CN105097413A - Novel ion source and ionization method - Google Patents
Novel ion source and ionization method Download PDFInfo
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- CN105097413A CN105097413A CN201510595870.2A CN201510595870A CN105097413A CN 105097413 A CN105097413 A CN 105097413A CN 201510595870 A CN201510595870 A CN 201510595870A CN 105097413 A CN105097413 A CN 105097413A
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- insulated tube
- electrode
- ion source
- novel ion
- openend
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- 238000000752 ionisation method Methods 0.000 title abstract 2
- 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 10
- 150000002500 ions Chemical class 0.000 description 38
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 5
- 229960005489 paracetamol Drugs 0.000 description 5
- 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
- 238000013461 design Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000001788 irregular Effects 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
- 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
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000009849 deactivation 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
- -1 and flow is 2.0L/min Substances 0.000 description 1
- 230000004888 barrier function 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
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000010223 real-time analysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- 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, particularly ion source and ioning method.
Background technology
Mass-spectrometric technique is the sensitiveest known and one of analytical method that range of application is the widest at present.In mass-spectrometric technique, ion source is the Primary Component of sample ionization technology.
At present, there is different kinds of ions source, 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), atmosphere pressure chemical ion source (APCI) etc.For these ion sources, sample must through loaded down with trivial details preliminary treatment before ionization, therefore, these ionogenic common deficiencies are: sample can not the directly attached ionization of fast desorption, also namely cannot continuous, the Real-Time Monitoring of realize target component and high throughput analysis or imaging analysis.
In recent years, desorption electro-spray ionization (DESI), Direct Analysis in Real Time (DART) ionization and dielectric barrier discharge (DBDI) ionogenic appearance, these Ionization mode all can direct rapid analysis under sample surfaces realizes normal pressure, and sample is without the need to preliminary treatment.These ion sources have deficiency, as:
DESI ion source, needs high voltage source to build high-voltage electrostatic field, makes electron spray capillary front end easily corona occur, and high pressure also limit and ion source is developed into hand-held and direct possibility human skin being done to harmless rapid analysis; The ionizing solvent used and the gas of high flow rate, not only cost is high but also can cause certain pollution to environment.
DART ion source, eliminate solvent, but need the ionized gas of high-tension electricity and high flow rate, and in order to obtain stable, efficient ionising effect, need to use electrode, right multi-electrode (high-field electrode, gate electrode, grounding electrode) design is complicated, should not realize the miniaturization of instrument.
DBDI ion source, in the DBDI of ion source positioned inside bipolar electrode, interior electrode is especially bar-shaped, needle electrode very easily oxidation deactivation under high temperature, high gas flow condition, causes device reliability poor, and will take into full account maintainability, causes global design complicated.And the DBDI of bipolar electrode respectively in ion source inside and outside is not good enough to the Ionized applicability of sample surfaces, usually the thin layer solid sample of liquid sample Sum fanction is applicable to, be not suitable for the sample that external ground electrode is difficult to place, such as irregular or thick large sample etc., thus limit the range of application of scene, real-time analysis.
Summary of the invention
For solving the deficiency in above-mentioned prior art, the invention provides a kind of applied range, the simple Novel ion source of structure, achieving the surface ionizing of irregular or thick large sample.
The object of the invention is to be achieved through the following technical solutions:
A kind of Novel ion source, described Novel ion source comprises:
First insulated tube, described first insulated tube both ends open;
Electrode, described electrode is only one, is arranged on the outside of described insulated tube, and described electrode has terminals;
Second insulated tube, described second insulated tube is arranged on the described first outside of insulating and is in the sidepiece of the radial direction of non-first insulated tube of described electrode.
According to above-mentioned Novel ion source, preferably, have internal diametric reduction at the openend away from described second insulated tube of the first insulated tube, described internal diametric reduction is in the sidepiece of described electrode.
According to above-mentioned Novel ion source, alternatively, described Novel ion source also comprises:
Connector, described connector is for connecting described electrode and the second insulated tube.
According to above-mentioned Novel ion source, preferably, in described second insulated tube, there is cavity, for vacuum or be filled with gas in described cavity.
According to above-mentioned Novel ion source, preferably, described first insulated tube comprises:
Part I, described Part I is arranged on the inner side of described electrode;
Part II, described Part II is arranged on the inner side of described second insulated tube, and one end of described Part I is enclosed within described Part II.
The present invention also aims to provide a kind of ioning method, achieve the surface ionizing of irregular or thick large sample, this goal of the invention is achieved by the following technical programs:
Ioning method, described ioning method comprises the following steps:
(A1) testing sample is placed in the first openend of the first insulated tube;
(A2) electrode applies exchange or direct voltage, described electrode is only one, and described electrode is arranged on the outside of described first insulated tube; Second insulated tube is arranged on the described first outside of insulating and is in the sidepiece of the radial direction of non-first insulated tube of described electrode;
In the first insulated tube, carrier gas is passed into from the second openend of described first insulated tube;
(A3) discharge between described electrode and testing sample, the ionized gas of generation makes testing sample surface ionizing.
According to above-mentioned ioning method, preferably, the first openend of described insulated tube has internal diametric reduction.
According to above-mentioned ioning method, preferably, the flow velocity of described carrier gas is 0.02-10L/min.
According to above-mentioned ioning method, preferably, the power of described alternating current is 5-30W, and voltage is 1-20kV, and frequency is 10-1000Hz.
According to above-mentioned ioning method, preferably, in described second insulated tube, there is cavity, for vacuum or be filled with gas in described cavity.
Compared with prior art, the beneficial effect that the present invention has is:
1. by the electric discharge inhibitory action of insulating regions, realizing carrier gas ion when lacking grounding electrode, in DBDI ion source, namely achieving single electrode design.Namely which has evaded the oxidation deactivation risk of electrode under high temperature, high gas flow condition in ground connection, improves device reliability; Also solve the application restricted problem of sample area grounding electrode, the surface ionizing of irregular or thick large sample can be performed well in, improve ionogenic scene, in real time application power;
2., by the electric discharge inhibitory action of insulating regions, avoid DBDI high-field electrode to the direction electric discharge outside sample end, improve ionized gas formation efficiency and stability;
3. in DBDI ion source, realize single electrode design, simplified structure, be beneficial to miniaturized and integrated, be convenient to safeguard.
Accompanying drawing explanation
With reference to accompanying drawing, disclosure of the present invention will be easier to understand.Those skilled in the art it is easily understood that: these accompanying drawings only for illustrating technical scheme of the present invention, and and are not intended to be construed as limiting protection scope of the present invention.In figure:
Fig. 1 is the ionogenic cutaway view according to the embodiment of the present invention 1;
Fig. 2 is the ionogenic cutaway view according to the embodiment of the present invention 2;
Fig. 3 is the mass spectrogram of the caffeine according to the embodiment of the present invention 3;
Fig. 4 is the mass spectrogram of the paracetamol according to the embodiment of the present invention 4.
Embodiment
Fig. 1-4 and following description describe Alternate embodiments of the present invention and how to implement to instruct those skilled in the art and to reproduce the present invention.In order to instruct technical solution of the present invention, simplifying or having eliminated some conventional aspects.Those skilled in the art should understand that the modification that is derived from these execution modes or replace will within the scope of the invention.Those skilled in the art should understand that following characteristics can combine to form multiple modification of the present invention in every way.Thus, the present invention is not limited to following Alternate embodiments, and only by claim and their equivalents.
Embodiment 1:
Fig. 1 schematically illustrates the cutaway view in the Novel ion source of the embodiment of the present invention, and as shown in Figure 1, described Novel ion source comprises:
First insulated tube 11, described first insulated tube both ends open; Described first insulation adopts the dielectric such as glass, pottery;
Electrode 21, described electrode is only one, and be arranged on the outside of described first insulated tube, described electrode has terminals;
Second insulated tube 31, described second insulated tube is arranged on the described first outside of insulating and is in the sidepiece of the radial direction of non-first insulated tube of described electrode.Have internal diametric reduction 12 at the openend away from described second insulated tube of the first insulated tube, described internal diametric reduction is in the sidepiece of described electrode.
The ioning method of the embodiment of the present invention, the i.e. course of work in above-mentioned Novel ion source, described ioning method comprises the following steps:
(A1) testing sample is placed in the first openend of the first insulated tube; First openend of described first insulated tube has internal diametric reduction;
(A2) electrode applies exchange or direct voltage, described electrode is only one, and described electrode is arranged on the outside of described first insulated tube; Second insulated tube is arranged on the described first outside of insulating and is in the sidepiece of the radial direction of non-first insulated tube of described electrode;
In the first insulated tube, carrier gas is passed into from the second openend of described first insulated tube;
Preferably, the flow velocity of described carrier gas is 0.02-10L/min; The power of alternating current is 5-30W, and voltage is 1-20kV, and frequency is 10-1000Hz.
(A3) discharge between described electrode and testing sample, the ionized gas of generation makes testing sample surface ionizing.
Embodiment 2:
Fig. 2 schematically illustrates the cutaway view in the Novel ion source of the embodiment of the present invention, and as shown in Figure 2, described Novel ion source comprises:
First insulated tube, described first insulated tube both ends open; Described first insulated tube comprises Part I 18 and Part II 19, and one end of described Part I 18 is enclosed within one end of described Part II 19; Described Part II adopts ceramic material, to go the carrier gas be heated by as heating element;
Electrode 21, described electrode is only one, and be arranged on the outside of described first insulated tube (Part I), described electrode has terminals;
Second insulated tube 31, described second insulated tube is arranged on the described first outside of insulating and is in the sidepiece of the radial direction of non-first insulated tube of described electrode; Between described second insulated tube and the second insulated tube, there is cavity 51, be filled with gas or for vacuum;
First connector 41, described first connector for connecting described electrode and the second insulated tube, as being threaded connection;
Second connector 61, described second connector is used for described second insulated tube 31 to be fixed on outside the Part II 19 of described first insulated tube;
Temperature element, described temperature element is arranged on described Part II, for detecting the temperature of described Part II, and is sent to control device; The end of temperature element and the distance of described electrode are not less than 0.5cm;
Control device, described control device is used for going to adjust heating power, to realize temperature control according to the output temperature of temperature element.
The ioning method of the embodiment of the present invention, the i.e. course of work in above-mentioned Novel ion source, described ioning method comprises the following steps:
(A1) testing sample is placed in the first openend of the first insulated tube; First openend of described first insulated tube has internal diametric reduction;
(A2) electrode applies exchange or direct voltage, described electrode is only one, and described electrode is arranged on the outside of described first insulated tube; Second insulated tube is arranged on the described first outside of insulating and is in the sidepiece of the radial direction of non-first insulated tube of described electrode;
In the first insulated tube, pass into carrier gas from the second openend of described first insulated tube, the carrier gas that the Part II as heating element is heated by, make carrier gas temperature reach 800 degree by temperature control;
Preferably, the flow velocity of described carrier gas is 0.02-10L/min; The power of alternating current is 5-30W, and voltage is 1-20kV, and frequency is 10-1000Hz.
(A3) discharge between described electrode and testing sample, the ionized gas of generation makes testing sample surface ionizing.
Embodiment 3:
According to Novel ion source and the application examples of ioning method in caffeine detects of the embodiment of the present invention 2.
In this application examples, the Part I of the first insulated tube adopts glass, and Part II adopts pottery; Second insulated tube adopts pottery; The AC power be applied on electrode is 7W, maximum voltage 5kV, frequency 50Hz; Temperature element adopts thermocouple, is contained on described Part II, top distance electrode 5 centimetres.Build DBDI ion source and mass spectrographic combination analysis platform, get the caffeine standards sample (concentration 100ppb) that 100uL is dissolved in methyl alcohol and be placed in ion source sample district, helium is as carrier gas, and flow is 1.2L/min, and the carrier gas temperature after heating is 250 DEG C.Obtain in mass spectral results the hydrogenation quasi-molecular ions [M+H] of caffeine+, m/z value is 195.09, as shown in Figure 3,
Embodiment 4:
According to Novel ion source and the application examples of ioning method in paracetamol detects of the embodiment of the present invention 1.
In this application examples, the first insulated tube and the second insulated tube adopt pottery; The AC power be applied on electrode is 7W, maximum voltage 5kV, frequency 50Hz; Build DBDI ion source and mass spectrographic combination analysis platform, get paracetamol tablet and be placed in ion source sample district, helium is as carrier gas, and flow is 2.0L/min, and carrier gas temperature is 500 DEG C.Obtain in mass spectral results the hydrogenation quasi-molecular ions [M+H] of paracetamol tablet principal component paracetamol+, m/z value is 152.18, and mass spectrogram is as shown in Figure 4.
Claims (10)
1. a Novel ion source, is characterized in that: described Novel ion source comprises:
First insulated tube, described first insulated tube both ends open;
Electrode, described electrode is only one, is arranged on the outside of described insulated tube, and described electrode has terminals;
Second insulated tube, described second insulated tube is arranged on the described first outside of insulating and is in the sidepiece of the radial direction of non-first insulated tube of described electrode.
2. Novel ion source according to claim 1, is characterized in that: have internal diametric reduction at the openend away from described second insulated tube of the first insulated tube, described internal diametric reduction is in the sidepiece of described electrode.
3. Novel ion source according to claim 1, is characterized in that: described Novel ion source also comprises:
Connector, described connector is for connecting described electrode and the second insulated tube.
4. Novel ion source according to claim 1, is characterized in that: have cavity in described second insulated tube, for vacuum or be filled with gas in described cavity.
5. Novel ion source according to claim 1, is characterized in that: described first insulated tube comprises:
Part I, described Part I is arranged on the inner side of described electrode;
Part II, described Part II is arranged on the inner side of described second insulated tube, and one end of described Part I is enclosed within described Part II.
6. ioning method, described ioning method comprises the following steps:
(A1) testing sample is placed in the first openend of the first insulated tube;
(A2) electrode applies exchange or direct voltage, described electrode is only one, and described electrode is arranged on the outside of described first insulated tube; Second insulated tube is arranged on the described first outside of insulating and is in the sidepiece of the radial direction of non-first insulated tube of described electrode;
In the first insulated tube, carrier gas is passed into from the second openend of described first insulated tube;
(A3) discharge between described electrode and testing sample, the ionized gas of generation makes testing sample surface ionizing.
7. ioning method according to claim 6, is characterized in that: the first openend of described insulated tube has internal diametric reduction.
8. ioning method according to claim 6, is characterized in that: the flow velocity of described carrier gas is 0.02-10L/min.
9. ioning method according to claim 6, is characterized in that: the power of alternating current is 5-30W, and voltage is 1-20kV, and frequency is 10-1000Hz.
10. ioning method according to claim 6, is characterized in that: have cavity in described second insulated tube, for vacuum or be filled with gas in described 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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| Publication Number | Publication Date |
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| CN105097413A true CN105097413A (en) | 2015-11-25 |
| CN105097413B CN105097413B (en) | 2017-03-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106531609A (en) * | 2016-11-10 | 2017-03-22 | 宁波大学 | Ion beam strengthening device and method |
| CN107195528A (en) * | 2017-05-19 | 2017-09-22 | 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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| 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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2015
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Patent Citations (6)
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| CN201017845Y (en) * | 2007-03-14 | 2008-02-06 | 万京林 | Differential feeding media blocking discharging low-temperature plasma device |
| WO2010037238A1 (en) * | 2008-10-03 | 2010-04-08 | 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 |
| CN102519938A (en) * | 2011-12-13 | 2012-06-27 | 清华大学 | Atomic vapor generation method and device based on dielectric barrier discharge |
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| CN106531609A (en) * | 2016-11-10 | 2017-03-22 | 宁波大学 | Ion beam strengthening device and method |
| CN107195528A (en) * | 2017-05-19 | 2017-09-22 | 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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| CN105097413B (en) | 2017-03-22 |
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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 |