CN210722952U - Composite ionization source device for mass spectrometry - Google Patents
Composite ionization source device for mass spectrometry Download PDFInfo
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- CN210722952U CN210722952U CN201922142613.XU CN201922142613U CN210722952U CN 210722952 U CN210722952 U CN 210722952U CN 201922142613 U CN201922142613 U CN 201922142613U CN 210722952 U CN210722952 U CN 210722952U
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Abstract
The utility model relates to a mass spectrometry instrument, specific compound light ionization source device for mass spectrometry that says so. Comprises an ionization cavity, a vacuum ultraviolet lamp, a discharge needle, a sample gas inlet, a purge gas inlet, a tail gas outlet, a repulsion electrode, a focusing electrode and a transmission electrode. Combines the advantages of two ionization modes of atmospheric pressure chemical ionization and atmospheric pressure photoionization. The inner diameter of the focusing electrode is smaller, the ionization region is divided into a left region and a right region, and the interference of nitrogen-containing oxide and ozone generated by corona discharge on gas-phase molecule-ion reaction can be reduced by the design that airflow reversely flows through the discharge needles. The device combines the advantages of an atmospheric pressure photoionization source and an atmospheric pressure chemical ionization source, expands the range of ionizable compounds of the instrument, enhances the transmission efficiency of ions by introducing the repulsion electrode, the focusing electrode and the transmission electrode, and improves the detection sensitivity.
Description
Technical Field
The utility model relates to a mass spectrometry instrument, specific compound ionization source device that is used for atmospheric pressure photoionization and atmospheric pressure chemical ionization of mass spectrometry that says so.
Background
The soft ionization technology developed in recent years has the characteristics of high molecular ion yield and easy spectrogram analysis. Soft ionization techniques such as electrospray ionization, Atmospheric Pressure Chemical Ionization (APCI), and Atmospheric Pressure Photoionization (APPI) have opened up a new era of mass spectrometry ionization techniques.
Atmospheric pressure chemical ionization is to utilize sharp high-voltage (corona) discharge to promote reaction gas ionization under the atmospheric pressure condition to form a plasma region, and when sample gaseous molecules pass through the plasma region, the sample gaseous molecules collide with the reaction gas ions to generate proton or charge transfer, so as to form molecular ions or quasi-molecular ions. In the traditional atmospheric pressure chemical ionization, an ionization region is only provided with one region, and nitrogen-containing oxides and ozone generated during corona discharge can interfere gas phase molecule-ion reaction and reduce the response sensitivity of sample ions. Atmospheric pressure chemical ionization is suitable for ionization of weakly polar compounds.
The single photon ionization is used as a soft ionization source and has the characteristics of high molecular ion yield and easy spectrogram analysis. Vacuum ultraviolet lamps are one of the common single photon ionization sources. Atmospheric pressure photoionization techniques, as early as 2000, were applied by Robb et al in LC/MS for ionization of non-polar compounds and some polar compounds.
The mass spectrometry has the advantages of high analysis speed, high resolution and sensitivity and strong qualitative capability. Atmospheric pressure ionization techniques such as electrospray ionization, atmospheric pressure chemical ionization, atmospheric pressure photoionization and the like are suitable for rapid and online analysis of organic matter samples.
In 2011, plum sea and the like invented a composite ionization source differential ion mobility spectrometry (patent application No. 201110428647.0). The invention combines the advantages of Ni63 from the ionization source of a vacuum ultraviolet lamp, is a detection instrument capable of effectively detecting charged nano aerosol particles, and increases the detection range of the instrument and the selectivity of the instrument.
In 2012, wanxin et al invented a composite ionization device for ion mobility spectrometry (patent application No. 201210339229.9). The invention relates to a composite ionization source of a vacuum ultraviolet lamp and a nickel source ionization source for ion mobility spectrometry detection. After samples are injected by sample injectors with different modes, the samples are carried by carrier gas and firstly enter an ionization chamber of a vacuum ultraviolet lamp, and the carrier gas and the components of the samples are ionized; then the sample molecules are carried by carrier gas to enter an ion migration tube containing a nickel source, and after the sample molecules are doubly ionized firstly and secondly, the sample molecules enter a drift region formed by a uniform electric field through an ion gate which is periodically opened, and are separated and detected in the drift region.
In 2015, Zhao, Bao, et al invented a two-zone reverse airflow atmospheric pressure chemical ionization source (patent application No. 201510658263.6). Including ionization source chamber, discharge needle, introduction port to and mass spectrum introduction cone mouth, the characteristic is: the ionization source cavity is divided into an upper part and a lower part by a partition plate, the upper part is a discharge area, the lower part is an ionization area, the two areas are communicated through a small hole in the center of the partition plate, a gas outlet is arranged in the discharge area, and a sweeping gas inlet is arranged in the ionization area. And the neutral products generated by discharge are reduced from flowing into an ionization region by utilizing reverse blowing of sweeping gas, so that the influence of the neutral products generated by discharge on the ionization of sample molecules is reduced.
Therefore, the invention designs a composite ionization source device for mass spectrometry. The advantages of the atmospheric pressure photoionization source and the atmospheric pressure chemical ionization source are combined, the range of ionizable compounds of the instrument is expanded, the introduction of the repulsion electrode, the focusing electrode and the transmission electrode enhances the transmission efficiency of ions, and the detection sensitivity is improved.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a compound ionization source device for mass spectrometry. The advantages of the atmospheric pressure photoionization source and the atmospheric pressure chemical ionization source are combined, and the range of ionizable compounds of the instrument is expanded. In order to achieve the above object, the utility model adopts the following technical scheme:
a composite ionization source apparatus for mass spectrometry comprising: the device comprises an ionization cavity, a vacuum ultraviolet lamp, a discharge needle, a repulsion electrode, a focusing electrode, a transmission electrode, a differential electrode, a sample gas inlet pipe, a purge gas inlet pipe and a tail gas outlet;
the ionization chamber is a container with a closed left end and an open right end, flat-plate-shaped repulsion electrodes with through holes in the middle, flat-plate-shaped focusing electrodes with through holes in the middle and more than 2 flat-plate-shaped transmission electrodes with through holes in the middle are sequentially arranged in the container from left to inside at intervals and in parallel, flat-plate-shaped differential electrodes with through holes in the middle are arranged at the right opening end of the container, the repulsion electrodes, the focusing electrodes, the transmission electrodes and the through holes in the middle of the differential electrodes are coaxial, and the left side surface of each differential electrode is hermetically connected with the end face of the right opening;
a through hole is arranged above the ionization cavity, the vacuum ultraviolet light source is arranged above the through hole, and the peripheral edge of the light window of the light outlet is hermetically connected with the inner wall surface of the through hole or the upper end surface of the container around the through hole;
the light emitted by the vacuum ultraviolet light source is emitted into the area between the repulsion electrode and the focusing electrode in the ionization cavity from top to bottom;
a discharge needle is arranged in the ionization cavity along the axis direction of the central through hole of the repulsion electrode, and the needle point of the discharge needle is positioned in the area between the repulsion electrode and the focusing electrode;
a sample gas inlet pipe is arranged on the side wall surface of the ionization cavity, and the gas outlet of the sample gas inlet pipe faces to the area between the focusing electrode and the transmission electrode;
a purge gas inlet pipe is arranged on the side wall surface of the ionization cavity, and the gas outlet of the purge gas inlet pipe faces to the area between the transmission electrode and the differential electrode;
and a tail gas outlet is arranged on the side wall surface of the ionization cavity close to the repulsion electrode.
The discharge needle is located in the ionization chamber, and the needle point is 2 ~ 10mm apart from the focus electrode.
The repulsion electrode, the focusing electrode, the transmission electrode and the differential electrode are all flat-plate-shaped round stainless steel electrodes and are coaxially arranged; the number of the transmission electrodes is 1-6; the inner diameters of the repulsion electrode and the transmission electrode are the same, the size is 8-18 mm, and the inner diameter of the focusing electrode is 2-4 mm; the lower end of the differential electrode is provided with a mass spectrometer.
The sample gas inlet pipe is positioned between the focusing electrode and the first piece of transmission electrode close to the focusing electrode; the purge gas inlet is positioned between the last transmission electrode close to the differential electrode and the differential electrode; the tail gas outlet is positioned between the repulsion electrode and the vacuum ultraviolet lamp.
The repulsion electrode is fixed on the ionization cavity through an insulating upright post, and the focusing electrode and the transmission electrode are fixed on the differential electrode through the insulating upright post.
The repulsion electrode, the focusing electrode and the transmission electrode are all applied with direct current high voltage.
The utility model provides a but compound ionization source during actual work selects atmospheric pressure chemical ionization mode or atmospheric pressure light ionization mode, and accessible control vacuum ultraviolet lamp power switch realizes switching in the twinkling of an eye with discharge needle power switch between two kinds of modes. The advantages of two ionization modes are combined, and the range of the instrument for detecting the compound is expanded.
Drawings
Fig. 1 is a schematic structural diagram of a composite ionization source device for mass spectrometry.
1. A vacuum ultraviolet lamp; 2. a discharge needle; 3. an ionization chamber; 4. a sample gas inlet tube; 5. a purge gas inlet pipe; 6. a tail gas exhaust port; 7. a repulsion electrode; 8. a focusing electrode; 9. a transmission electrode; a differential electrode; 11. an insulating upright post I; 12. an insulating upright post II; 13; a mass spectrometer.
Detailed Description
The invention will be further described, by way of example, with reference to the accompanying drawings
Referring to fig. 1, a schematic structural diagram of a composite ionization source device for mass spectrometry according to the present invention is shown.
The method comprises the following steps: the device comprises an ionization cavity 3, a vacuum ultraviolet lamp 1, a discharge needle 2, a repulsion electrode 7, a focusing electrode 8, a transmission electrode 9, a differential electrode 10, a sample gas inlet pipe 4, a purge gas inlet pipe 5 and a tail gas outlet 6;
the ionization cavity 3 is a container with a closed left end and an open right end, flat-plate-shaped repulsion electrodes 7 with through holes in the middle, flat-plate-shaped focusing electrodes 8 with through holes in the middle, more than 2 flat-plate-shaped transmission electrodes 9 with through holes in the middle are sequentially arranged in the container from left to inside at intervals and in parallel, a flat-plate-shaped differential electrode 10 with through holes in the middle is arranged at the right opening end of the container, the repulsion electrodes 7, the focusing electrodes 8, the transmission electrodes 9 and the through holes in the middle of the differential electrodes 10 are coaxial, and the left side surface of the differential electrode 10 is connected with the end face of the right opening;
a through hole is arranged above the ionization cavity 3, the vacuum ultraviolet lamp 1 is arranged above the through hole, and the peripheral edge of a light window of a light outlet of the vacuum ultraviolet lamp is hermetically connected with the inner wall surface of the through hole or the upper end surface of the container around the through hole;
the light emitted by the vacuum ultraviolet lamp 1 is emitted into the area between the repulsion electrode 7 and the focusing electrode 8 in the ionization cavity 3 from top to bottom;
a discharge needle 2 is arranged in the ionization cavity 3 along the axial direction of the central through hole of the repulsion electrode 7, and the needle point of the discharge needle 2 is positioned in the area between the repulsion electrode 7 and the focusing electrode 8;
a sample gas inlet pipe 4 is arranged on the side wall surface of the ionization cavity 3, and the gas outlet of the sample gas inlet pipe 4 faces the area between the focusing electrode 8 and the transmission electrode 9;
a purge gas inlet pipe 5 is arranged on the side wall surface of the ionization cavity 3, and the gas outlet of the purge gas inlet pipe 5 faces the region between the transmission electrode 9 and the differential electrode 10;
and a tail gas outlet 6 is arranged on the side wall surface of the ionization cavity 3 close to the repulsion electrode 7.
The discharge needle is located in the ionization chamber, and the needle point is 2mm apart from the focus electrode.
The repulsion electrode 7, the focusing electrode 8, the transmission electrode 9 and the differential electrode 10 are all plate-shaped circular stainless steel electrodes and are coaxially arranged; the number of the transmission electrodes 9 is 2; the inner diameters of the repulsion electrode 7 and the transmission electrode 9 are the same, the size is 8mm, and the inner diameter of the focusing electrode 8 is 3 mm; the lower end of the differential electrode 10 is provided with a mass spectrometer 13.
The sample gas inlet 4 is positioned between the focusing electrode 8 and the first sheet of transmission electrode; the purge gas inlet 5 is positioned between the last transmission electrode and the differential electrode 10; the exhaust gas outlet 6 is located between the repeller electrode 7 and the vacuum ultraviolet lamp 1.
The repulsion electrode 7 is fixed on the ionization chamber 3 through an insulating column 12, and the focusing electrode 8 and the transmission electrode 9 are fixed on the differential electrode 10 through an insulating column 11.
The repulsion electrode 7, the focusing electrode 8 and the transmission electrode 9 are all applied with direct current high voltage.
The operation principle of the utility model is explained as follows:
atmospheric pressure chemical ionization mode: the discharge needle applies direct current high voltage, sample gas enters the ionization region from the sample gas inlet 4, purge gas enters from the purge gas inlet 5 and is blown back to the ionization region of the discharge needle on the left side of the focusing electrode 8, and neutral nitrogen oxides and ozone generated by discharge are discharged from the tail gas outlet 6. Metastable ions generated by discharge react with sample molecules and then enter a mass spectrometer for detection after passing through a focusing electrode 8, a transmission electrode 9 and a differential electrode 10.
Atmospheric pressure photoionization mode: the sample introduction and purging mode is the same as the atmospheric pressure chemical ionization mode, and ions generated by photoionization enter a mass spectrometer for detection after passing through a focusing electrode 8, a transmission electrode 9 and a differential electrode 10 under the action of a repulsion electrode direct-current high-voltage electric field.
Claims (6)
1. A composite ionization source device for mass spectrometry is characterized in that
The method comprises the following steps: the device comprises an ionization cavity (3), a vacuum ultraviolet lamp (1), a discharge needle (2), a repulsion electrode (7), a focusing electrode (8), a transmission electrode (9), a differential electrode (10), a sample gas inlet pipe (4), a purge gas inlet pipe (5) and a tail gas outlet (6);
the ionization cavity (3) is a container with a closed left end and an open right end, flat-plate-shaped repulsion electrodes (7) with through holes in the middle, flat-plate-shaped focusing electrodes (8) with through holes in the middle and more than 2 flat-plate-shaped transmission electrodes (9) with through holes in the middle are sequentially arranged in the container from left to inside at intervals and in parallel, a flat-plate-shaped differential electrode (10) with through holes in the middle is arranged at the right opening end of the container, the repulsion electrodes (7), the focusing electrodes (8), the transmission electrodes (9) and the differential electrodes (10) are coaxial in the middle through holes, and the left side surface of the differential electrode (10) is hermetically connected with the end surface;
a through hole is arranged above the ionization cavity (3), the vacuum ultraviolet lamp (1) is arranged above the through hole, and the peripheral edge of a light window of a light outlet of the vacuum ultraviolet lamp is hermetically connected with the inner wall surface of the through hole or the upper end surface of the container around the through hole;
light emitted by the vacuum ultraviolet lamp (1) is emitted into a region between the repulsion electrode (7) and the focusing electrode (8) in the ionization cavity (3) from top to bottom;
a discharge needle (2) is arranged in the ionization cavity (3) along the axial direction of the central through hole of the repulsion electrode (7), and the needle point of the discharge needle (2) is positioned in the area between the repulsion electrode (7) and the focusing electrode (8);
a sample gas inlet pipe (4) is arranged on the side wall surface of the ionization cavity (3), and the gas outlet of the sample gas inlet pipe (4) faces to the region between the focusing electrode (8) and the transmission electrode (9);
a purge gas inlet pipe (5) is arranged on the side wall surface of the ionization cavity (3), and the gas outlet of the purge gas inlet pipe (5) faces to the region between the transmission electrode (9) and the differential electrode (10);
the side wall surface of the ionization cavity (3) close to the repulsion electrode (7) is provided with a tail gas outlet (6).
2. The complex ionization source device for mass spectrometry of claim 1, wherein:
the discharge needle is located in the ionization chamber, and the needle point is 2 ~ 10mm apart from focusing electrode (8).
3. The complex ionization source device for mass spectrometry of claim 1, wherein:
the repulsion electrode (7), the focusing electrode (8), the transmission electrode (9) and the differential electrode (10) are all flat round stainless steel electrodes and are coaxially arranged; the number of the transmission electrodes (9) is 1-6; the inner diameters of the repulsion electrode (7) and the transmission electrode (9) are the same, the size is 8-18 mm, and the inner diameter of the focusing electrode (8) is 2-4 mm; the lower end of the differential electrode (10) is provided with a mass spectrometer (13).
4. The complex ionization source device for mass spectrometry of claim 1, wherein:
the sample gas inlet pipe (4) is positioned between the focusing electrode (8) and the first transmission electrode close to the focusing electrode; the purge gas inlet pipe (5) is positioned between the last transmission electrode close to the differential electrode and the differential electrode (10); the tail gas outlet (6) is positioned between the repulsion electrode (7) and the vacuum ultraviolet lamp (1).
5. The complex ionization source device for mass spectrometry of claim 1, wherein:
the repulsion electrode (7) is fixed on the ionization cavity (3) through an insulating upright post II (12), and the focusing electrode (8) and the transmission electrode (9) are fixed on the differential electrode (10) through an insulating upright post I (11).
6. The complex ionization source device for mass spectrometry of claim 1, wherein:
the repulsion electrode (7), the focusing electrode (8) and the transmission electrode (9) are all applied with direct current high voltage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922142613.XU CN210722952U (en) | 2019-12-04 | 2019-12-04 | Composite ionization source device for mass spectrometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922142613.XU CN210722952U (en) | 2019-12-04 | 2019-12-04 | Composite ionization source device for mass spectrometry |
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| Publication Number | Publication Date |
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| CN210722952U true CN210722952U (en) | 2020-06-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201922142613.XU Active CN210722952U (en) | 2019-12-04 | 2019-12-04 | Composite ionization source device for mass spectrometry |
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