. a kind of inverse expansion HADAMARD conversion ionic migration spectrometer according to claim 1 it is characterised in that：Described
Ionized region (1) and described reaction zone (3) are intercepted by described Lian Qi area (2), and described Lian Qi area is used for completely cutting off sample molecule entrance electricity
From area.
5. a kind of inverse expansion HADAMARD conversion ionic migration spectrometer according to claim 1 it is characterised in that：Described
The opening time of ion gate is 50 μ s～600 μ s, and migration electric field strength is 260～500V/cm.
6. a kind of inverse expansion HADAMARD conversion ionic migration spectrometer according to claim 1 it is characterised in that：Described
Migration area (5) replaces placement by a series of beckets and polytetrafluoroethylene ring and forms, by equivalent even resistance by each metal
Ring connects formation and uniformly migrates electric field (14).
7. a kind of inverse expansion HADAMARD conversion ionic migration spectrometer according to claim 1 it is characterised in that：Described
Charge detection area includes faraday's plate (16) and Signal Pretreatment unit (17), detects ionic charge signal by faraday's plate,
And signal is accessed Signal Pretreatment unit, complete ion current and amplify and the conversion of current/voltage signal.
8. a kind of inverse expansion HADAMARD conversion ionic migration spectrometer according to claim 1 it is characterised in that：Described
Inverse HADAMARD conversion signal processing module (7) will carry out inverse HADAMARD through detecting area pretreated superposition spectrum signal and become
Change process, obtain the migration modal data reducing, complete display and the comparison of data.
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| CN106324078A (en) * | 2016-09-12 | 2017-01-11 | 安徽理工大学 | Modified Hadamard multiplexing counter ion migration spectrum experimental apparatus |
| CN106248780A (en) * | 2016-09-12 | 2016-12-21 | 安徽理工大学 | A kind of reverse impulse HADAMARD ion mobility spectrometry |
| CN107516628B (en) * | 2017-08-15 | 2019-08-27 | 中国科学院合肥物质科学研究院 | A kind of bipolarity Hadamard transformation ionic migration spectrometer |
| CN108776166A (en) * | 2018-05-29 | 2018-11-09 | 中国科学院合肥物质科学研究院 | A kind of spectrum modulation Hadamard transform ionic migration spectrometer |
| CN113466318A (en) * | 2021-06-22 | 2021-10-01 | 西安电子科技大学 | Control method, system and equipment of super-resolution ion mobility spectrometer |
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