CN106783509A - Open type atmospheric pressure ionization device and method - Google Patents
Open type atmospheric pressure ionization device and method Download PDFInfo
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- CN106783509A CN106783509A CN201610991572.XA CN201610991572A CN106783509A CN 106783509 A CN106783509 A CN 106783509A CN 201610991572 A CN201610991572 A CN 201610991572A CN 106783509 A CN106783509 A CN 106783509A
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- atmospheric pressure
- open type
- shower nozzle
- nozzle
- type atmospheric
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- 238000000034 method Methods 0.000 title abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 230000004888 barrier function Effects 0.000 claims abstract description 17
- 238000001819 mass spectrum Methods 0.000 claims description 22
- 230000008676 import Effects 0.000 claims description 11
- 238000000752 ionisation method Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 238000006276 transfer reaction Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 150000008043 acidic salts Chemical class 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims 1
- 150000002500 ions Chemical class 0.000 description 22
- 239000000243 solution Substances 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000002347 injection Methods 0.000 description 9
- 239000007924 injection Substances 0.000 description 9
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- JBTHDAVBDKKSRW-UHFFFAOYSA-N chembl1552233 Chemical compound CC1=CC(C)=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 JBTHDAVBDKKSRW-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229940073450 sudan red Drugs 0.000 description 4
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 3
- 229960001948 caffeine Drugs 0.000 description 3
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000010884 ion-beam technique Methods 0.000 description 3
- WJNRPILHGGKWCK-UHFFFAOYSA-N propazine Chemical compound CC(C)NC1=NC(Cl)=NC(NC(C)C)=N1 WJNRPILHGGKWCK-UHFFFAOYSA-N 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001601 dielectric barrier discharge ionisation Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 235000011167 hydrochloric acid Nutrition 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
Abstract
The invention provides a kind of open type atmospheric pressure ionization device and method, the open type atmospheric pressure ionization device includes dielectric barrier discharge ion gun, and container, the container accommodates auxiliary liquid；Supply unit, the supply unit is used to for the auxiliary liquid in the container to be transported to shower nozzle；Shower nozzle, is ionized from the auxiliary liquid of the shower nozzle outgoing by the beam-plasma of the nozzle outgoing from the dielectric barrier discharge ion gun；Power supply, the power supply applies DC voltage to the shower nozzle；Injector, from the auxiliary liquid ionization that the testing sample of the injector outgoing is ionized.The present invention has the advantages that sample ionization efficiency high, signal to noise ratio are high.
Description
Technical field
The present invention relates to mass spectral analysis, more particularly to open type atmospheric pressure ionization device and method.
Background technology
Open type mass ion source is that one kind or need not only need little sample pre-treatments, can be in unlimited atmospheric pressure environment
In direct novel ion source that sample is desorbed and ionized, in situ, real-time, quick mass spectral analysis needs can be met,
And with detection stability higher and sensitivity (up to ppb grade), be current mass spectrometer field compete focus, focus and
Forward position.
DBDI is to teach a kind of new mass ions proposed first in the world in 2007 by Tsing-Hua University Zhang Xinrong
Source, general principle is：The inert gases such as helium in insulated dielectric tube are excited by ac high-voltage, sprayable plasma is formed
Body beam, recycles the mechanism such as Penning ionization to realize sample ionization, be a kind of non-surface contact-type atmospheric pressure parsing/ionization-
Analytical technique of mass spectrum.
At present, have that sample ionization efficiency is low, the low deficiency of signal to noise ratio using the mass spectrograph of DBDI.
The content of the invention
To solve the deficiency in above-mentioned prior art, the invention provides a kind of sample ionization efficiency high, noise
The open type atmospheric pressure ionization device higher than high, detection sensitivity.
The purpose of the present invention is achieved through the following technical solutions：
A kind of open type atmospheric pressure ionization device, the open type atmospheric pressure ionization device includes dielectric barrier discharge
Ion gun；The open type atmospheric pressure ionization device is further included：
Container, the container accommodates auxiliary liquid；
Supply unit, the supply unit is used to for the auxiliary liquid in the container to be transported to shower nozzle；
Shower nozzle, from the auxiliary liquid of the shower nozzle outgoing by the nozzle outgoing from the dielectric barrier discharge ion gun etc.
Ion beam ion；
Power supply, the power supply applies DC voltage to the shower nozzle；
Injector, from the auxiliary liquid ionization that the testing sample of the injector outgoing is ionized.
According to above-mentioned open type atmospheric pressure ionization device, it is preferable that the shower nozzle is hollow acicular texture.
According to above-mentioned open type atmospheric pressure ionization device, it is preferable that the internal diameter of the shower nozzle is 20-100 μm, described
The internal diameter in the exit of shower nozzle is 5-30 μm.
According to above-mentioned open type atmospheric pressure ionization device, it is preferable that the end of the shower nozzle, the end of injector with
The inwall of the end for facing mass spectrum import of the nozzle of the dielectric barrier discharge ion gun is outside along the central axis of nozzle
The outer rim for extending the solid for being formed is tangent.
According to above-mentioned open type atmospheric pressure ionization device, it is preferable that the central axis of the nozzle and mass spectrum import
Central axis it is conllinear.
According to above-mentioned open type atmospheric pressure ionization device, alternatively, the inner and outer wall of the shower nozzle has conduction
Layer, the power supply connects the conductive layer.
According to above-mentioned open type atmospheric pressure ionization device, it is preferable that the auxiliary liquid is acid or acidic salt solution.
According to above-mentioned open type atmospheric pressure ionization device, it is preferable that the DC voltage is 0-20KV.
The present invention also aims to provide, a kind of ion beam jet length is remote, intensity is high, gas utilization efficiency is high
Gene transferring by N~+ method, the goal of the invention is achieved by the following technical programs：
Open type atmospheric pressure ionization method, the open type atmospheric pressure ionization method is comprised the following steps：
(A1) gas is ionized to form plasma beam in dielectric barrier discharge ion gun, and from nozzle outgoing；
(A2) with the plasma beam from nozzle outgoing there is electric charge in the auxiliary liquid for being applied in voltage from shower nozzle outgoing
Transfer reaction, so as to be ionized；
(A3) there is charge transfer reaction with the auxiliary liquid of ionization from the testing sample of injector outgoing, so as to by from
Sonization.
According to above-mentioned open type atmospheric pressure ionization method, it is preferable that the end of the shower nozzle, the end of injector with
The inwall of the end for facing mass spectrum import of the nozzle stretches out the outer of the solid to be formed along the central axis of nozzle
Edge is tangent.
Compared with prior art, the device have the advantages that being：
1. the Ionization Efficiency of sample can be improved, increases signal intensity, reduce ambient noise, significantly improved cut-off and stop
The detection sensitivity of discharge ion source；
2. by aiding in different solution distinctive adduct ion form can be formed for different samples.
Brief description of the drawings
Referring to the drawings, the disclosure will be easier to understand.Skilled addressee readily understands that be：This
A little accompanying drawings are used only for illustrating technical scheme, and are not intended to be construed as limiting protection scope of the present invention.
In figure：
Fig. 1 is the structure diagram of according to embodiments of the present invention 1 open type atmospheric pressure ionization device；
Fig. 2 is the mass spectrogram of the caffeine measured according to prior art；
Fig. 3 is the mass spectrogram of according to embodiments of the present invention 2 caffeines measured；
Fig. 4 is the mass spectrogram of the propazine measured according to prior art；
Fig. 5 is the mass spectrogram of according to embodiments of the present invention 3 propazines measured；
Fig. 6 is the Sudan red mass spectrogram measured according to prior art；
Fig. 7 is the according to embodiments of the present invention 4 Sudan red mass spectrograms measured.
Specific embodiment
Fig. 1-7 and following description describe optional embodiment of the invention to instruct how those skilled in the art implement
It is of the invention with reproducing.In order to instruct technical solution of the present invention, some conventional aspects are simplified or have eliminated.Those skilled in the art
It should be appreciated that modification or replacement from these implementation methods will within the scope of the invention.Those skilled in the art should understand that
Following characteristics can combine to form multiple modifications of the invention in a variety of ways.Thus, the invention is not limited in it is following can
Implementation method is selected, and is only limited by claim and their equivalent.
Embodiment 1：
Fig. 1 schematically illustrates the structure diagram of the open type atmospheric pressure ionization device of the embodiment of the present invention, such as Fig. 1
Shown, the open type atmospheric pressure ionization device includes：
Dielectric barrier discharge ion gun；
Container, the container accommodates auxiliary liquid, such as correspondingly sets acid or acid salt solution according to detection object difference
As assisted solution, such as hydrochloric acid, phosphoric acid, formic acid, acetic acid, benzoic acid；Such as carbonate, phosphate, borate solution；
Supply unit, the supply unit is used to for the auxiliary liquid in the container to be transported to shower nozzle, such as using pump, pipe
Quantitative, conveying auxiliary liquid is removed in the combination in road；
Shower nozzle, from the auxiliary liquid of the shower nozzle outgoing by the nozzle outgoing from the dielectric barrier discharge ion gun etc.
Ion beam ion；
Power supply, the power supply applies DC voltage to the shower nozzle；
Injector, from the auxiliary liquid ionization that the testing sample of the injector outgoing is ionized.
Open type atmospheric pressure ionization method, the open type atmospheric pressure ionization method is comprised the following steps：
(A1) gas is ionized to form plasma beam in dielectric barrier discharge ion gun, and from nozzle outgoing；
(A2) with the plasma beam from nozzle outgoing there is electric charge in the auxiliary liquid for being applied in voltage from shower nozzle outgoing
Transfer reaction, so as to be ionized；
(A3) there is charge transfer reaction with the auxiliary liquid of ionization from the testing sample of injector outgoing, so as to by from
Sonization.
Embodiment 2：
Application of the according to embodiments of the present invention 1 open type atmospheric pressure ionization device and method in caffeine is detected
Example.
In the application examples, container selection closed glass jar, volume 50mL；Shower nozzle selects quartz glass capillary, internal diameter
It it is 20 μm, exit internal diameter is 10 μm, shower nozzle connection voltage is set to 0V；The heating-up temperature of dielectric barrier discharge ion gun is set to
140 DEG C, nozzle is away from mass spectrum injection port 1.5cm；Injector uses sample introduction capillary, away from mass spectrum injection port 0.5cm, shower nozzle be located at from
Between component nozzle and sample introduction capillary, away from mass spectrum injection port 1cm, the end of the shower nozzle, the end of injector and given an account of
The inwall of the end for facing mass spectrum import of the nozzle of matter barrier discharge ion gun stretches out shape along the central axis of nozzle
Into solid outer rim it is tangent, the shower nozzle and injector outlet central axis respectively with the central axis phase of the nozzle
Hand over, the central axis of the nozzle is conllinear with the central axis of mass spectrum import；Mass Spectrometer Method m/z scopes are set to 50~1000, lazy
Property gas flow rate be set to 0.8L/min, detection sample is caffeine standards sample (being dissolved in methyl alcohol, concentration 50ppb), assisted solution
It is the hydrochloric acid solution of 5mol.As Figure 2-3, Mass Spectrometer Method sensitivity improves 12 times.
Embodiment 3：
Application of the according to embodiments of the present invention 1 open type atmospheric pressure ionization device and method in propazine is detected
Example.
In the application examples, container selection closed metal bottle, volume 50mL；Shower nozzle uses quartz glass capillary, inwall
Conductive layer is coated with outer wall, internal diameter is 50 μm, and exit internal diameter is 30 μm；Conductive layer connection DC voltage is set to 10V；Ion gun
Heating-up temperature be set to 140 DEG C, away from mass spectrum injection port 1.5cm, sample introduction capillary is away from mass spectrum injection port 0.5cm, shower nozzle position for nozzle
Between ion gun nozzle and sample introduction capillary, away from mass spectrum injection port 1cm, the end of the shower nozzle, the end of injector and institute
State the nozzle of dielectric barrier discharge ion gun the end for facing mass spectrum import inwall along the central axis of nozzle to extension
The outer rim for stretching the solid to be formed is tangent, the shower nozzle and injector outlet central axis respectively with the central shaft of the nozzle
Line intersects, and the central axis of the nozzle is conllinear with the central axis of mass spectrum import；Mass Spectrometer Method m/z scopes are set to 50~
1000, inert gas flow velocity is set to 0.8L/min, and detection sample is propazine standard sample (being dissolved in methyl alcohol, concentration 50ppb), auxiliary
Hydrotropy liquid is the acetic acid solution of 5mol.As illustrated in figures 4-5, Mass Spectrometer Method sensitivity improves 10 times.
Embodiment 4：
Application of the according to embodiments of the present invention 1 open type atmospheric pressure ionization device and method in detection is Sudan red
Example.
In the application examples, container selection closed metal bottle, volume is 50mL；Shower nozzle selects metal material, and internal diameter is 50 μ
M, the internal diameter in exit is 15 μm；Shower nozzle connection voltage is set to 20V；The heating-up temperature of ion gun is set to 140 DEG C, ion gun nozzle
Away from mass spectrum injection port 1.5cm, sample introduction capillary is located between nozzle and sample introduction capillary away from mass spectrum injection port 0.5cm, shower nozzle, away from
Mass spectrum injection port 1cm, the end of the shower nozzle, the end of injector are faced with the nozzle of the dielectric barrier discharge ion gun
The inwall of the end of mass spectrum import along the central axis of nozzle stretch out the solid to be formed outer rim it is tangent, the shower nozzle
Central axis of the central axis exported with injector respectively with the nozzle intersects, and central axis and the mass spectrum of the nozzle enter
The central axis of mouth is conllinear；Mass Spectrometer Method m/z scopes are set to 50~1000, and inert gas flow velocity is set to 0.8L/min, detect sample
Product are Sudan red standard sample (being dissolved in methyl alcohol, concentration 100ppb), and assisted solution is the carbonate solution of 10mol.Such as Fig. 6-7
Shown, Mass Spectrometer Method sensitivity improves 6 times.
Claims (10)
1. a kind of open type atmospheric pressure ionization device, the open type atmospheric pressure ionization device include dielectric barrier discharge from
Component；It is characterized in that：The open type atmospheric pressure ionization device is further included：
Container, the container accommodates auxiliary liquid；
Supply unit, the supply unit is used to for the auxiliary liquid in the container to be transported to shower nozzle；
Shower nozzle, the auxiliary liquid from the shower nozzle outgoing is by the plasma of the nozzle outgoing from the dielectric barrier discharge ion gun
Beam；
Power supply, the power supply applies DC voltage to the shower nozzle；
Injector, from the auxiliary liquid ionization that the testing sample of the injector outgoing is ionized.
2. open type atmospheric pressure ionization device according to claim 1, it is characterised in that：The shower nozzle is hollow pin
Shape structure.
3. open type atmospheric pressure ionization device according to claim 2, it is characterised in that：The internal diameter of the shower nozzle is
20-100 μm, the internal diameter in the exit of the shower nozzle is 5-30 μm.
4. open type atmospheric pressure ionization device according to claim 1, it is characterised in that：The end of the shower nozzle, enter
The inwall of the end of sample device and the end for facing mass spectrum import of the nozzle of the dielectric barrier discharge ion gun is along nozzle
Central axis stretch out the solid to be formed outer rim it is tangent.
5. open type atmospheric pressure ionization device according to claim 4, it is characterised in that：The central axis of the nozzle
Central axis with mass spectrum import is conllinear.
6. open type atmospheric pressure ionization device according to claim 1, it is characterised in that：The inwall of the shower nozzle and outer
Wall has conductive layer, and the power supply connects the conductive layer.
7. open type atmospheric pressure ionization device according to claim 1, it is characterised in that：The auxiliary liquid be acid or
Acidic salt solution.
8. open type atmospheric pressure ionization device according to claim 1, it is characterised in that：The DC voltage is 0-
20KV。
9. open type atmospheric pressure ionization method, the open type atmospheric pressure ionization method is comprised the following steps：
(A1) gas is ionized to form plasma beam in dielectric barrier discharge ion gun, and from nozzle outgoing；
(A2) with the plasma beam from nozzle outgoing there is electric charge transfer in the auxiliary liquid for being applied in voltage from shower nozzle outgoing
Reaction, so as to be ionized；
(A3) there is charge transfer reaction in testing sample and the auxiliary liquid of ionization from injector outgoing, so as to by ion
Change.
10. open type atmospheric pressure ionization method according to claim 9, it is characterised in that：The end of the shower nozzle, enter
The end of sample device stretches out to be formed with the inwall of the end for facing mass spectrum import of the nozzle along the central axis of nozzle
Solid outer rim it is tangent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610991572.XA CN106783509B (en) | 2016-11-10 | 2016-11-10 | Open type atmospheric pressure ionization device and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610991572.XA CN106783509B (en) | 2016-11-10 | 2016-11-10 | Open type atmospheric pressure ionization device and method |
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| Publication Number | Publication Date |
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| CN106783509A true CN106783509A (en) | 2017-05-31 |
| CN106783509B CN106783509B (en) | 2018-02-09 |
Family
ID=58972992
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| CN201610991572.XA Active CN106783509B (en) | 2016-11-10 | 2016-11-10 | Open type atmospheric pressure ionization device and method |
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Cited By (3)
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| CN108133878A (en) * | 2017-12-31 | 2018-06-08 | 宁波大学 | Open type ion source |
| CN108445073A (en) * | 2018-03-16 | 2018-08-24 | 常州英诺激光科技有限公司 | Solve the method and mass spectrograph that plasma lifetime to be measured is short in normal pressure open-type laser mass spectrograph |
| CN109686648A (en) * | 2018-12-26 | 2019-04-26 | 广州市华粤行仪器有限公司 | Mass spectrometer and manufacturing method |
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| Publication number | Publication date |
|---|---|
| CN106783509B (en) | 2018-02-09 |
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