CN104716009A - Composite ionization source based on vacuum ultraviolet light ionization and atmospheric pressure ionization - Google Patents
Composite ionization source based on vacuum ultraviolet light ionization and atmospheric pressure ionization Download PDFInfo
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- CN104716009A CN104716009A CN201310687505.5A CN201310687505A CN104716009A CN 104716009 A CN104716009 A CN 104716009A CN 201310687505 A CN201310687505 A CN 201310687505A CN 104716009 A CN104716009 A CN 104716009A
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Abstract
The invention relates to mass spectrometry instrument, and particularly to a composite ionization source based on vacuum ultraviolet light ionization and atmospheric pressure ionization. The composite ionization source based on vacuum ultraviolet light ionization and atmospheric pressure ionization comprises a vacuum ultraviolet light source, an ionization chamber cavity, an ion funnel and an atmospheric pressure ionization source; a sample gas capillary tube connector, a vacuum gauge connector and a mechanical vacuum pump extraction opening are formed in the wall of the ionization chamber cavity. A direct voltage and a radio-frequency voltage are applied to the ion funnel, so that ions which are not in the axis can be focused on the axis, and the ions are transferred into a mass analyzer below the ion funnel to be analyzed. According to the composite ionization source based on vacuum ultraviolet light ionization and atmospheric pressure ionization, the vacuum ultraviolet light source can ionize polar molecules and nonpolar molecules, the atmospheric pressure ionization source can ionize compounds with the ionization energy higher than the photon energy of vacuum ultraviolet light, and the range of ionizable compounds is widened; in addition, after sample molecules which are not ionized in the atmospheric pressure ionization source enter the ionization chamber cavity, secondary ionization can be conducted on the sample molecules through the vacuum ultraviolet light, and the ionization efficiency and the detection sensitivity are improved.
Description
Technical field
The present invention relates to mass spectrometer, a kind of based on vacuum ultraviolet ionized and composite ionization source that is atmospheric pressure ionization specifically.Vacuum ultraviolet ionized ionizable polarity and nonpolar molecule in the composite ionization source of the present invention's design, and the ionizable ionization energy of atmospheric pressure ionization source is higher than the compound of vacuum-ultraviolet light photon energy, has widened the scope of ionizable compound; Further, double ionization can be carried out by vacuum-ultraviolet light after the sample molecule be not ionized in atmospheric pressure ionization source enters ionization chamber cavity, improve ionizing efficiency and detection sensitivity.
Background technology
In recent years, develop multiple atmospheric pressure ionization source, as low temperature plasma ionization source (LTP), electron spray ionisation source (ESI), surface acoustic wave atomization ionization source (SAWN), resolve electron spray ionisation source (DESI), atmosphere pressure chemical ion source (APCI), dielectric barrier discharge ionization source (DBDI) or direct real-time analysis (DART) ionization source etc.These atmospheric pressure ionization sources have many merits, comprise efficient, soft ionization, structure simple, without the need to the sample pre-treatments of complexity, directly carry out ionization analysis etc. to complex sample.But these atmospheric pressure ionization sources are suitable for ionizing polar molecule, lower to nonpolar molecule ionizing efficiency.
Vacuum ultraviolet ionized is a kind of soft ionization source, mainly produces molecular ion, does not almost have fragment ion, ionizable polarity and nonpolar molecule.But, the optical window material that vacuum ultraviolet light source uses limits the photon energy through light.At present, LiF optical window material is the highest through the photon energy of light, is 11.8eV, effectively can ionize the compound of ionization energy lower than 11.8eV, then helpless higher than the compound of 11.8eV to ionization energy.And the optical density of commercial vacuum UV lamp luminescence is limited, limits vacuum ultraviolet ionized ionizing efficiency to a certain extent.
Thus, the present invention devises a kind of based on vacuum ultraviolet ionized and composite ionization source that is atmospheric pressure ionization.Vacuum ultraviolet ionized ionizable polarity and nonpolar molecule, compensate for the deficiency that atmospheric pressure ionization source is lower to polar molecule ionizing efficiency; And the ionizable ionization energy of atmospheric pressure ionization source is higher than the compound of vacuum-ultraviolet light photon energy, widen the scope of ionizable compound.Further, double ionization can be carried out by vacuum-ultraviolet light after the sample molecule be not ionized in atmospheric pressure ionization source enters ionization chamber cavity, ionizing efficiency and detection sensitivity can be improved.In addition, vacuum ultraviolet ionized and atmospheric pressure ionization is all soft ionization source, and ionized sample produces fragment ion hardly, is very suitable for online qualitative and quantitative analysis.
Summary of the invention
The object of the present invention is to provide a kind of based on vacuum ultraviolet ionized and composite ionization source that is atmospheric pressure ionization.
For achieving the above object, the technical solution used in the present invention is:
A kind of based on vacuum ultraviolet ionized and composite ionization source that is atmospheric pressure ionization, comprise vacuum ultraviolet light source, ionization chamber cavity, ion funnel and atmospheric pressure ionization source, on ionization chamber cavity wall, be provided with sample gas capillary interface, vacuum gauge interface and oil-sealed rotary pump bleeding point;
Ion funnel is placed in ionization chamber inside cavity, and ion funnel is applied with direct voltage and radio-frequency voltage;
Directly over ion funnel, the ionization chamber cavity wall at place is provided with ultraviolet light entrance, and ultraviolet light entrance is coaxial with ion funnel;
Sample gas capillary enters ionization chamber inside by the sample gas capillary interface on ionization chamber cavity wall; The axis of sample gas capillary and the axis being parallel of ion funnel; The gas vent of sample gas capillary is positioned at the electrode slice through hole of ion funnel;
The near gas inlets of sample gas capillary is provided with atmospheric pressure ionization source.
Ion funnel is applied with direct voltage and radio-frequency voltage, can by the ion focusing not on axis on axis, the mass analyzer transferred to below ion funnel is analyzed;
Described mass analyzer is time of flight mass analyzer, level Four bar mass analyzer, ion strap mass analyzer, sector magnetic field mass analyzer or ion cyclotron resonance mass analyzer.
Atmospheric pressure ionization source is low temperature plasma ionization source, electron spray ionisation source, surface acoustic wave atomization ionization source, parsing electron spray ionisation source, atmosphere pressure chemical ion source, dielectric barrier discharge ionization source or direct real-time analysis (DART) ionization source.
Vacuum ultraviolet light source is gas-discharge light source, LASER Light Source or synchrotron radiation light source.
Sample is by sample gas capillary sample inlet;
Vacuum gauge interface is connected with vacuum gauge, and oil-sealed rotary pump bleeding point is connected with oil-sealed rotary pump through control valve; Ionization chamber vacuum degree is controlled by oil-sealed rotary pump and control valve, and vacuum degree maintains between 0.01Torr to 30Torr.
Beneficial effect of the present invention is: vacuum ultraviolet ionized ionizable polarity and nonpolar molecule in the composite ionization source of the present invention's design, and the ionizable ionization energy of atmospheric pressure ionization source is higher than the compound of vacuum-ultraviolet light photon energy, widen the scope of ionizable compound; Further, double ionization can be carried out by vacuum-ultraviolet light after the sample molecule be not ionized in atmospheric pressure ionization source enters ionization chamber cavity, improve ionizing efficiency and detection sensitivity.In addition, vacuum ultraviolet ionized and atmospheric pressure ionization is all soft ionization source, and ionized sample produces fragment ion hardly, is very suitable for online qualitative and quantitative analysis.
Accompanying drawing explanation
Fig. 1 is of the present invention based on the vacuum ultraviolet ionized structural representation with the composite ionization source of atmospheric pressure ionization.
Wherein, 1-vacuum ultraviolet light source; 2-ionization chamber cavity; 3-ion funnel; 4-atmospheric pressure ionization source; 5-sample gas capillary; 6-control valve; 7-oil-sealed rotary pump; 8-vacuum gauge; 9-ion strap mass analyzer.
Embodiment
As shown in Figure 1, a kind of based on vacuum ultraviolet ionized and composite ionization source that is atmospheric pressure ionization, comprise vacuum ultraviolet light source 1, ionization chamber cavity 2, ion funnel 3 and atmospheric pressure ionization source 4, on ionization chamber cavity 2 wall, be provided with sample gas capillary 5 interface, vacuum gauge 8 interface and oil-sealed rotary pump 7 bleeding point.
It is inner that ion funnel 3 is placed in ionization chamber cavity 2, and ion funnel 3 is applied with direct voltage and radio-frequency voltage; Ion funnel 3 is made up of 70 thick electrode slices for 0.5mm, and the direct voltage of applying forms the DC electric field of 16V/cm in ion funnel 3, and the radio-frequency voltage frequency of applying is 800kHz, and peak-to-peak value is 70V
p-p; Ion funnel 3 can by the ion focusing not on axis on axis, and the ion strap mass analyzer 9 transferred to below ion funnel 3 is analyzed.
Directly over ion funnel 3, ionization chamber cavity 2 wall at place is provided with ultraviolet light entrance, and ultraviolet light entrance is coaxial with ion funnel 3; Vacuum ultraviolet light source 1 is commercialization Kr lamp, and its photon energy of launching is 10.6eV.
Sample gas capillary 5 enters ionization chamber inside by sample gas capillary 5 interface on ionization chamber cavity 2 wall; The axis of sample gas capillary 5 and the axis being parallel of ion funnel 3; The gas vent of sample gas capillary 5 is positioned at the electrode slice through hole of ion funnel 3; Sample gas capillary 5 selects that internal diameter is 250 μm, length is the metal capillary of 5cm.
The atmospheric pressure ionization source 4 that the near gas inlets of sample gas capillary 5 is arranged is low temperature plasma ionization source (LTP).
Vacuum gauge 8 interface is connected with vacuum gauge 8, and oil-sealed rotary pump 7 bleeding point is connected with oil-sealed rotary pump 7 through control valve 6; Ionization chamber vacuum degree is controlled by oil-sealed rotary pump 7 and control valve 6, maintains 1Torr.
Claims (5)
1. one kind based on vacuum ultraviolet ionized and composite ionization source that is atmospheric pressure ionization, it is characterized in that: comprise vacuum ultraviolet light source (1), ionization chamber cavity (2), ion funnel (3) and atmospheric pressure ionization source (4), on ionization chamber cavity (2) wall, be provided with sample gas capillary (5) interface, vacuum gauge (8) interface and oil-sealed rotary pump (7) bleeding point;
It is inner that ion funnel (3) is placed in ionization chamber cavity (2), and ion funnel (3) is applied with direct voltage and radio-frequency voltage;
Directly over ion funnel (3), ionization chamber cavity (2) wall at place is provided with ultraviolet light entrance, and ultraviolet light entrance is coaxial with ion funnel (3);
Sample gas capillary (5) enters ionization chamber inside by sample gas capillary (5) interface on ionization chamber cavity (2) wall; The axis of sample gas capillary (5) and the axis being parallel of ion funnel (3); The gas vent of sample gas capillary (5) is positioned at the electrode slice through hole of ion funnel (3);
The near gas inlets of sample gas capillary (5) is provided with atmospheric pressure ionization source (4).
2. composite ionization source according to claim 1, is characterized in that:
Ion funnel (3) is applied with direct voltage and radio-frequency voltage, can by the ion focusing not on axis on axis, the mass analyzer (9) transferring to ion funnel (3) below is analyzed;
Described mass analyzer (9) is time of flight mass analyzer, level Four bar mass analyzer, ion strap mass analyzer, sector magnetic field mass analyzer or ion cyclotron resonance mass analyzer.
3. composite ionization source according to claim 1, is characterized in that:
Atmospheric pressure ionization source (4) is low temperature plasma ionization source, electron spray ionisation source, surface acoustic wave atomization ionization source, resolve electron spray ionisation source, atmosphere pressure chemical ion source, dielectric barrier discharge ionization source or direct real-time analysis (DART) ionization source.
4. composite ionization source according to claim 1, is characterized in that:
Vacuum ultraviolet light source (1) is gas-discharge light source, LASER Light Source or synchrotron radiation light source.
5. composite ionization source according to claim 1, is characterized in that:
Sample is by sample gas capillary (5) sample introduction;
Vacuum gauge (8) interface is connected with vacuum gauge (8), and oil-sealed rotary pump (7) bleeding point is connected with oil-sealed rotary pump (7) through control valve (6); Ionization chamber vacuum degree is controlled by oil-sealed rotary pump (7) and control valve (6), and vacuum degree maintains between 0.01Torr to 30Torr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310687505.5A CN104716009A (en) | 2013-12-13 | 2013-12-13 | Composite ionization source based on vacuum ultraviolet light ionization and atmospheric pressure ionization |
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| CN201310687505.5A CN104716009A (en) | 2013-12-13 | 2013-12-13 | Composite ionization source based on vacuum ultraviolet light ionization and atmospheric pressure ionization |
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| CN104716009A true CN104716009A (en) | 2015-06-17 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106449349A (en) * | 2016-10-26 | 2017-02-22 | 上海大学 | Compound ion source based on low temperature plasma discharge |
| CN110648898A (en) * | 2019-08-16 | 2020-01-03 | 上海裕达实业有限公司 | Mass spectrum device and method for detecting multi-component gas in freeze-drying process |
| CN111223749A (en) * | 2018-11-25 | 2020-06-02 | 中国科学院大连化学物理研究所 | Photo-ionization source device for improving sensitivity of mass spectrum |
| CN111653470A (en) * | 2020-05-25 | 2020-09-11 | 清华大学深圳国际研究生院 | Ultraviolet lamp ionization source |
| CN112908828A (en) * | 2019-12-04 | 2021-06-04 | 中国科学院大连化学物理研究所 | Composite ionization source for surface acoustic wave ionization and atmospheric pressure photoionization for liquid sample detection |
-
2013
- 2013-12-13 CN CN201310687505.5A patent/CN104716009A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106449349A (en) * | 2016-10-26 | 2017-02-22 | 上海大学 | Compound ion source based on low temperature plasma discharge |
| CN106449349B (en) * | 2016-10-26 | 2018-04-27 | 上海大学 | Compound ion source based on discharge of plasma in low temperature |
| CN111223749A (en) * | 2018-11-25 | 2020-06-02 | 中国科学院大连化学物理研究所 | Photo-ionization source device for improving sensitivity of mass spectrum |
| CN111223749B (en) * | 2018-11-25 | 2021-01-26 | 中国科学院大连化学物理研究所 | Photo-ionization source device for improving sensitivity of mass spectrum |
| CN110648898A (en) * | 2019-08-16 | 2020-01-03 | 上海裕达实业有限公司 | Mass spectrum device and method for detecting multi-component gas in freeze-drying process |
| CN112908828A (en) * | 2019-12-04 | 2021-06-04 | 中国科学院大连化学物理研究所 | Composite ionization source for surface acoustic wave ionization and atmospheric pressure photoionization for liquid sample detection |
| CN112908828B (en) * | 2019-12-04 | 2022-05-17 | 中国科学院大连化学物理研究所 | Composite ionization source for surface acoustic wave ionization and atmospheric pressure photoionization for liquid sample detection |
| CN111653470A (en) * | 2020-05-25 | 2020-09-11 | 清华大学深圳国际研究生院 | Ultraviolet lamp ionization source |
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