CN217983263U - Electron bombardment ionization source - Google Patents
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- CN217983263U CN217983263U CN202221905595.1U CN202221905595U CN217983263U CN 217983263 U CN217983263 U CN 217983263U CN 202221905595 U CN202221905595 U CN 202221905595U CN 217983263 U CN217983263 U CN 217983263U
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Abstract
The utility model relates to an electron bombardment ionization source, which is provided with a filament fixing seat, a magnetic element, a first electron baffle, an electron grid component, an ion repulsion electrode, a first ionization chamber and a focusing lens group in sequence along the axial direction of a sample injection capillary; one end of the sample injection capillary is used for sample injection, and the other end of the sample injection capillary is arranged in the first ionization chamber; the first filament part and the first ionization chamber are axially installed, the first filament part is installed on the filament fixing seat, the first electronic baffle is installed on the first filament part, the magnetic element is installed in a mode of being tightly attached to the first filament fixing seat, and the electronic grid mesh is installed on the grid mesh seat. The utility model discloses a structural design has improved the ionization efficiency in electron bombardment ionization source to through the control to electron bombardment ionization source, make solitary mass spectrum can carry out the component separation of complicated sample, give up and fall gas chromatography, realize analytic system real-time, reliable.
Description
Technical Field
The utility model relates to an ionization technology field, in particular to electron bombardment ionization source.
Background
The mass spectrometer is a scientific instrument for analyzing chemical substance components, and the working mode of the mass spectrometer is to ionize molecules of a substance to be detected by a certain means and then sieve and measure the ions by an ion optical system. A mass spectrometer is generally composed of a sample introduction system, an ion source, a mass analyzer, a detector, a vacuum system, and an electrical control system.
The ion source is a key component in a mass spectrometer and has the function of ionizing gaseous sample molecules introduced by a sample introduction system into ions. Ionization of sample molecules is the primary link in mass spectrometry. The performance of the ion source has great influence on multiple indexes of the instrument, and whether effective ionization of sample molecules can directly influence important indexes such as the type, detection limit and sensitivity of a detectable substance. An electron impact ionization (EI) source is an ion source with wide application, and the basic principle is that a filament emits electrons, an accelerating electric field accelerates the electrons, and high-energy electrons impact molecules of an object to be detected to ionize the molecules of the object to be detected.
In recent years, with the development of industry, the requirements for real-time performance and accuracy of on-line gas monitoring in the process industry are higher and higher. Due to the limitation of application technology, the gas components in the traditional process industry are generally separated in advance by a gas chromatography system, and then the gas components are detected by an electron bombardment ionization source mass spectrometry system.
The electron bombardment ionization source adopted by the current commercial gas chromatography-mass spectrometer has a plurality of defects, for example, electrons enter an ionization chamber through a slit or a small hole, so that most of the electrons do not enter the ionization chamber; the sample molecule introduction path is orthogonally distributed to the electron introduction path, resulting in a low electron utilization rate. These defects result in poor ionization efficiency of the electron-bombarded ionization source, which results in a less sensitive instrument.
SUMMERY OF THE UTILITY MODEL
In order to achieve the above objects and other advantages in accordance with the present invention, the present invention provides an electron bombardment ionization source, including: the device comprises a sample injection capillary tube, a filament fixing seat, a magnetic element, a first electronic baffle, a first filament part, an electronic grid part, an ion repulsion electrode, a first ionization chamber and a focusing lens group, wherein one end of the sample injection capillary tube is used for sample injection, and the other end of the sample injection capillary tube is arranged in the first ionization chamber; the filament fixing seat, the magnetic element, the first electronic baffle, the electronic grid component, the ion repulsion electrode, the first ionization chamber and the focusing lens group are sequentially arranged along the axial direction of the sample injection capillary; the first filament part and the first ionization chamber are axially installed, the first filament part is installed on the filament fixing seat, the first electronic baffle is installed on the first filament part, the magnetic element is tightly attached to the first filament fixing seat, and the electronic grid mesh is installed on the grid mesh seat.
The filament fixing seat is arranged on the lamp body, and the second filament part and the second electronic baffle are arranged on the lamp body.
Further, first filament part, second filament part all include first filament electrode, second filament electrode, filament electrode ceramic cover, filament, the filament is installed first filament electrode with between the second filament electrode, filament electrode ceramic cover is installed on the first filament electrode, first filament electrode with the second filament electrode is fixed the filament fixing base, first electron plate washer second electron plate washer all is fixed second filament electrode and on the filament electrode ceramic cover, the filament be located corresponding electron plate washer with between the electron grid mesh part.
Furthermore, the second electronic baffle and the second electronic baffle are both baffles with bending angles.
Further, the electronic grid component comprises an electronic grid and a grid seat, and the electronic grid is arranged on the grid seat.
Further, the lens system further comprises a second ionization chamber, wherein the first ionization chamber is communicated with the second ionization chamber, and the second ionization chamber is located between the first ionization chamber and the focusing lens group.
Further, still include the heating ring, the heating ring cover is established on the second ionization chamber.
Further, the heating ring is a ceramic heating ring.
Further, the focusing lens group comprises an ion extraction lens, an ion focusing lens and an ion expelling lens; and the second ionization chamber, the ion extraction lens, the ion focusing lens and the ion expelling lens are sequentially arranged along the ion emitting direction.
Further, the filament fixing seat is a ceramic filament fixing seat.
Compared with the prior art, the beneficial effects of the utility model are that:
the utility model provides an electron bombardment ionization source improves the ionization efficiency in electron bombardment ionization source through structural design to through the control to electron bombardment ionization source, make solitary mass spectrum can carry out the component separation of complicated sample, give up and fall gas chromatography, realize real-time, the reliable of analytic system.
The above description is only an overview of the technical solution of the present invention, and in order to make the technical means of the present invention clearer and can be implemented according to the content of the description, the following detailed description is made with reference to the preferred embodiments of the present invention and accompanying drawings. The detailed description of the present invention is given by the following examples and the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without undue limitation to the invention. In the drawings:
FIG. 1 is a schematic diagram of an electron bombardment ionization source;
FIG. 2 is a cross-sectional view of a first electron bombardment ionization source;
FIG. 3 is a second cross-sectional view of an electron bombardment ionization source;
FIG. 4 is a schematic view of a filament assembly;
FIG. 5 is a schematic diagram of an electric field equipotential line at an electron entrance;
FIG. 6 is a first schematic diagram of electron flow at the electron entrance;
FIG. 7 is a second schematic diagram of electron flow at the electron entrance;
FIG. 8 is a schematic diagram of aliasing of various species spectral peaks;
FIG. 9 is a diagram of the spectrum signals of the same substance under different electron energies.
In the figure: 1. sampling a capillary tube; 2. a filament fixing seat; 3. a magnetic element; 4. a first electronic baffle; 5. a first filament part; 51. a second filament electrode; 52. a first filament electrode; 53. a filament; 54. a filament electrode ceramic sheath; 6. an electron grid member; 7. an ion repulsion electrode; 8. a first ionization chamber; 9. a second ionization chamber; 10. a heating ring; 11. a focusing lens group; 111. an ion extraction lens; 112. an ion focusing lens; 113. ejecting ions from the lens; 12. a second filament part.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and the detailed description, and it should be noted that the embodiments or technical features described below can be arbitrarily combined to form a new embodiment without conflict.
In the following description, suffixes such as "module", "part", or "unit" used to denote elements are used only for the convenience of description of the present invention, and have no specific meaning in itself. Thus, "module", "component" or "unit" may be used mixedly.
Example 1
An electron bombardment ionization source, as shown in fig. 1-3, comprising: the device comprises a sample injection capillary tube, a filament fixing seat, a magnetic element, a first electronic baffle, a first filament part, an electronic grid part, an ion repulsion electrode, a first ionization chamber and a focusing lens group, wherein one end of the sample injection capillary tube is used for sample injection, and the other end of the sample injection capillary tube is arranged in the first ionization chamber and is used for introducing a substance to be detected into the ionization chamber for ionization; the filament fixing seat, the magnetic element, the first electronic baffle, the electronic grid mesh component, the ion repulsion electrode, the first ionization chamber and the focusing lens group are sequentially arranged along the axial direction of the sample injection capillary; first filament part and first ionization chamber are according to the axial installation, and first filament part is installed on the filament fixing base, and in this embodiment, the filament fixing base is ceramic filament fixing base. The first electronic baffle is arranged on the first filament part and used for providing an electric field and repelling electrons emitted by the filament into the ionization chamber; the magnetic element is tightly attached to the first filament fixing seat and is a magnet in the embodiment and used for providing a magnetic field for the electron bombardment ionization source, so that electrons spirally advance, and the collision cross section of the electrons and molecules of an object to be detected is improved. The electronic grid is arranged on the grid seat. The electron grid provides an electric field which can deflect electrons into the axis of the ionization chamber, so that the electrons are positioned at the axis position when entering the ionization chamber, and the collision probability of the electrons and molecules is increased.
In order to prevent the damage of the first filament part from affecting the use of the device, the embodiment designs a double-filament structure so as to start the second filament when one filament is damaged; preferably, the filament lamp further comprises a second filament part and a second electronic baffle, wherein the second filament part is mounted on the filament fixing seat, and the second electronic baffle is mounted on the second filament part.
As shown in fig. 4, the first and second filament parts each include a first filament electrode, a second filament electrode, a ceramic filament electrode sheath, and a filament, the filament is installed between the first and second filament electrodes, the ceramic filament electrode sheath is installed on the first filament electrode, the first and second filament electrodes are fixed on the filament fixing base, the first and second electronic baffles are fixed on the second filament electrode and the ceramic filament electrode sheath, and the filament is located between the corresponding electronic baffles and the electronic grid mesh parts. The filament is used for emitting electrons, the two filaments are switched to be used, and when one of the two filaments works, the other filament does not work.
Furthermore, the second electronic baffle and the second electronic baffle are both baffles with bending angles.
Further, the electronic grid part comprises an electronic grid and a grid seat, and the electronic grid is arranged on the grid seat.
To achieve deep ionization of analyte molecules. Further, still include the second ionization chamber, first ionization chamber and second ionization chamber intercommunication, the second ionization chamber is located between first ionization chamber and the focusing lens group. And enabling the electrons to collide and ionize with the molecules of the object to be tested at the first ionization chamber, and enabling the electrons to further collide with the molecules of the object to be tested which are not ionized at the second ionization chamber, so that the deep ionization of the molecules of the object to be tested is realized.
Furthermore, the ionization chamber also comprises a heating ring which is sleeved on the second ionization chamber. In this embodiment, the heating ring is a ceramic heating ring. The ceramic heating ring is sleeved outside the second ionization chamber and used for heating the whole ionization chamber, on one hand, liquefaction and deposition of molecules of the object to be detected are prevented, the cleanness and pollution resistance of the ion source are guaranteed, on the other hand, the activity of electrons and the molecules of the object to be detected is improved, and the high ionization efficiency is guaranteed.
As shown in fig. 3, the focusing lens group includes an ion extracting lens, an ion focusing lens, and an ion expelling lens; and a second ionization chamber, an ion extraction lens, an ion focusing lens and an ion expelling lens are sequentially arranged along the ion emitting direction. The ion leading-out lens can lead ionized ions out of the ionization chamber and reflect electrons back, and the reflected electrons can collide with non-ionized molecules of the object to be detected in the second ionization chamber to be further ionized; the ion focusing lens is used for focusing ions led out of the ionization chamber so that the ions can efficiently enter a rear ion optical system; the ion expelling lens is used for introducing ions into the ion optical system.
The utility model discloses a filament and ionization chamber axial installation of electron bombardment ionization source, but in order to give the appearance capillary and let the space, two filament positions are not on the center pin of ionization chamber. The utility model discloses utilize the electric field that electron plate washer, electron grid and ion repel utmost point three formed, the electric field is as shown in fig. 5, lets the electron take place the skew when getting into the ionization chamber for the electron axial gets into the ionization chamber, as shown in fig. 6, 7. The utility model discloses well electron introduces first ionization chamber for the axial, and the ionization chamber is also introduced for the axial to the sample molecule. Compared with the scheme that the electron introduction direction and the sample molecule introduction direction are distributed orthogonally, the axial introduction of the two directions has the advantages that the movement path of the electrons can be superposed with the movement path of the molecules of the object to be detected, the collision between the electrons and the molecules of the object to be detected is fully ensured, and the molecules of the object to be detected are fully ionized.
The utility model discloses drive out lens to electron plate washer, first filament, second filament, electron grid, ion repulsion pole, ceramic heating ring, ion extraction lens, ion focusing lens, ion and carry out electrical connection. The electric fields of the three parts of the electronic baffle plate, the electronic grid mesh and the ion repulsion electrode guide the electrons to the central shaft of the ionization chamber. The voltage of the electronic baffle plate and the electronic grid can be changed, the energy of electrons entering the ionization chamber can be changed, and when the voltage difference between the electronic baffle plate, the electronic grid and the ion repeller becomes small, the energy of the electrons becomes small; the first ionization chamber and the second ionization chamber are grounded; the ion extraction lens, the ion focusing lens and the ion expelling lens jointly form a focusing lens group for extracting and focusing ions; the ion extraction lens applies negative voltage to extract ions and reflect electrons, so that the electrons cannot escape from the ionization chamber and are reflected back to the second ionization chamber to be subjected to collision deep ionization with non-ionized gas molecules.
A method of operating an electron-bombarded ionization source comprising:
at present, the electron bombardment ionization source mostly adopts the electron energy of 70eV to bombard sample molecules, and in this case, if separation by chromatography is not carried out, the spectrum peaks of a plurality of substances are mixed together, and the amount of each substance is difficult to distinguish, as shown in FIG. 8.
By adjusting the voltage of the electron baffle and the electron grid, the energy of the electrons entering the ionization chamber is different, and the proportion of each spectral peak in the spectrogram formed by the same substance is different under different electron energies, as shown in fig. 9. The utility model discloses a single material spectral peak ratio under the electron energy of difference and the spectrogram of mixing material under the different energy calculate the concentration ratio of each material in the mixing material.
For example: the mixed material contains n kinds of materials with concentration of x 1 、x 2 ……x n The formed spectrogram has five spectrogram peaks of a, b, c, d and e. The peak ratio of the spectrum formed by the mixed substance is a at 70eV 1 、b 1 、c 1 、d 1 、e 1 . According to the spectrum library, the first substance forms a spectrum with a peak value ratio a at 70eV 11 、b 11 、c 11 、d 11 、e 11 The second substance has a peak ratio of a at 70eV 12 、b 12 、c 12 、d 12 、e 12 By analogy, the peak ratio of the spectrum formed by the n-th substance at 70eV is a 1n 、b 1n 、c 1n 、d 1n 、e 1n . From the above data, a matrix equation can be obtained:
wherein x is 1 、x 2 ……x n Is the quantity required to be solved; a is 11 、b 11 、c 11 、d 11 、e 11 、a 12 、b 12 、c 12 、d 12 、e 12 ……a 1n 、b 1n 、c 1n 、d 1n 、e 1n The equivalent value is the value of a 70eV standard spectrum library, and is a known quantity; a is 1 、b 1 、c 1 、d 1 、e 1 The value of the mixture measured at 70eV is a known amount.
At a second electron energy, e.g. 60eV, the peak ratio of the spectrum formed by the mixed species is a 2 、b 2 、c 2 、d 2 、e 2 . According to the spectrogram library, the first substance forms a spectrum peak value ratio a at 60eV 21 、b 21 、c 21 、d 21 、e 21 The second substance has a peak ratio of a at 70eV 22 、b 22 、c 22 、d 22 、e 22 By analogy, the peak ratio of the spectrum formed by the n-th substance at 70eV is a 2n 、b 2n 、c 2n 、d 2n 、e 2n . From the above data, a matrix equation can be obtained:
by analogy, at the nth energy, a matrix equation can be obtained:
by the above n matrix equations, x can be solved 1 、x 2 ……x n And calculating the ratio of the amount of each substance in the mixture. On the basis of the method, automatic energy regulation and automatic calculation are added, so that the quantity of each substance in the mixed substance can be calculated quickly.
The foregoing is merely an example of the present specification and is not intended to limit one or more embodiments of the present specification. Various modifications and alterations to one or more embodiments described herein will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of one or more embodiments of the present specification should be included in the scope of claims of one or more embodiments of the present specification. One or more embodiments of this specification.
Claims (10)
1. An electron-bombardment ionization source, comprising: the device comprises a sample injection capillary tube, a filament fixing seat, a magnetic element, a first electronic baffle, a first filament part, an electronic grid part, an ion repulsion electrode, a first ionization chamber and a focusing lens group, wherein one end of the sample injection capillary tube is used for sample injection, and the other end of the sample injection capillary tube is arranged in the first ionization chamber; the filament fixing seat, the magnetic element, the first electronic baffle, the electronic grid component, the ion repulsion electrode, the first ionization chamber and the focusing lens group are sequentially arranged along the axial direction of the sample injection capillary; the first filament part and the first ionization chamber are axially installed, the first filament part is installed on the filament fixing seat, the first electronic baffle is installed on the first filament part, the magnetic element is tightly attached to the first filament fixing seat, and the electronic grid mesh is installed on the grid mesh seat.
2. An electron-bombarded ionization source as recited in claim 1, wherein: the filament fixing seat is arranged on the lamp body, and the second filament part and the second electronic baffle are arranged on the lamp body.
3. An electron-bombarded ionization source as recited in claim 2, wherein: first filament part, second filament part all include first filament electrode, second filament electrode, filament electrode ceramic sheathing, filament, the filament is installed first filament electrode with between the second filament electrode, filament electrode ceramic sheathing is installed on the first filament electrode, first filament electrode with the second filament electrode is fixed the filament fixing base, first electron plate washer second electron plate washer all is fixed second filament electrode and on the filament electrode ceramic sheathing, the filament be located corresponding electron plate washer with between the electron grid part.
4. An electron bombardment ionization source as recited in claim 2, wherein: the second electronic baffle and the second electronic baffle are both baffles with bending angles.
5. An electron bombardment ionization source as recited in claim 1, wherein: the electronic grid mesh component comprises an electronic grid mesh and a grid mesh seat, and the electronic grid mesh is arranged on the grid mesh seat.
6. An electron-bombarded ionization source as recited in claim 1, wherein: the first ionization chamber is communicated with the second ionization chamber, and the second ionization chamber is located between the first ionization chamber and the focusing lens group.
7. An electron-bombarded ionization source as recited in claim 6, wherein: the second ionization chamber is provided with a heating ring, and the heating ring is sleeved on the second ionization chamber.
8. An electron bombardment ionization source as recited in claim 7, wherein: the heating ring is a ceramic heating ring.
9. An electron-bombarded ionization source as recited in claim 6, wherein: the focusing lens group comprises an ion extraction lens, an ion focusing lens and an ion expelling lens; and the second ionization chamber, the ion extraction lens, the ion focusing lens and the ion expelling lens are sequentially arranged along the ion emitting direction.
10. An electron-bombarded ionization source as recited in claim 1, wherein: the filament fixing seat is a ceramic filament fixing seat.
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| CN115295396A (en) * | 2022-07-22 | 2022-11-04 | 天津国科医工科技发展有限公司 | Electron bombardment ionization source |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115295396A (en) * | 2022-07-22 | 2022-11-04 | 天津国科医工科技发展有限公司 | Electron bombardment ionization source |
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Address after: Building 4, No.16 Wujing Road, development zone, Dongli District, Tianjin Patentee after: Tianjin Guoke Medical Technology Development Co.,Ltd. Country or region after: China Address before: Building 4, No.16 Wujing Road, development zone, Dongli District, Tianjin Patentee before: TIANJIN GUOKE YIGONG TECHNOLOGY DEVELOPMENT Co.,Ltd. Country or region before: China |
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Effective date of registration: 20240426 Address after: Building 4, No.16 Wujing Road, development zone, Dongli District, Tianjin Patentee after: Tianjin Guoke Medical Technology Development Co.,Ltd. Country or region after: China Patentee after: Suzhou Institute of Biomedical Engineering and Technology Chinese Academy of Sciences Address before: Building 4, No.16 Wujing Road, development zone, Dongli District, Tianjin Patentee before: Tianjin Guoke Medical Technology Development Co.,Ltd. Country or region before: China |