CN106645380A - Reaction ion purification ion mobility spectrometry device and method based on air two-stage discharge - Google Patents
Reaction ion purification ion mobility spectrometry device and method based on air two-stage discharge Download PDFInfo
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- CN106645380A CN106645380A CN201611149430.5A CN201611149430A CN106645380A CN 106645380 A CN106645380 A CN 106645380A CN 201611149430 A CN201611149430 A CN 201611149430A CN 106645380 A CN106645380 A CN 106645380A
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- ion
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- area
- disengagement zone
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/68—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas
- G01N27/70—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas and measuring current or voltage
Abstract
The invention discloses a reaction ion purification ion mobility spectrometry device and method based on air two-stage discharge. Dielectric barrier discharge is performed in a primary discharge region, and hollow cathode discharge or corona discharge is performed in a secondary discharge region; after air is subjected to discharge in the primary discharge region, a neutral gas component is changed, the part of neutral gas enters the secondary discharge region, and high-purity NO2 plus can be produced. A two-stage air discharge ion purification technology is combined with an ion mobility spectrometry technology, the high-purity NO2 plus ion is taken as the reaction ion for an ion mobility spectrometry, and enters an ion mobility region through an ion grid door after being reacted with matter to be tested, and moves to an ion detection region under the effect of electric field. As the mobility ratios of different product ions are different, the speeds of ions are different, and the time arriving at the detection is different after the same mobility distance. The matter to be tested is detected and analyzed according to the difference of detection time.
Description
Technical field
The present invention relates to trace species analysis detection field, specifically a kind of reactive ion discharged based on air the two poles of the earth is pure
Change ion mobility spectrometry apparatus and method.
Background technology
Ion mobility spectrometry（Ion Mobility Spectrometry, IMS）It is two kinds of very important traces with mass spectrum
Detection of gas technology.Compared with mass spectrum, the most important feature of Ion mobility spectrometry is not need vacuum system, can be in air
Pressure work.Therefore ion mobility spectrometry instrument small volume, analysis cost are low, in environmental pollution, food safety, biological medicine, quick-fried
Fried thing and chemical agent detection field have a wide range of applications.
Through years of researches and development, Ion mobility spectrometry has defined traditional ion mobility spectrometry, asymmetric
The multiple technologies such as rf electric field ion mobility spectrometry and High-Field asymmetric waveform ion mobility spectrometry.Although these technologies are in the knot of device
Structure, the mode of applied voltage and gas circuit flow direction etc. has difference, but all includes ion source, three portions of ion isolation and detection
Point.In ion source region, by corona discharge or radioactive substance air molecule is ionized to form reactive ion（Containing it is various from
Son）, reactive ion enters into ionic reaction area in the presence of electric field and air-flow, anti-with test substance molecule generation chemi-ionization
Should, test substance is converted into into product ion.The very short time that reactive ion and product ion are opened in ion fence gate
（About hundreds of microsecond）It is interior, ion migration Disengagement zone is entered into, travel motion is made in the presence of electric field E and reaches ion acceptor.
Due to configuration and the difference of quality, the travel motion speed of different ions is different, migrates identical distance, different ions reach from
There is difference the time of sub-receiver, so as to separate and detect reactive ion and product ion, is reached by measuring product ion
The time of ion detector realizes the identification and detection to test substance.
Ionogenic main purpose is that test substance is become into ion, in order to the separation and detection of ion, be from
The important component part of son migration spectral technology.Mode and efficiency that test substance is converted into ion will be affected ion to move by ion source
Move the key indexs such as resolution, accuracy, sensitivity and the rate of false alarm of spectrum.In existing commercial Ion mobility spectrometry,
The ionizing of test substance is realized mainly by the way of chemi-ionization, i.e., by radioactive ionization gauge source, photoionization
The modes such as source, corona discharge ionization source, air ionization is generated comprising H3O+、NO+、O2 +In interior various reactive ions, and profit
There is ion-molecule reaction with reactive ion and test substance, test substance is converted into into ion.But direct ionization air
Various reactive ions, wherein H will be produced3O+、NO+、O2 +The signal intensity of three kinds of ions is most strong and for same magnitude, differential responses
Ion may react with test substance, complicate cause product ion, be unfavorable for the detection and identification of test substance.More
It is for complicated situation, H3O+、NO+、O2 +The signal intensity of three kinds of ions changes with the change of air humidity, have a strong impact on from
The stability of son migration spectrum.The method that at present commercial apparatus are adopted is to be dried under test gas and use process in instrument
In repeatedly calibrate repeatedly.If ambient humidity there occurs change and calibrate not in time, it will affect the accuracy of ion mobility spectrometry
And sensitivity, the rate of false alarm of instrument is improved, calibration process reduces the convenience that instrument is used.
Analysis finds, reactive ion wide variety and its relative scale becomes with test point ambient humidity in ion mobility spectrometry
Change and change be affect ion mobility spectrometry accuracy, rate of false alarm and the convenience for using key.How atmospherical discharges are utilized,
On the basis of the volume and ease of use for not dramatically increasing ion mobility spectrometry instrument, not tested pilot air humidity shadow is obtained
Loud single reactive ion be improve ion mobility spectrometry accuracy and sensitivity, the key of the rate of false alarm of lowering apparatus.
The content of the invention is it is an object of the invention to provide a kind of reactive ion purification ion discharged based on air the two poles of the earth is moved
Spectral apparatus and method are moved, is discharged using air two-stage, produce high purity N O2 +As the reactive ion of migration spectrum, utilization is solved
Air directly discharges can not produce the problem of high-purity single ionic, such that it is able to improving the resolution of ion mobility spectrometry, stablizing
Property and detectivity.In order to achieve the above object, the technical solution adopted in the present invention is：
A kind of reactive ion purification ion mobility spectrometry apparatus discharged based on air the two poles of the earth, it is characterised in that：Including：
One-level region of discharge, it adopts dielectric barrier discharge, by the N in air2, O2, H2The compositions such as O are converted into N through electric discharge2,
O2, H2O, O3, NO2, NO etc.；
Two-stage discharge area, the N that the gas for producing that front end is discharged is produced2, O2, H2O, O3, NO2, NO etc. imports two-stage discharge area,
Jing electric discharges produce highly purified NO2 +Primary response ion of the ion as ion mobility spectrometry.Two-stage discharge area adopts hollow cathode
Electric discharge or corona discharge；
Ionic reaction area, concentrically axle is connected with two-stage discharge area axial end for its front end, and ionic reaction area has for be measured
The entrance that organic molecule is entered；
Ion migration Disengagement zone, it is drift tube structure, during ion migration Disengagement zone front end is common with ionic reaction area axial end
Heart axle is connected, and connectivity part is provided with ion fence gate between ion migration Disengagement zone, ionic reaction area；
Ion detection area, it is Faraday plate, and the collector of Faraday plate is detected in ion migration Disengagement zone end.
A kind of described reactive ion purification ion mobility spectrometry apparatus discharged based on air the two poles of the earth, it is characterised in that：From
Sub- transport area is made up of electrode retaining collar and dead ring, and migration ring is connected by the equal resistance of resistance.The two of transport area
Plus migration voltage on the electrode retaining collar at end, so as to form uniform electric field in migration area.
A kind of reactive ion purification devices of described the two poles of the earth electric discharge, it is characterised in that：The ion fence gate is by being arranged on
A pair of ion fence gates of connectivity part are constituted between ion migration Disengagement zone, ionic reaction area, and for controlling ion migration area is entered.
When the voltage between the parallel pole on ion fence gate is equal, ion can enter drift region, reach in the presence of electric field
Ion detection area, when the voltage between the parallel pole on ion fence gate is unequal, ion source produce initial ion then without
Method enters into drift region.
A kind of reactive ion purification process of the two poles of the earth electric discharge, it is characterised in that：Air enters one-level region of discharge from air inlet,
Pass through dielectric barrier discharge in one-level region of discharge；Tail gas Jing after one-level region of discharge dielectric barrier discharge enters two-stage discharge
Area, produces in the case of hollow cathode discharge highly purified NO in two-stage discharge area2 +, and NO2 +Purity receive vapor
The impact of concentration；The highly purified NO that two-stage discharge area produces2 +Into ionic reaction area, at the same organic molecule to be measured enter from
Sub- reaction zone, the highly purified NO in ionic reaction area2 +Ion is reacted and generated with organic molecule to be measured；Give birth in ionic reaction area
Into ion when ion fence gate is opened enter ion migration Disengagement zone, and ion migration Disengagement zone intermediate ion migration electric field make
Migrated to the Faraday plate of ion migration Disengagement zone end with lower, Jing electric current is amplified and conversion after export to outside detection and set
It is standby.
Compared with the prior art, beneficial effects of the present invention are embodied in：
After dielectric barrier discharge, the composition of gas will change air, then this portion gas be imported into low pressure
Hollow cathode discharge, can produce the NO of high purity more than 95%2 +Even if, and the vapor of addition saturation, still will not shadow
Ring NO2 +The purity of ion.
Conventional ion mobility spectrometry is, using the direct ionization of atmospheric air, inevitably to produce different kinds of ions.
The present invention devises the device of two-stage atmospherical discharges ion mobility spectrometry reactive ion, and is obtained using atmospheric pressure two-stage atmospherical discharges
High purity N O2 +Ion obtains method.Highly purified NO is prepared using atmospheric pressure two-stage atmospherical discharges2 +Ion, it is not necessary to highly purified
Compression cyclinder gas, it is not necessary to access desiccant, the volume of increase instrument that will not be excessive because deionizing purification technology is introduced.
There is larger advantage on the ease of use and economy of instrument.
High purity N O is produced using two-stage atmospherical discharges2 +Reactive ion of the ion as ion mobility spectrometry.Due to reaction from
Subcategory is single, can simplify the identification of ion mobility spectrometry；The accuracy that instrument recognizes test substance is increased, instrument is reduced
Rate of false alarm.Simultaneously because the reactive ion for producing is not affected by ambient humidity, the stability of ion mobility spectrometry is improve, solved
The problem that existing ion mobility spectrometry of having determined needs to calibrate repeatedly.
Description of the drawings
Fig. 1 is the structural representation of the present invention.
Specific embodiment
As shown in figure 1, a kind of reactive ion purification ion mobility spectrometry apparatus discharged based on air the two poles of the earth, including：
One-level region of discharge 1, it adopts dielectric barrier discharge, and the front end of one-level region of discharge 1 is air inlet 11, air hence into；
Two-stage discharge area 2, concentrically axle is connected with the axial end of one-level region of discharge 1 for its front end, and two-stage discharge area 2 adopts hollow the moon
Discharge pole；
Ionic reaction area 3, concentrically axle is connected with the axial end of two-stage discharge area 2 for its front end, and ionic reaction area 3 has for be measured
The entrance 4 that gas is entered, bleeding point；
Ion migration Disengagement zone 6, it is drift tube structure, and the front end of ion migration Disengagement zone 6 is total to the axial end of ionic reaction area 3
Central shaft is connected, and connectivity part is provided with ion fence gate 7 between ion migration Disengagement zone 6, ionic reaction area 3；
There is Faraday plate ion detector 8 in the end of ion migration Disengagement zone 6.
Ion migration Disengagement zone 6 be drift tube structure, be provided with the drift tube it is multigroup under a certain pressure concentrically axle consolidate
Becket 9 together is scheduled on, multigroup becket constitutes drift rings, using becket as conducting ring, by gathering between adjacent metal ring
Tetrafluoroethene ring 10 insulate and seals, and is formed with ion migration electric field in drift tube between conducting ring；
Ion fence gate 7 is made up of a pair of aperture plates being arranged between ion migration Disengagement zone 4, ionic reaction area 3, two ion fence gates
Electric field perpendicular to ion migration Disengagement zone axial direction, the highfield of about 600V/cm is applied on ion fence gate, ion can be prevented
Pass through, when ion fence gate is opened, i.e. when the electric field of the aperture plate of ion fence gate two is zero, it is allowed to which ion passes through.
A kind of reactive ion purification process of the two poles of the earth electric discharge, air enters one-level region of discharge from air inlet, in one-level electric discharge
Pass through dielectric barrier discharge in area；Tail gas Jing after one-level region of discharge dielectric barrier discharge enters two-stage discharge area, two-stage discharge
Highly purified NO is produced in the case of hollow cathode discharge in area2 +, and NO2 +Purity do not affected by water vapor concentration；
The highly purified NO that two-stage discharge area produces2 +Into ionic reaction area, while organic molecule to be measured enters ionic reaction area,
Highly purified NO in ionic reaction area2 +Ion is reacted and generated with organic molecule to be measured；The ion that ionic reaction area generates exists
Ion fence gate enters ion migration Disengagement zone in the case of allowing to pass through, and makees in ion migration Disengagement zone intermediate ion migration electric field
Migrate with to ion migration Disengagement zone end；The collector of Faraday plate in ion detection area is constituted in ion migration Disengagement zone
End is detected, and when ion hits collector, ion is neutralized and produces faint electric current, electric current is amplified and conversion after it is defeated
Go out to outside testing equipment.
In the present invention, including one-level region of discharge 1, two-stage discharge area 2, ionic reaction area 3, ion migration Disengagement zone 6, ion
Detecting area 8, ion fence gate 7.Specifically, one-level region of discharge 1 is dielectric barrier discharge；Two-stage discharge area 2 is hollow cathode discharge；
And then ionic reaction area 3 is determinand organic molecule behind two-stage discharge area 2, the NO produced with two-stage discharge2 +Reaction is carried
For place；Ion migration Disengagement zone 6 links together with ionic reaction area 3, when ion fence gate is opened, produces after reaction
Ion enter drift region, drifted about in the presence of drift field；Ion fence gate 7 be placed in the ionic reaction area 3 and from
Between sub- transport area 4, reaction zone is separated with migration area；Ion detection area is placed in the end of ion migration Disengagement zone 4
End detects ion signal by Faraday plate, and drift rings 7 are placed in whole drift tube, by one group of becket under certain pressure effect
It is fixed together.
Claims (4)
1. it is a kind of based on air the two poles of the earth discharge reactive ion purification ion mobility spectrometry apparatus, it is characterised in that：Including：
One-level region of discharge, it adopts dielectric barrier discharge, and air is converted into containing N2, O2, H2O, O3, NO2, the composition such as NO
Gas；
Two-stage discharge area, the N that the gas for producing that front end is discharged is produced2, O2, H2O, O3, NO2, NO etc. imports two-stage discharge area, Jing
Electric discharge produces highly purified NO2 +Primary response ion of the ion as ion mobility spectrometry；Put using hollow cathode in two-stage discharge area
Electricity or corona discharge；
Ionic reaction area, concentrically axle is connected with two-stage discharge area axial end for its front end, and ionic reaction area has for be measured
The entrance that organic molecule is entered, in ionic reaction area, NO2 +Ion generates product ion with test substance reaction；
Ion migration Disengagement zone, it is drift tube structure, during ion migration Disengagement zone front end is common with ionic reaction area axial end
Heart axle is connected, and connectivity part is provided with ion fence gate between ion migration Disengagement zone, ionic reaction area；
Ion detection area, it is Faraday plate, and the collector of Faraday plate is detected in ion migration Disengagement zone end.
2. it is according to claim 1 it is a kind of based on air the two poles of the earth discharge reactive ion purification ion mobility spectrometry apparatus, its
It is characterised by：Ion migration Disengagement zone is made up of electrode retaining collar and dead ring, and migration ring is connected by the equal resistance of resistance；In migration
Plus migration voltage on the electrode retaining collar at the two ends of Disengagement zone, so as to form uniform electric field in migration area.
3. the reactive ion purification devices that a kind of the two poles of the earth according to claim 1 and 2 are discharged, it is characterised in that：It is described from
The ion grid that sub- fence gate is made up of a pair of parallel electrode for being arranged on connectivity part between ion migration Disengagement zone, ionic reaction area
Door；When the voltage between the parallel pole on ion fence gate is equal, ion can enter drift region, arrive in the presence of electric field
Up to ion detection area；When the voltage between the parallel pole on ion fence gate is more than 50 volts, the initial ion that ion source is produced
Then cannot be introduced into drift region.
4. the reactive ion purification process that a kind of the two poles of the earth are discharged, it is characterised in that：Air enters one-level region of discharge from air inlet,
Pass through dielectric barrier discharge in one-level region of discharge；Tail gas Jing after one-level region of discharge dielectric barrier discharge enters two-stage discharge area,
Highly purified NO is produced in the case of hollow cathode discharge in two-stage discharge area2 +, and NO2 +Purity by vapor it is dense
The impact of degree；The highly purified NO that two-stage discharge area produces2 +Into ionic reaction area, while organic molecule to be measured enters ion
Reaction zone, the highly purified NO2 in ionic reaction area+Ion is reacted and generated with organic molecule to be measured；Give birth in ionic reaction area
Into ion when ion fence gate is opened enter ion migration Disengagement zone, and ion migration Disengagement zone intermediate ion migration electric field make
Migrated to the Faraday plate of ion migration Disengagement zone end with lower, Jing electric current is amplified and conversion after export to outside detection and set
It is standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611149430.5A CN106645380A (en) | 2016-12-14 | 2016-12-14 | Reaction ion purification ion mobility spectrometry device and method based on air two-stage discharge |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611149430.5A CN106645380A (en) | 2016-12-14 | 2016-12-14 | Reaction ion purification ion mobility spectrometry device and method based on air two-stage discharge |
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| CN201611149430.5A Pending CN106645380A (en) | 2016-12-14 | 2016-12-14 | Reaction ion purification ion mobility spectrometry device and method based on air two-stage discharge |
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