CN102903599B - The transference tube of application surface desorption atmospheric chemical ionization technology - Google Patents
The transference tube of application surface desorption atmospheric chemical ionization technology Download PDFInfo
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- CN102903599B CN102903599B CN201210413718.4A CN201210413718A CN102903599B CN 102903599 B CN102903599 B CN 102903599B CN 201210413718 A CN201210413718 A CN 201210413718A CN 102903599 B CN102903599 B CN 102903599B
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Abstract
The invention discloses the transference tube of application surface desorption atmospheric chemical ionization technology, comprise ionization reaction zone, ion gate grid, migration area and signal collector, it also comprises surface desorption atmospheric chemical ionization source, described surface desorption atmospheric chemical ionization source is communicated with ionization reaction zone, and it comprises: reaction reagent adding set; High pressure ionization device, described high pressure ionization device comprises a housing, spray point and capillary, provided a through hole in described housing, and on housing, offered the connecting hole be communicated with through hole, described connecting hole is communicated with reaction reagent adding set by wireway; Described spray point is worn in the through hole penetrated on housing, and the needle point of spray point stretches out in housing, and the backshank of spray point connects high voltage source; Described capillary is placed in through hole.Have the advantage of two aspects compared with application of nickel 63 ionization source, one be new ionization source is cold ionization source; Two be sample without the need to preliminary treatment, solid, Powdered.
Description
Technical field
The present invention relates to a kind of Ion mobility spectrometry, be specifically related to a kind of transference tube of application surface desorption atmospheric chemical ionization technology.
Background technology
Ion mobility spectrometry is through the development of several years, and, detection sensitivity advantages of higher fast by means of its analysis speed, this technology is ripe is applied in the on-the-spot field of fast detection such as drugs, explosive.
The basis of Ion mobility spectrometry analysis is that sample molecule is converted into charged ion, and completes under the effect of linear transport electric field and move and the process be separated, and ion is finally converted into the signal of telecommunication, to complete the separation of different sample, the object of confirmation.
Sample molecule is converted into charged ion finally becomes the signal of telecommunication, and whole process completes in transference tube, and transference tube is the core of ionic migration spectrometer.What sample molecule was converted into that charged ion then leans on is ionization source, and ionization source conventional is at present Beta-ray nickel 63 source of release.Although nickel 63 source has many good qualities in the application of Ion mobility spectrometry, but shortcoming is obvious too, because nickel 63 source belongs to radioactive ionization source, laws and regulations have strict regulation to links such as the purchase of user in nickel 63 source, use, management, recovery, and environmental protection is built consensus gradually due to present society, user also slowly starts to conflict for the ion mobility spectrometry equipment that nickel 63 source is housed.
So provide a kind of transference tube without radiation ionization source will to be the problem that this area needs solution badly.
Summary of the invention
The present invention is directed to the problem of existing transference tube employing existing for radiation ionization source, and a kind of transference tube without radiation ionization source is provided.This transference tube realizes based on application surface desorption atmospheric chemical ionization technology, and the transference tube of alternative former application of nickel 63 ionization source is used for Ion mobility spectrometry.
In order to achieve the above object, the present invention adopts following technical scheme:
The transference tube of application surface desorption atmospheric chemical ionization technology, comprise ionization reaction zone, ion gate grid, migration area and signal collector, described transference tube also comprises surface desorption atmospheric chemical ionization source, described surface desorption atmospheric chemical ionization source is communicated with ionization reaction zone, and it comprises:
Reaction reagent adding set;
High pressure ionization device, described high pressure ionization device comprises a housing, spray point and capillary, provided a through hole in described housing, and on housing, offered the connecting hole be communicated with through hole, described connecting hole is communicated with reaction reagent adding set by wireway; Described spray point is worn in the through hole penetrated on housing, and the needle point of spray point stretches out in housing, and the backshank of spray point connects high voltage source; Described capillary is placed in through hole.
In preferred embodiment of the present invention, described reaction reagent adding set comprises carrier gas source and reaction reagent bogey, described carrier gas source is communicated with reaction reagent bogey by wireway, and described reaction reagent bogey is communicated with the connecting hole on high pressure ionization device middle shell by wireway.
Further, making for rhenium alloys or stainless steel of described spray point, the tip diameter of spray point is about 100-200 μm.
Further, the needle point of described spray point stretches out the length of housing is 0.5mm-1mm.
Further, described carrier gas source is nitrogen or air.
Further, described capillary to be internal diameter the be Peek pipe of 350 μm.
Have the following advantages according to the present invention that such scheme obtains:
(1) this transference tube applies cold ionization source, and the transference tube of alternative former application of nickel 63 ionization source of this transference tube;
(2) for the transference tube in application of nickel 63 source, sample must do preliminary treatment, sample needs at high temperature heating and gasifying to be that gaseous state effectively could carry out ionization reaction, surface desorption atmospheric chemical ionization source does not then need to carry out preliminary treatment to sample, therefore to the solid-state sample comprising pulverulence, effective desorption ionization can occur under normal temperature, normal pressure.
Accompanying drawing explanation
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Fig. 1 is the structural representation of structure of the present invention;
Fig. 2 is the schematic diagram in surface desorption atmospheric chemical ionization source;
Fig. 3 is operating diagram of the present invention.
Embodiment
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
See Fig. 1, transference tube provided by the invention forms primarily of Ion transfer tube body 100 and surface desorption atmospheric chemical ionization source 200.
Wherein, Ion transfer tube body 100 connects to form successively primarily of ionization reaction zone 101, ion gate grid 102, migration area 103 and signal collector 104.
Surface desorption atmospheric chemical ionization source 200 is communicated with ionization reaction zone 101, forms transference tube of the present invention thus.
During transference tube work provided by the invention: first, surface desorption atmospheric chemical ionization source 200 is under the acting in conjunction of high pressure and chemical reagent, produce highdensity reagent ion, namely initial ion, initial ion is moving the move under influence of electrode to ionization reaction zone 101, in ionization reaction zone 101, reagent carries out the chemical desorption ionization of free of contamination surperficial normal pressure to sample, form sample ions, sample ions is moved to ion gate grid 102 direction under the effect of electric field, the sample be not ionized and impurity are extracted out body by air-flow, simultaneously, ion gate grid 102 are with certain cycle switch door, sample ions is made to enter migration area 103 with certain cycle, finally move to signal collector 104, be converted into the signal of telecommunication by charge collection dish 104a wherein and amplified by amplification module 104b.
Based on above-mentioned principle, specific embodiment of the invention is as follows:
See Fig. 2, it is depicted as the concrete composition structure in surface desorption atmospheric chemical ionization source in the present invention.As seen from the figure, this ionization source 200 mainly comprises reaction reagent adding set 201 and high pressure ionization device 202 two parts.
Wherein reaction reagent adding set 201 comprises carrier gas source 201a and reaction reagent bogey 201b, carrier gas source 201a provides corresponding carrier gas, it is communicated with reaction reagent bogey 201b by the first wireway 203, and reaction reagent bogey 201b is communicated with high pressure ionization device 202 by the second wireway 204.The carrier gas that carrier gas source 201a provides enters in reaction reagent bogey 201b by the first wireway 203, and taken out of by the reaction reagent in reaction reagent bogey 201b and entered in high pressure ionization device 202 by the second wireway 204, thus arrive corresponding reaction zone.
In actual applications, carrier gas source 201a is air or pure nitrogen, and in reaction reagent bogey 201b, the reaction reagent of carrying is water, acetic acid or ammonia etc.Concrete, if reaction reagent is water, in order to reach good reaction effect, carrier gas source adopts pure nitrogen or air, and its humidity is generally about 50%, and air-flow is 0-0.2Mpa.
High pressure ionization device 202 mainly utilizes electrion pin to form corona ionization, connects with the end of Ion transfer tube body 100.It comprises a housing 202a, spray point 202b and capillary 202c.
Housing 202a is a three-port structure, it has provided a through hole 202a1 in housing, and on housing, offer the connecting hole 202a2 be communicated with through hole 202a1, this connecting hole 202a2 is communicated with the second wireway 204, then realizes being communicated with of high pressure ionization device 202 and reaction reagent adding set 201.In order to realize connecting of high pressure ionization device 202 and Ion transfer tube body 100, one end of this housing 202a connects with the end of Ion transfer tube body 100, and is communicated with the ionization reaction zone 101 in Ion transfer tube body 100.
Capillary 202c is placed in housing and connects in the through hole 202a1 of a section with Ion transfer tube body 100, for the reaction reagent ejection of will be brought into by carrier gas in through hole 202a1.Concrete this capillary 202c employing internal diameter is the Peek pipe of 350 μm.
Spray point 202b is used for around it, forming electric field in high-pressure situations and ambient substance is ionized.It is worn in the through hole 202a1 that penetrates on housing, and passes from the capillary 202c in through hole 202a1, and then make the needle point of spray point 202b stretch out in housing, concrete extension elongation is 0.5mm-1mm; The backshank of spray point 202b connects high voltage source.
In order to reach good ionization effect, in the present invention, the tip diameter of spray point 202b is about 100-200 μm, and adding high pressure during work is about 3kV-5kV, DC, and generation current is about 0.01-20mA, and this depends on spray point tip size and surrounding environment.
For Ion transfer tube body 100, it connects to form successively primarily of ionization reaction zone 101, ion gate grid 102, migration area 103 and signal collector 104.
Sample ionization for ease of being formed in ionization reaction zone 101 can effectively enter ion gate grid 102, and the sample be not ionized and impurity are extracted out body by air-flow, the present invention is provided with electrical field draw pole plate 105(as shown in Figure 3 between ionization reaction zone 101 and ion gate grid 102).
Make sample ionization enter migration area 103 with certain cycle, ion gate grid 102 are with certain cycle switch door, and its switch periods is 20ms, and the opening time in the single cycle is 200 μ s.Meanwhile, the intensity of migration area 103 is about 200V/cm.
Based on above-mentioned example approach, the present invention is when embody rule, according to such scheme by each parts installed in series in order of Ion transfer tube body 100 in stainless steel shell, whole body accesses outside gas circuit, and and atmospheric isolation, ionization source part 200 is fixed on body end by flange, and junction O type circle sealing, forms complete transference tube thus.Its course of work following (see Fig. 2 and 3):
First, sample 300 is positioned in ionization reaction zone 101;
Then, add positive/negative high pressure on spray point 201b, when spray point surrounding electric field reaches some strength, first the material be easily ionized around needle point is ionized generation ionization reaction, generate corresponding cation and electronics, these charged particles obtain energy rapidly under the effect of electric field, continue to collide with other neutral molecule generation ionization reaction.
Reaction reagent is brought in the through hole 202a1 on housing 202a by carrier gas in addition, sprayed by the mouth of pipe of capillary 202c, and under the collision effect of the charged ion of said process generation, there is ionization reaction, then a large amount of positive/negative reagent ions is produced, also can be described as initial ion, these highdensity initial ion pair samples carry out the chemical desorption ionization of surface no-pollution then.If reaction reagent is water, after above-mentioned ionization reaction, producing a large amount of reagent ions is H
3o
+, the initial ion that this ionization source produces is pure, pollution-free, can not produce new interfering ion.
Ionization source produces a large amount of initial ion, initial ion at the move under influence of electric field and air-flow to ionization reaction zone 101, collide rapidly sample 300 surface, generation surface desorption ionizes, form sample belt electron ion, sample ions continues to enter migration area 103 by ion gate grid 102 under the effect of electric field, and the ion collection dish 104a finally reached in signal collector 104 is formed the signal of telecommunication and amplified by amplifier 104b; The sample be not ionized and impurity are extracted out body by air-flow.
This scheme has the advantage of two aspects compared with application of nickel 63 ionization source, and one be new ionization source is cold ionization source; Two be sample without the need to preliminary treatment, solid, Powdered.
More than show and describe general principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection range is defined by appending claims and equivalent thereof.
Claims (6)
1. the transference tube of application surface desorption atmospheric chemical ionization technology, comprise ionization reaction zone, ion gate grid, migration area and signal collector, it is characterized in that, described transference tube also comprises surface desorption atmospheric chemical ionization source, described surface desorption atmospheric chemical ionization source is communicated with ionization reaction zone, and it comprises:
Reaction reagent adding set;
High pressure ionization device, described high pressure ionization device comprises a housing, spray point and capillary, provided a through hole in described housing, and on housing, offered the connecting hole be communicated with through hole, described connecting hole is communicated with reaction reagent adding set by wireway; One end of described housing connects with the end of Ion transfer tube body, and be communicated with the ionization reaction zone in Ion transfer tube body, described capillary is placed in housing and connects in the through hole of a section with Ion transfer tube body, described spray point is worn in the through hole penetrated on housing, and pass from the capillary in through hole, then make the needle point of spray point stretch out in housing, the backshank of spray point connects high voltage source.
2. the transference tube of application surface desorption atmospheric chemical ionization technology according to claim 1, it is characterized in that, described reaction reagent adding set comprises carrier gas source and reaction reagent bogey, described carrier gas source is communicated with reaction reagent bogey by wireway, and described reaction reagent bogey is communicated with the connecting hole on high pressure ionization device middle shell by wireway.
3. the transference tube of application surface desorption atmospheric chemical ionization technology according to claim 1, is characterized in that, making for rhenium alloys or stainless steel of described spray point, and the tip diameter of spray point is 100-200 μm.
4. the transference tube of application surface desorption atmospheric chemical ionization technology according to claim 1, is characterized in that, the length that the needle point of described spray point stretches out housing is 0.5mm-1mm.
5. the transference tube of application surface desorption atmospheric chemical ionization technology according to claim 2, is characterized in that, described carrier gas source is nitrogen or air.
6. the transference tube of application surface desorption atmospheric chemical ionization technology according to claim 1, is characterized in that, described capillary to be internal diameter the be Peek pipe of 350 μm.
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| CN103776893B (en) * | 2014-02-17 | 2016-09-21 | 哈尔滨工业大学（威海） | A kind of dielectric barrier discharge ionization source ionic migration spectrometer |
| CN103940899B (en) * | 2014-03-21 | 2019-03-29 | 东华理工大学 | A kind of rapid detection method and device of trace explosive |
| CN107561150A (en) * | 2017-07-03 | 2018-01-09 | 宁波华仪宁创智能科技有限公司 | The detection method of drug abuse |
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| CN101201335A (en) * | 2006-12-29 | 2008-06-18 | 东华理工学院 | Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum |
| CN201185172Y (en) * | 2006-12-29 | 2009-01-21 | 东华理工大学 | Surface desorption atmospheric chemical ionization source |
| US7544933B2 (en) * | 2006-01-17 | 2009-06-09 | Purdue Research Foundation | Method and system for desorption atmospheric pressure chemical ionization |
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|---|---|---|---|---|
| US7544933B2 (en) * | 2006-01-17 | 2009-06-09 | Purdue Research Foundation | Method and system for desorption atmospheric pressure chemical ionization |
| CN101201335A (en) * | 2006-12-29 | 2008-06-18 | 东华理工学院 | Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum |
| CN201185172Y (en) * | 2006-12-29 | 2009-01-21 | 东华理工大学 | Surface desorption atmospheric chemical ionization source |
Non-Patent Citations (2)
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| 基于脉冲正电晕放电离子源的离子迁移谱仪研究;檀景辉;《中国优秀硕士学位论文全文数据库工程科技Ⅱ辑》;20120315;第8-25页 * |
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