CN105097413B - Novel ion source and ionization method - Google Patents
Novel ion source and ionization method Download PDFInfo
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- CN105097413B CN105097413B CN201510595870.2A CN201510595870A CN105097413B CN 105097413 B CN105097413 B CN 105097413B CN 201510595870 A CN201510595870 A CN 201510595870A CN 105097413 B CN105097413 B CN 105097413B
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- insulation tube
- electrode
- ion source
- novel ion
- insulation
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- 238000000752 ionisation method Methods 0.000 title abstract 2
- 238000009413 insulation Methods 0.000 claims description 88
- 238000000034 method Methods 0.000 claims description 23
- 239000012159 carrier gas Substances 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 12
- 230000009467 reduction Effects 0.000 claims description 8
- 230000008602 contraction Effects 0.000 claims 1
- 150000002500 ions Chemical class 0.000 description 37
- 238000001601 dielectric barrier discharge ionisation Methods 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 8
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 7
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 4
- 229960001948 caffeine Drugs 0.000 description 4
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229960005489 paracetamol Drugs 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000000688 desorption electrospray ionisation Methods 0.000 description 3
- 238000000375 direct analysis in real time Methods 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- 230000009849 deactivation Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000010265 fast atom bombardment Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000451 chemical ionisation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a novel ion source and an ionization method. The novel ion source comprises a first insulating pipe, an electrode and a second insulating pipe, wherein openings are formed in two ends of the first insulating pipe; only one electrode is arranged at the outer side of the first insulating pipe; the electrode comprises a wiring end; and the second insulating pipe is arranged at the outer side of the first insulating pipe and is located at the non-radial side part of the first insulating pipe of the electrode. The novel ion source has the advantages of wide application range and the like.
Description
Technical field
The present invention relates to ion source, more particularly to ion source and ioning method.
Background technology
Mass-spectrometric technique is one of most wide analysis method of the most sensitive and range of application being currently known.In mass-spectrometric technique,
Ion source is the Primary Component of sample ionization technology.
At present, there are different kinds of ions source, such as electron impact ion source (EI), chemical ionization source (CI), field-ionization/field
Desorption ionization source (FI/FD), fast atom bombardment source (FAB), electron spray ionisation source (ESI), laser desorption source (LD), atmospheric pressure
Learn ionization source (APCI) etc..For these ion sources, sample before ionizing must through loaded down with trivial details pretreatment, therefore, these
Ionogenic common deficiency is：Sample can not the directly attached ionizing of fast desorption, namely the continuous, real of target components cannot be realized
When monitoring and high throughput analysis or imaging analysis.
In recent years, desorption electro-spray ionization (DESI), Direct Analysis in Real Time (DART) ionizing and dielectric impedance are put
Electric (DBDI) ionogenic appearance, these Ionization modes directly quick in the case where sample surfaces realize normal pressure can be analyzed, sample
Without the need for pretreatment.These ion sources have deficiency, such as：
DESI ion sources, need high voltage power supply to build high-voltage electrostatic field, make electron spray capillary tube front end be susceptible to corona,
High pressure also limit and for ion source develop into probability that is hand-held and directly making lossless quick analysis to human skin；Institute
The ionizing solvent for using and the gas of high flow rate, not only high cost but also can cause certain pollution to environment.
DART ion sources, eliminate solvent, but need the ionized gas of high-tension electricity and high flow rate, and in order to obtain
Must stablize, efficient ionising effect, need to use electrode, right multi-electrode (high-field electrode, gate electrode, ground electrode) design is multiple
It is miscellaneous, the miniaturization of instrument should not be realized.
DBDI ion sources, in the DBDI of ion source positioned inside bipolar electrode, interior electrode is especially bar-like, needle electrode pole
The oxidation deactivation easily under the conditions of high temperature, high gas flow, causes device reliability poor, and will take into full account maintainability, cause whole
Body design is complicated.And the DBDI suitability to sample surfaces ionizing of the bipolar electrode respectively in ion source inside and outside be not good enough, generally
Suitable for liquid sample and the thin layer solid sample of rule, the sample that external ground electrode is difficult to place is not suitable for, for example not
Rule or thick big sample etc., so that limit the range of application of scene, analysis in real time.
The content of the invention
For solving the deficiency in above-mentioned prior art, the invention provides a kind of applied range, simple structure
Novel ion source, realizes the surface ionizing of irregular or thick large sample.
The purpose of the present invention is achieved through the following technical solutions：
A kind of novel ion source, the novel ion source include：
First insulation tube, the first insulation tube both ends open；
Electrode, the electrode are only one, are arranged on the outside of the insulation tube, and the electrode has terminals；
Second insulation tube, second insulation tube are arranged on the outside of first insulation tube and in the non-of the electrode
The sidepiece of the radial direction of the first insulation tube.
According to above-mentioned novel ion source, it is preferable that in the opening away from second insulation tube of the first insulation tube
With internal diametric reduction, sidepiece of the internal diametric reduction in the electrode.
According to above-mentioned novel ion source, alternatively, the novel ion source also includes：
Connector, the connector are used for connecting the electrode and the second insulation tube.
According to above-mentioned novel ion source, it is preferable that it is vacuum to have in second insulation tube in cavity, the cavity
Or filled with gas.
According to above-mentioned novel ion source, it is preferable that first insulation tube includes：
Part I, the Part I are arranged on the inner side of the electrode；
Part II, the Part II are arranged on the inner side of second insulation tube, one end set of the Part I
On the Part II.
The present invention also aims to provide a kind of ioning method, realize the surface of irregular or thick large sample from
Sonization, the goal of the invention are achieved by the following technical programs：
Ioning method, the ioning method are comprised the following steps：
(A1) testing sample is placed in the first opening of the first insulation tube；
(A2) apply AC or DC voltage on electrode, the electrode is only one, and the electrode is arranged on described first
The outside of insulation tube；Second insulation tube is arranged on the outside of first insulation tube and non-first insulation tube in the electrode
Radial direction sidepiece；
Carrier gas is passed through in from the second opening of first insulation tube to the first insulation tube；
(A3) discharge between the electrode and testing sample, the ionized gas of generation make testing sample surface ionizing.
According to above-mentioned ioning method, it is preferable that the first opening of the insulation tube has internal diametric reduction.
According to above-mentioned ioning method, it is preferable that the flow velocity of the carrier gas is 0.02-10L/min.
According to above-mentioned ioning method, it is preferable that the power of the alternating current is 5-30W, and voltage is 1-20kV, frequency
For 10-1000Hz.
According to above-mentioned ioning method, it is preferable that it is vacuum to have in second insulation tube in cavity, the cavity
Or filled with gas.
Compared with prior art, the device have the advantages that being：
1., by the electric discharge inhibitory action of insulating regions, carrier gas ion is realized, i.e., in the case where ground electrode is lacked
Single electrode design is realized in DBDI ion sources.Which has evaded the interior electrode of ground connection under the conditions of high temperature, high gas flow
Oxidation deactivation risk, improves device reliability；Also the application restricted problem of sample area ground electrode is solved, can be used well
In the surface ionizing of irregular or thick large sample, ionogenic scene, real-time application ability is improve；
2. by the electric discharge inhibitory action of insulating regions, it is to avoid the direction electric discharge outside DBDI high-field electrodes to sample end,
Improve ionized gas formation efficiency and stability；
3. realize that single electrode is designed in DBDI ion sources, simplify structure, beneficial to miniaturization and integrated, be easy to safeguard.
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 according to embodiments of the present invention 1 ionogenic sectional view；
Fig. 2 is according to embodiments of the present invention 2 ionogenic sectional view；
Fig. 3 is the mass spectrum of according to embodiments of the present invention 3 caffeine；
Fig. 4 is the mass spectrum of according to embodiments of the present invention 4 acetaminophen.
Specific embodiment
Fig. 1-4 and following description describe the present invention optional embodiment 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 the modification or replacement from these embodiments 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 present invention in a variety of ways.Thus, the invention is not limited in it is following can
Embodiment is selected, and is only limited by claim and their equivalent.
Embodiment 1：
Fig. 1 schematically illustrates the sectional view in the novel ion source of the embodiment of the present invention, as shown in figure 1, described new
Ion source includes：
First insulation tube 11, the first insulation tube both ends open；First insulation tube is using the insulation such as glass, ceramics
Medium；
Electrode 21, the electrode are only one, are arranged on the outside of first insulation tube, and the electrode has wiring
End；
Second insulation tube 31, second insulation tube are arranged on the outside of first insulation tube and in the electrode
The sidepiece of the radial direction of non-first insulation tube.There is internal diameter to shrink in the opening away from second insulation tube of the first insulation tube
Section 12, sidepiece of the internal diametric reduction in the electrode.
The ioning method of the embodiment of the present invention, i.e., the course of work in above-mentioned novel ion source, the ioning method bag
Include following steps：
(A1) testing sample is placed in the first opening of the first insulation tube；First opening of first insulation tube has
Internal diametric reduction；
(A2) apply AC or DC voltage on electrode, the electrode is only one, and the electrode is arranged on described first
The outside of insulation tube；Second insulation tube is arranged on the outside of first insulation tube and non-first insulation tube in the electrode
Radial direction sidepiece；
Carrier gas is passed through in from the second opening of first insulation tube to the first insulation tube；
Preferably, the flow velocity of the carrier gas is 0.02-10L/min；The power of alternating current is 5-30W, and voltage is 1-20kV,
Frequency is 10-1000Hz.
(A3) discharge between the electrode and testing sample, the ionized gas of generation make testing sample surface ionizing.
Embodiment 2：
Fig. 2 schematically illustrates the sectional view in the novel ion source of the embodiment of the present invention, as shown in Fig. 2 described new
Ion source includes：
First insulation tube, the first insulation tube both ends open；First insulation tube includes Part I 18 and second
Part 19, one end of the Part I 18 are enclosed within one end of the Part II 19；The Part II adopts ceramic material,
To go to heat the carrier gas for passing through as heating element heater；
Electrode 21, the electrode are only one, are arranged on the outside of the first insulation tube (Part I), the electricity
Have terminals；
Second insulation tube 31, second insulation tube are arranged on the outside of first insulation tube and in the electrode
The sidepiece of the radial direction of non-first insulation tube；There is between second insulation tube and the second insulation tube cavity 51, filled with gas or
For vacuum；
First connector 41, first connector are used for connecting the electrode and the second insulation tube, are such as connected by screw thread
Connect；
Second connector 61, second connector is for being fixed on first insulation tube by second insulation tube 31
Part II 19 on the outside of；
Temperature element, the temperature element are arranged on the Part II, for detecting the temperature of the Part II,
And it is sent to control device；The distance of the end of temperature element and the electrode is not less than 0.5cm；
Control device, the control device for according to the output temperature of temperature element go adjust heating power, with realize
Temperature control.
The ioning method of the embodiment of the present invention, i.e., the course of work in above-mentioned novel ion source, the ioning method bag
Include following steps：
(A1) testing sample is placed in the first opening of the first insulation tube；First opening of first insulation tube has
Internal diametric reduction；
(A2) apply AC or DC voltage on electrode, the electrode is only one, and the electrode is arranged on described first
The outside of insulation tube；Second insulation tube is arranged on the outside of first insulation tube and non-first insulation tube in the electrode
Radial direction sidepiece；
Carrier gas is passed through in from the second opening of first insulation tube to the first insulation tube, as the second of heating element heater
The carrier gas for passing through is heated partly, by temperature control so that carrier gas temperature reaches 800 degree；
Preferably, the flow velocity of the carrier gas is 0.02-10L/min；The power of alternating current is 5-30W, and voltage is 1-20kV,
Frequency is 10-1000Hz.
(A3) discharge between the electrode and testing sample, the ionized gas of generation make testing sample surface ionizing.
Embodiment 3：
Application examples of the according to embodiments of the present invention 2 novel ion source and ioning method in caffeine detection.
In the application examples, the Part I of the first insulation tube adopts glass, and Part II is using ceramics；Second insulation tube
Using ceramics；It is 7W to be applied to AC power on electrode, maximum voltage 5kV, frequency 50Hz；Temperature element adopts thermoelectricity
It is even, it is mounted on the Part II, 5 centimetres of top distance electrode.DBDI ion sources and mass spectrographic combination analysis platform is built, is taken
100uL is dissolved in the caffeine standards sample (concentration 100ppb) of methanol and is placed in ion source sample area, and helium as carrier gas, flow is
1.2L/min, the carrier gas temperature after heating are 250 DEG C.In mass spectral results obtain caffeine hydrogenation quasi-molecular ions [M+H]+, m/z values
For 195.09, as shown in figure 3,
Embodiment 4：
Application examples of the according to embodiments of the present invention 1 novel ion source and ioning method in acetaminophen detection.
In the application examples, the first insulation tube and the second insulation tube are using ceramics；The AC power being applied on electrode
For 7W, maximum voltage 5kV, frequency 50Hz；DBDI ion sources and mass spectrographic combination analysis platform is built, paracetamol tablet is taken and is put
In ion source sample area, used as carrier gas, flow is 2.0L/min to helium, and carrier gas temperature is 500 DEG C.Obtain in mass spectral results and flutter heat
The hydrogenation quasi-molecular ions [M+H] of breath pain tablet main constituent acetaminophen+, m/z values are 152.18, and mass spectrum is as shown in Figure 4.
Claims (10)
1. a kind of novel ion source, it is characterised in that：The novel ion source includes：
First insulation tube, the first insulation tube both ends open；
Electrode, the electrode are only one, are arranged on the outside of the insulation tube, and the electrode has terminals；
Second insulation tube, second insulation tube are arranged on the outside of first insulation tube and in non-the first of the electrode
The sidepiece of the radial direction of insulation tube.
2. novel ion source according to claim 1, it is characterised in that：In the first insulation tube away from the described second insulation
The opening of pipe has internal diametric reduction, sidepiece of the internal diametric reduction in the electrode.
3. novel ion source according to claim 1, it is characterised in that：The novel ion source also includes：
Connector, the connector are used for connecting the electrode and the second insulation tube.
4. novel ion source according to claim 1, it is characterised in that：There is in second insulation tube cavity, it is described
For vacuum or filled with gas in cavity.
5. novel ion source according to claim 1, it is characterised in that：First insulation tube includes：
Part I, the Part I are arranged on the inner side of the electrode；
Part II, the Part II are arranged on the inner side of second insulation tube, and one end of the Part I is enclosed within institute
State on Part II.
6. ioning method, the ioning method are comprised the following steps：
（A1）Testing sample is placed in the first opening of the first insulation tube；
（A2）Apply AC or DC voltage on electrode, the electrode is only one, the electrode is arranged on first insulation
The outside of pipe；Second insulation tube is arranged on the footpath of the outside of first insulation tube and non-first insulation tube in the electrode
To sidepiece；
Carrier gas is passed through in from the second opening of first insulation tube to the first insulation tube；
（A3）Discharge between the electrode and testing sample, the ionized gas of generation make testing sample surface ionizing.
7. ioning method according to claim 6, it is characterised in that：First opening of the insulation tube has internal diameter
Contraction section.
8. ioning method according to claim 6, it is characterised in that：The flow velocity of the carrier gas is 0.02-10L/min.
9. ioning method according to claim 6, it is characterised in that：The power of alternating current is 5-30W, and voltage is 1-
20kV, frequency are 10-1000Hz.
10. ioning method according to claim 6, it is characterised in that：There is in second insulation tube cavity, it is described
For vacuum or filled with gas in cavity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510595870.2A CN105097413B (en) | 2015-09-18 | 2015-09-18 | Novel ion source and ionization method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510595870.2A CN105097413B (en) | 2015-09-18 | 2015-09-18 | Novel ion source and ionization method |
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| CN105097413A CN105097413A (en) | 2015-11-25 |
| CN105097413B true CN105097413B (en) | 2017-03-22 |
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| CN106531609A (en) * | 2016-11-10 | 2017-03-22 | 宁波大学 | Ion beam strengthening device and method |
| CN107195528B (en) * | 2017-05-19 | 2019-04-02 | 北京大学 | A kind of multi-functional open type compound ion source and its application method |
| CN108364848A (en) * | 2017-12-31 | 2018-08-03 | 宁波大学 | Portable ion source and its working method |
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| CN201017845Y (en) * | 2007-03-14 | 2008-02-06 | 万京林 | Differential feeding media blocking discharging low-temperature plasma device |
| EP2335270A1 (en) * | 2008-10-03 | 2011-06-22 | National Research Council of Canada | Plasma-based direct sampling of molecules for mass spectrometric analysis |
| JP2010205446A (en) * | 2009-02-27 | 2010-09-16 | Kobe Steel Ltd | Ion source |
| CN102519938B (en) * | 2011-12-13 | 2014-06-25 | 清华大学 | Atomic vapor generation method and device based on dielectric barrier discharge |
| CN102522310A (en) * | 2012-01-06 | 2012-06-27 | 昆山禾信质谱技术有限公司 | Ring dielectric barrier discharge ionization device |
| CN204991649U (en) * | 2015-09-18 | 2016-01-20 | 宁波华仪宁创智能科技有限公司 | Novel ion source |
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Address after: West side of 1st floor, 1st floor, Building A, No. 288 Jingu Middle Road (East), Yinzhou District, Ningbo City, Zhejiang Province, 315000 Patentee after: CHINA INNOVATION INSTRUMENT Co.,Ltd. Country or region after: China Address before: Room 304-311, Building D, Kexin Building, No. 655 Bachelor's Road, Yinzhou District, Ningbo City, Zhejiang Province, 310012 Patentee before: CHINA INNOVATION INSTRUMENT Co.,Ltd. Country or region before: China |