CN104733280B - A kind of orthogonal ion source apparatus - Google Patents
A kind of orthogonal ion source apparatus Download PDFInfo
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- CN104733280B CN104733280B CN201510172131.2A CN201510172131A CN104733280B CN 104733280 B CN104733280 B CN 104733280B CN 201510172131 A CN201510172131 A CN 201510172131A CN 104733280 B CN104733280 B CN 104733280B
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- ion
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- tungsten filament
- heating tungsten
- direct injected
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Abstract
The invention discloses a kind of orthogonal ion source apparatus, comprise three-dimensional chamber and the ion lens group being positioned at its outside; Three-dimensional chamber comprises ion repeller, thermionic emission filament, electronics reception trap, direct injected pipe and sample heating tungsten filament; Ion lens group comprises Ion Extraction pole, ion focusing pole, ion intensifying ring and ion outlet; In chamber X-direction, ion repeller, sample heating tungsten filament and ion lens group are on the same line; In chamber Y direction, it is just right that thermionic emission filament, electronics receive trap; In chamber Z-direction, sample feeding pipe is just right with heating tungsten filament.Apparatus of the present invention realize liquid towards sample direct injected, and heating tungsten filament carries out electronics bombardment to while adsorption sample heating, by controlling heating tungsten filament electric current, reduce ambient interferences.Mainly single charge ion that Ionization mode of the present invention produces, energy spread is few, and spectral line is simple, is applicable to the fast ionic of metallic element in the water body of difficult volatilization.
Description
Technical field
The invention belongs to ion source field, be specifically related to a kind of orthogonal ion source apparatus, be applicable to the fast ionic of metallic element in water body.
Background technology
Ion source is that the molecule of centering or atom carry out ionization, and draws a kind of device of ion.Ionogenic performance determines Ionization Efficiency, and then determines mass spectrometric sensitivity to a great extent.At present, common several ion sources have: electron-bombardment-type ion source, inductively coupled plasma ion source, chemical ionization source, fast atom bombardment source, atmospheric pressure ionization source, field-ionization source and field desorption ionization source etc.
In current water body, the detection of metallic element uses icp ms usually, and this instrument adopts inductively coupled plasma ion source to carry out ionization; But ICP-MS, due to comparatively large by extraneous factor interference effects such as carrier gas stream, interface effect, matrix effects, can only be suitable for carrying out in the lab, on the small spectrometer device of inapplicable Site Detection.Traditional electronics bombardment (EI) ion source is only applicable to gas, low-boiling compound fast ionic, is not suitable for the ionization of metallic compound in water body.
At present, be badly in need of wanting a kind of little by ectocine, can sample introduction at ambient pressure, may be used on the small spectrometer device of Site Detection.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, and a kind of small-sized orthogonal ion source apparatus being applicable to Site Detection is provided, this device realizes ionization to carrying out electronics bombardment while sample heating, achieves the efficient ionization of metallic compound; Meanwhile, device can sample introduction at ambient pressure, can realize on-the-spot to water body direct ion, reduce external interference.
The present invention is achieved through the following technical solutions:
A kind of orthogonal ion source apparatus, comprises three-dimensional chamber and ion lens group; Described three-dimensional chamber comprises ion repeller, thermionic emission filament, electronics reception trap, direct injected pipe and sample heating tungsten filament; It is outside that described ion lens group is positioned at three-dimensional chamber, comprises Ion Extraction pole, ion focusing pole, ion intensifying ring and ion outlet; The X-direction of three-dimensional chamber, ion repeller, sample heating tungsten filament and ion lens group are on the same line; The Y direction of three-dimensional chamber, it is just right that thermionic emission filament, electronics receive trap; The Z-direction of three-dimensional chamber, it is just right that direct injected pipe and sample heat tungsten filament.
Further, described sample heating tungsten filament is positioned at the center of three-dimensional chamber inside.
Further, it is inner that described ion repeller is positioned at three-dimensional chamber, and thermionic emission filament, electronics receive trap and be positioned at three-dimensional chamber outside.
Further, in three-dimensional chamber Z-direction, direct injected pipe connects bellows outward, controls the position of direct injected pipe.
Further, described direct injected pipe is in three-dimensional chamber Z-direction during sample introduction, and direct injected pipe protracts in three-dimensional chamber, apart from sample heating tungsten filament 1-2mm.
Further, described direct injected pipe after in three-dimensional chamber Z-direction, sample introduction completes, moves after sample feeding pipe away from sample heating tungsten filament.
Further, in above-mentioned ion source device ionization process, the sample being attached to sample heating tungsten filament is heated, and is subject to electronics bombardment simultaneously.
The present invention also provides a kind of method using above-mentioned orthogonal ion source apparatus to carry out bombarding electronics: comprise the following steps:
(1) under ion source device is in vacuum state, testing sample is incorporated on sample heating tungsten filament by direct injected pipe under vacuum conditions, is gathered in rapidly on heating tungsten filament owing to being in vacuum environment sample;
(2) after sample is introduced, away from sample heating tungsten filament under the effect of direct injected pipe external force, on heating tungsten filament, apply electric current subsequently, sample is heated, while heating, carry out ionization by the mode of electronics bombardment;
(3) enter in mass analyzer through ion outlet through the ion beam of being drawn by Ion Extraction pole, ion focusing pole focuses on, ion intensifying ring is formed after accelerating after sample ionization.
Ion source device of the present invention, mainly for liquid direct injected, in ionization process, the sample of sample heating tungsten filament to absorption directly heats, and carries out electronics bombardment simultaneously; By controlling heating tungsten filament electric current, reduce ambient interferences.Mainly single charge ion that Ionization mode of the present invention produces, energy spread is few, and spectral line is simple, is applicable to the fast ionic of metallic element in the water body of difficult volatilization.
Accompanying drawing explanation
Fig. 1, ion source device xy section plan of the present invention;
Cutaway view under Fig. 2, ion source device xz plane sample introduction state of the present invention;
Cutaway view under Fig. 3, ion source device xz plane electronics bombardment state of the present invention;
Cutaway view under Fig. 4, ion source device yz plane sample introduction state of the present invention;
Cutaway view under Fig. 5, ion source device yz plane electronics bombardment state of the present invention;
Fig. 6, embodiment of the present invention cation movement locus simulation drawing
Wherein: 1, ion repeller; 2, thermionic emission filament; 3, electronics receives trap; 4, three-dimensional chamber; 5, Ion Extraction pole; 6, ion focusing pole; 7, ion intensifying ring; 8, ion outlet; 9, direct injected pipe; 10, sample heating tungsten filament; 11, bellows.
Embodiment
Below in conjunction with accompanying drawing, ion source device of the present invention is specifically described:
A kind of orthogonal ion source apparatus, comprises three-dimensional chamber 4 and the ion lens group being positioned at its outside, and three-dimensional chamber comprises ion repeller 1, thermionic emission filament 2, electronics reception trap 3, direct injected pipe 9 and sample heating tungsten filament 10; Ion lens group comprises Ion Extraction pole 5, ion focusing pole 6, ion intensifying ring 7 and ion outlet 8; Sample heating tungsten filament is positioned at the center of three-dimensional chamber inside, and it is inner that ion repeller is positioned at three-dimensional chamber, and thermionic emission filament, electronics receive trap and be positioned at three-dimensional chamber outside.
Ion source device XY section plan as shown in Figure 1, in the X-direction of three-dimensional chamber, ion repeller 1, sample heating tungsten filament 10, Ion Extraction pole 5, ion focusing pole 6, ion intensifying ring 7 and ion outlet 8 are located along the same line; In the Y direction of three-dimensional chamber, it is just right that thermionic emission filament 2, electronics receive trap 3, and middle is sample heating tungsten filament 10.
Ion source device XZ section plan as shown in Figure 2, in the Z-direction of three-dimensional chamber, it is just right that direct injected pipe 9 and sample heat tungsten filament 10, and direct injected pipe 9 is outer connects bellows 11, controls the position of direct injected pipe.During sample introduction, direct injected pipe castor sample heating tungsten filament 1-2mm, after sample introduction completes, moves after sample feeding pipe away from sample heating tungsten filament (as shown in Figure 3).On heating tungsten filament, apply electric current subsequently, sample is heated, carrying out ionization by the mode of electronics bombardment while heating, being introduced in mass analyzer through forming ion beam by ion repeller, extraction pole, focusing electrode and intensifying ring after sample ionization.Fig. 4 is cutaway view under ion source yz plane sample introduction state of the present invention, and Fig. 5 is cutaway view under ion source yz plane electronics bombardment state of the present invention.
The present invention also provides a kind of method using above-mentioned orthogonal ion source apparatus to carry out bombarding electronics: comprise the following steps:
(1), under ion source device is in vacuum state, testing sample is incorporated on sample heating tungsten filament by direct injected pipe under vacuum conditions, is gathered in rapidly on heating tungsten filament owing to being in vacuum environment sample;
(2), sample introduce after, under the effect of direct injected pipe external force away from sample heating tungsten filament, subsequently heating tungsten filament on apply electric current, sample is heated, while heating with electronics bombardment mode carry out ionization;
(3) enter in mass analyzer through ion outlet through the ion beam of being drawn by Ion Extraction pole, ion focusing pole focuses on, ion intensifying ring is formed after accelerating after sample ionization.
Below in conjunction with embodiment, apparatus of the present invention and method are specifically described:
Embodiment 1:
Get the aqueous solution that 25 μ L contain heavy metal element, be connected on direct injected pipe 9 by sampling valve.Start mass spectrometric vacuum system, when vacuum system reaches 1.0 × 10
-4pa, direct injected pipe 9 moves forward to sample heating tungsten filament 10, and during apart from sample heating tungsten filament 1-2mm, rapid opening and closing (being about 0.5s) is connected in the sampling valve outside direct injected pipe 9, under negative pressure of vacuum effect, complete sample introduction.After sample introduction completes, move after direct injected pipe 9 away from sample heating tungsten filament.Vacuum system is run all the time, when being stabilized in 1.0 × 10
-4during Pa, sample heating tungsten filament 10 applies electric current and heats, while sample heating, thermionic emission filament 2 electron emission, sample on bombardment sample heating tungsten filament 10 carries out ionization, through being formed ion beam and entered mass analyzer by ion repeller 1, Ion Extraction pole 5, ion focusing pole 6, ion intensifying ring 7 through ion outlet 8 after sample ionization.
Fig. 6 is the ion motion trace simulation drawing (simulation of Simion electrostatic lens analysis software) after embodiment of the present invention ionization, wherein ion repeller 1 for diameter be 20mm, thickness is 2mm stainless steel substrates.It is 34mm that Ion Extraction pole 5, ion focusing pole 6, ion intensifying ring 7 are respectively diameter, and thickness is 2mm stainless steel substrates, and middle circle bore dia is 4mm.Ion outlet 8 for diameter be 32mm, thickness is 2mm stainless steel substrates, and middle circle bore dia is 2mm.Ion repeller 1 applies voltage 100v, and Ion Extraction pole 5 applies voltage-50v, and ion focusing pole 6 applies voltage 0v and ion intensifying ring 7 applies voltage-100v.
Claims (6)
1. an orthogonal ion source apparatus, comprises three-dimensional chamber (4) and ion lens group; It is characterized in that, described three-dimensional chamber comprises ion repeller (1), thermionic emission filament (2), electronics reception trap (3), direct injected pipe (9) and sample heating tungsten filament (10); It is outside that described ion lens group is positioned at three-dimensional chamber, comprises Ion Extraction pole (5), ion focusing pole (6), ion intensifying ring (7) and ion outlet (8); The X-direction of three-dimensional chamber, ion repeller, sample heating tungsten filament and ion lens group are on the same line; The Y direction of three-dimensional chamber, it is just right that thermionic emission filament, electronics receive trap; The Z-direction of three-dimensional chamber, it is just right that direct injected pipe and sample heat tungsten filament; Described sample heating tungsten filament (10) is positioned at the inner center of three-dimensional chamber (1), it is inner that ion repeller (1) is positioned at three-dimensional chamber (4), and thermionic emission filament (2), electronics receive trap (3) and be positioned at three-dimensional chamber outside.
2. device according to claim 1, is characterized in that, in three-dimensional chamber (4) Z-direction, direct injected pipe (9) connects bellows (11) outward, controls the position of direct injected pipe.
3. device according to claim 1, is characterized in that, described direct injected pipe (9) is in three-dimensional chamber (4) Z-direction during sample introduction, and direct injected pipe protracts to sample heating tungsten filament, and distance is 1-2mm.
4. device according to claim 1, is characterized in that, described direct injected pipe (9) after in three-dimensional chamber (4) Z-direction, sample introduction completes, moves after sample feeding pipe away from sample heating tungsten filament (10).
5. device according to claim 1, is characterized in that, in above-mentioned ion source device ionization process, the sample being attached to sample heating tungsten filament (10) is heated, and vertical direction applies electronics bombardment.
6. use orthogonal ion source apparatus described in any one of claim 1-5 to carry out a method for bombarding ion, it is characterized in that, comprise the following steps:
(1), under ion source device is in vacuum state, testing sample is incorporated on sample heating tungsten filament (10) by direct injected pipe (9) under vacuum conditions, is gathered in rapidly on heating tungsten filament owing to being in vacuum environment sample;
(2), sample introduce after, under the effect of direct injected pipe external force away from sample heating tungsten filament, subsequently heating tungsten filament on apply electric current, sample is heated, while heating with electronics bombardment mode carry out ionization;
(3) enter in mass analyzer through ion outlet (8) through the ion beam of being drawn by Ion Extraction pole (5), ion focusing pole (6) focus on, ion intensifying ring (7) is formed after accelerating after sample ionization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510172131.2A CN104733280B (en) | 2015-04-13 | 2015-04-13 | A kind of orthogonal ion source apparatus |
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| CN201510172131.2A CN104733280B (en) | 2015-04-13 | 2015-04-13 | A kind of orthogonal ion source apparatus |
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| CN104733280A CN104733280A (en) | 2015-06-24 |
| CN104733280B true CN104733280B (en) | 2016-03-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107470991B (en) * | 2017-09-13 | 2019-02-12 | 成都睿坤科技有限公司 | A kind of high stability ion beam polishing device |
| CN111081529B (en) * | 2019-12-31 | 2023-08-15 | 四川红华实业有限公司 | Electron bombardment type ion source with double-filament structure and double-filament working method thereof |
| CN112700903A (en) * | 2020-12-28 | 2021-04-23 | 中国科学技术大学 | Cold atom and ion velocity imaging composite detection system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2012024468A2 (en) * | 2010-08-19 | 2012-02-23 | Leco Corporation | Time-of-flight mass spectrometer with accumulating electron impact ion source |
| CN102299038B (en) * | 2011-07-21 | 2013-07-24 | 厦门大学 | Compound ion source |
| CN103295872A (en) * | 2012-03-05 | 2013-09-11 | 北京普析通用仪器有限责任公司 | Compound ion source device and mass spectrometer |
| CN102903597A (en) * | 2012-10-19 | 2013-01-30 | 山东省科学院海洋仪器仪表研究所 | Ion source combining thermal desorption with electron bombardment |
| CN103594326A (en) * | 2013-11-27 | 2014-02-19 | 中国科学院大连化学物理研究所 | Double-ionization ion source |
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