CN219066754U - Device for effectively inhibiting generation and transmission of water cluster ions in associated ionization mass spectrometer - Google Patents
Device for effectively inhibiting generation and transmission of water cluster ions in associated ionization mass spectrometer Download PDFInfo
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- CN219066754U CN219066754U CN202320078316.7U CN202320078316U CN219066754U CN 219066754 U CN219066754 U CN 219066754U CN 202320078316 U CN202320078316 U CN 202320078316U CN 219066754 U CN219066754 U CN 219066754U
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Abstract
The utility model discloses a device for effectively inhibiting generation and transmission of water cluster ions in an associated ionization mass spectrometer, and relates to the field of mass spectrum detection. The ion migration system comprises an ion lens I, an ion lens II and an octupole ion guide rod which are arranged between the ion lens I and the ion lens II in a relative mode; the utility model can form uniform electric field between the ionizer and the differential plate, and can increase the collision movement of water cluster ions and background gas by adjusting the intensity of the electric fieldCan convert water cluster ions into H with small molecular weight 3 O + The combination of the low-quality discrimination effect of the octupole ion guide rod can effectively inhibit H 3 O + Thereby effectively reducing the generation and transmission of water cluster ions in the system, reducing the background signal height of mass spectrum, and enabling the associated ionization mass spectrometer to be used for the direct on-line detection of trace components.
Description
Technical Field
The utility model relates to the field of mass spectrometry detection, in particular to a device for effectively inhibiting generation and transmission of water cluster ions in an associated ionization mass spectrometer.
Background
Associative ionization is an ionization process that generates ions by collisions with neutral molecules in either an excited or non-excited state and involves the formation of new bonds, a common ionization reaction in nature, e.g., CH+O→CHO + +e - Is a very efficient ion generating channel in the hydrocarbon combustion process, and is also the basic reaction of the flame ionization detector; the excited inert gas atoms and the highly excited alkali metal atoms can also collide with specific substances to undergo association ionization reaction, such as He * +He→He 2 + +e - . However, because the association ionization form is single in nature, only a few specific ions can be generated, and the association ionization is limited to be an independent mass spectrum ionization technology. The excited state methylene dichloride induced association ionization is a new mass spectrum ionization technology which is discovered recently, and the ionization technology can react with almost all polar organic compounds containing oxygen, nitrogen, sulfur and the like. The occurrence of the induced association ionization of the excited state methylene dichloride overcomes the technical obstacle of single channel of the traditional association ionization reaction, and makes the association ionization become a high-efficiency mass spectrum ionization technology.
The association ionization induced by excited state dichloromethane has ultrahigh ionization efficiency, and can reach 10 -1 ion molecule -1 Sensitivity to oxygen-, nitrogen-and sulfur-containing organic compounds is in the range of hundreds to thousands of counts pptv -1 s -1 The method comprises the steps of carrying out a first treatment on the surface of the At the same time, the ultrahigh ionization efficiency also generates a large amount of H 3 O + And water cluster ions thereof. In the earlier-stage associated ionization mass spectrum device, an ion transmission system only consists of a simple electrostatic lens, and is lack of a mass selection function and a large amount of H 3 O + And its cluster ions are flushed into the ion transport and detection regions, resulting in a significant increase in background signal. At the same time, the ion source generates high flux H even if high purity nitrogen is used as carrier gas 3 O + And water cluster ions, wherein the ion is represented by (H 2 O) 2 H + The highest signal intensity, such high flux ions, render the ion detection device of the mass spectrometer non-loadable. Therefore, in order to protect the ion detector of the mass spectrometer, in the previous experiments, physical methods are adopted to reduce the number of ions reaching the ion detector, such as adjusting the voltage of the ion transmission system to reduce the ion transmission efficiency, or adding slits on the ion flight path, etc. However, the operation makes the instrument unable to directly measure the ultra-low concentration to-be-measured object, so that a certain gap exists between the actual minimum detection concentration of the instrument and the theoretical calculation detection limit of the instrument.
Disclosure of Invention
The utility model aims to provide a device for effectively inhibiting generation and transmission of water cluster ions in an associated ionization mass spectrometer, and the ionization efficiency of an ion source is fully exerted while an ion detector is protected.
In order to achieve the above object, the present utility model provides the following solutions:
an apparatus effective to inhibit generation and transport of water cluster ions in an associated ionization mass spectrometer, the apparatus comprising: the ion migration system comprises an ion lens I, an ion lens II and an octupole ion guide rod which are arranged between the ion lens I and the ion lens II in a relative mode;
the vacuum ultraviolet light source system is used for generating vacuum ultraviolet light;
the ionization system is used for enabling a sample and a protonating agent to generate association ionization reaction under the action of the vacuum ultraviolet light to generate ions of an object to be detected;
a metal mesh and a differential plate are arranged between an ionizer in the ionization system and the ion migration system;
the metal net is attached to the center of one side, close to the ionization system, of the differential plate and covers a through hole in the center of the differential plate;
the ion migration system is used for transmitting and focusing the ions of the to-be-detected object through the ion lens I, the octupole ion guide rod and the ion lens II, and the transmitted and focused ions of the to-be-detected object enter the mass spectrum detection system;
the mass spectrum detection system is used for detecting the ions of the object to be detected.
Preferably, the vacuum ultraviolet light source system comprises a vacuum ultraviolet lamp tube and a radio frequency generator.
Preferably, a magnesium fluoride lens or a lithium fluoride lens is arranged between the vacuum ultraviolet lamp tube and the ionizer of the ionization system, and vacuum ultraviolet light enters the ionizer through the magnesium fluoride lens or the lithium fluoride lens.
Preferably, the ionization system comprises a sample inlet pipe, an analysis device, a sample inlet pipe and an ionizer which are connected in sequence;
one end of the sample introducing pipe is connected with one end of the analyzing device, the other end of the analyzing device is connected with one end of the sample introducing pipe, and the other end of the sample introducing pipe is communicated with the ionizer.
Preferably, the direction of the sample inlet pipe of the ionization system is perpendicular to the direction of the vacuum ultraviolet irradiation.
Preferably, a metal mesh and a differential plate are arranged between the ionization system and the ion migration system;
the metal net is attached to the center of one side, close to the ionization system, of the differential plate and covers the through hole in the center of the differential plate.
Preferably, the ion migration system is communicated with the mass spectrum detection system through a slit; and the transmitted and focused object ions enter the reflection type mass spectrum device of the mass spectrum detection system through the slit.
Preferably, the mass spectrum detection system comprises a reflection type mass spectrum device, an ion detection device and a data acquisition system;
the ion detection device is arranged at the outlet of the reflection type mass spectrum device and is connected with the data acquisition device.
Preferably, the ionization system, the ion migration system and the mass spectrum detection system are respectively arranged in different vacuum chambers, and a molecular pump is arranged on the side wall of the vacuum chamber and is used for maintaining the vacuum environment required by the ionization system, the ion migration system and the mass spectrum detection system.
An ionization system in an apparatus according to any one of the preceding claims.
According to the specific embodiment provided by the utility model, the utility model discloses the following technical effects:
an apparatus effective to inhibit generation and transport of water cluster ions in an associated ionization mass spectrometer, the apparatus comprising: the ion migration system comprises an ion lens I, an ion lens II and an octupole ion guide rod which are arranged between the ion lens I and the ion lens II in a relative mode; the vacuum ultraviolet light source system is used for generating vacuum ultraviolet light; the ionization system is used for enabling a sample and a protonating agent to generate association ionization reaction under the action of the vacuum ultraviolet light to generate ions of an object to be detected; the ion migration system is used for transmitting and focusing the ions of the to-be-detected object through the ion lens I, the octupole ion guide rod and the ion lens II, and the transmitted and focused ions of the to-be-detected object enter the mass spectrum detection system; the mass spectrum detection system is used for detecting the ions of the object to be detected; the differential plate of the outlet of the ionizer and the inlet of the ion transfer system provided by the utility model is of a parallel structure, the metal net is attached to the center of the differential plate and covers the through holes in the center of the differential plate, so that a uniform electric field is formed between the outlet of the ionizer and the differential plate, the collision kinetic energy of water cluster ions and background gas can be increased by adjusting the voltage difference between the ionizer and the differential plate and properly enhancing the electric field, the water cluster ions are declustered and converted into small molecular weight hydrated protons (H) 3 O + ) The method comprises the steps of carrying out a first treatment on the surface of the The low-quality discrimination effect of the octupole ion guide rod is utilized to effectively inhibit H 3 O + The combined technology can effectively inhibit the generation and transmission of water cluster ions in a system, effectively reduce the background signal height of mass spectrum, ensure that an associated ionization mass spectrometer can be used for detecting trace components, and provide a novel online detection technology for directly detecting trace polar organic matters such as oxygen, nitrogen, phosphorus and the like.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present utility model, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an apparatus for effectively inhibiting the generation and transport of water cluster ions in an associated ionization mass spectrometer of the present utility model.
Symbol description:
the device comprises a vacuum ultraviolet light source system-1, an ionization system-2, an ion migration system-3, a mass spectrum detection system-4, a vacuum ultraviolet lamp tube-5, a radio frequency generator-6, a magnesium fluoride lens or lithium fluoride lens-7, a sample inlet tube-8, an analysis device-9, a sample inlet tube-10, an ionizer-11, a molecular pump-12, a metal net-13, a differential plate-14, an ion lens I-15, an ion lens II-16, an octapole ion guide rod-17, a slit-18, a reflection type mass spectrum device-19, an ion detection device-20 and a data acquisition system-21.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The utility model aims to provide a device for effectively inhibiting generation and transmission of water cluster ions in an associated ionization mass spectrometer, wherein a uniform electric field can be formed between an ionizer and a differential plate, and the collision kinetic energy of the water cluster ions and background gas is increased by adjusting the intensity of the electric field, so that the water cluster ions are converted into H with small molecular weight 3 O + Suppression of H by low quality discrimination combined with octapole ion guide 3 O + Thereby achieving the purpose of effectively inhibiting generation and transmission of water cluster ions in the associated ionization mass spectrometer.
In order that the above-recited objects, features and advantages of the present utility model will become more readily apparent, a more particular description of the utility model will be rendered by reference to the appended drawings and appended detailed description.
As shown in fig. 1, the present utility model is an apparatus for effectively inhibiting generation and transport of water cluster ions in an associated ionization mass spectrometer, the apparatus comprising: the ion migration system 3 comprises an ion lens I15, an ion lens II 16 and an octupole ion guide rod 17 which are arranged between the ion lens I15 and the ion lens II 16 in a relative mode; the vacuum ultraviolet light source system 1 is used for generating vacuum ultraviolet light; the ionization system 2 is used for enabling a sample and a protonating agent to generate association ionization reaction under the action of the vacuum ultraviolet light to generate ions of an object to be detected; the ion migration system 3 is configured to transmit and focus the object to be detected through an ion lens i 15, an octupole ion guide rod 17 and an ion lens ii 16, and the object to be detected after being transmitted and focused enters the mass spectrum detection system 4; the mass spectrum detection system 4 is used for detecting the ions of the object to be detected.
The vacuum ultraviolet light source system 1 comprises a vacuum ultraviolet lamp tube 5 and a radio frequency generator 6, the ionization system 2 comprises a sample inlet tube 8, an analysis device 9, a sample inlet tube 10 and an ionizer 11, and the mass spectrum detection system 4 comprises a reflection type mass spectrum device 19, an ion detection device 20 and a data acquisition system 21.
The vacuum ultraviolet light source system 1 and the ionization system 2 are connected by a magnesium fluoride lens or a lithium fluoride lens 7, the ionization system 2 and the ion migration system 3 are connected by a differential plate 14, and the ion migration system 3 and the mass spectrum detection system 4 are connected by a slit 18.
The vacuum required for ionization system 2, ion mobility system 3 and mass spectrometry detection system 4 is provided and maintained by molecular pump 12.
The vacuum ultraviolet lamp 5 is a krypton lamp, an argon lamp or a xenon lamp.
The metal net 13 is tightly attached to the differential plate 14, the metal net 13 completely covers the small hole in the center of the differential plate 14, and the metal net 13 is positioned on one side of the differential plate 14 close to the ionizer 11; the outlet end face of the ionizer is parallel to the differential plate, the structure can lead the ionizer 11 and the differential plate 14 to form a uniform electric field therebetween, the electric field is enhanced by properly increasing the voltage difference between the ionizer 11 and the differential plate 14, the collision kinetic energy of water cluster ions and background gas can be increased, the water cluster ions are declustered and converted into small molecular weight hydrated protons (H 3 O + ) The method comprises the steps of carrying out a first treatment on the surface of the Due to the low mass discrimination effect of the octupole ion guide 17, H is generated 3 O + Is effectively inhibited when passing through the octupole ion guide rod 17; thereby preventing a large amount of water cluster ions from entering the mass spectrometry detection system 4, and greatly reducing the background signal of the mass spectrum.
The central axes of the vacuum ultraviolet lamp tube 5, the magnesium fluoride lens or the lithium fluoride lens 7, the ionizer 11, the differential plate 14, the ion lens I15, the octupole ion guide rod 17, the ion lens II 16 and the slit 18 are positioned on the same straight line, and are sequentially arranged in sequence from front to back.
The sample introducing pipe 8, the analyzing device 9 and the sample introducing pipe 10 are sequentially connected with the ionizer 11, and the gas sample introducing direction is perpendicular to the vacuum ultraviolet irradiation direction.
After the sample enters the analysis device 9 through the sample inlet pipe 8, the sample gas enters the ionizer 11 through the sample inlet pipe 10, the sample gas undergoes association reaction under the irradiation of the vacuum ultraviolet lamp to generate ions of a substance to be detected, and the generated ions enter the reflection type mass spectrum device 19 after being transmitted and focused through the ion migration system 3, and then are subjected to signal recording by the ion detection device 20 and the data acquisition system 21.
The protonating agent in the association ionization reaction is methylene dichloride, and the sample can be one or more of gas state, liquid state, solid state and aerosol state.
The octupole ion guide rod 17 is composed of eight parallel columnar electrodes which are arrayed in a circumferential array, the potentials of the two electrodes are the same, the potentials of the two adjacent electrodes are opposite, and a radio frequency alternating voltage is provided for each electrode by a radio frequency power supply.
Examples
Step 1: the excited gas in the vacuum ultraviolet lamp tube 5 generates vacuum ultraviolet light under the action of the radio frequency generator 6, and the generated vacuum ultraviolet light enters the ionizer 11 through the magnesium fluoride lens or the lithium fluoride lens 7.
Step 2: the sample enters the analysis device 9 through the sample introduction pipe 8, and the generated gas phase sample enters the ionizer 11 through the sample introduction pipe 10.
Step 3: under the action of vacuum ultraviolet light, the sample and the methylene dichloride are subjected to a counter association ionization reaction in the ionizer 11 to generate ions of the object to be detected.
Step 4: the generated ions of the object to be detected enter the ion migration system 3 through the metal net 13 and the differential plate 14, and the ions enter the mass spectrum detection system 4 through the slit 18 after sequentially passing through the ion lens I15, the octupole ion guide rod 17 and the ion lens II 16.
According to the specific embodiment provided by the utility model, the utility model discloses the following technical effects:
an apparatus for effectively inhibiting generation and transport of water cluster ions in an associated ionization mass spectrometer in an embodiment of the utility model, the apparatus comprising: the ion migration system comprises an ion lens I, an ion lens II and an octupole ion guide rod which are arranged between the ion lens I and the ion lens II in a relative mode; the vacuum ultraviolet light source system is used for generating vacuum ultraviolet light; the ionization system is used for enabling a sample and a protonating agent to generate association ionization reaction under the action of the vacuum ultraviolet light to generate ions of an object to be detected; the ion migrationThe system is used for transmitting and focusing the ions of the object to be detected through the ion lens I, the octupole ion guide rod and the ion lens II, and the transmitted and focused ions of the object to be detected enter the mass spectrum detection system; the mass spectrum detection system is used for detecting the ions of the object to be detected; the ionizer and the differential plate provided by the embodiment of the utility model can form a uniform electric field therebetween, and the collision kinetic energy of water cluster ions and background gas can be increased by properly increasing the voltage difference between the ionizer and the differential plate and enhancing the electric field, so that the water cluster ions are declustered and converted into H with small molecular weight 3 O + The method comprises the steps of carrying out a first treatment on the surface of the The low quality discrimination effect of the octapole ion guide rod can effectively inhibit H 3 O + The ion detector is protected, meanwhile, the ionization efficiency of the ion source is fully exerted, the generation and transmission of water cluster ions in the system are effectively inhibited, the background signal height of mass spectrum is reduced, the associated ionization mass spectrometer can be used for detecting trace components, and a novel online detection technology is provided for directly detecting trace polar organic matters such as oxygen, nitrogen, phosphorus and the like.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
The principles and embodiments of the present utility model have been described herein with reference to specific examples, the description of which is intended only to assist in understanding the methods of the present utility model and the core ideas thereof; also, it is within the scope of the present utility model to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the utility model.
Claims (9)
1. An apparatus effective to inhibit generation and transport of water cluster ions in an associated ionization mass spectrometer, the apparatus comprising: the ion migration system comprises an ion lens I, an ion lens II and an octupole ion guide rod which are arranged between the ion lens I and the ion lens II in a relative mode;
the vacuum ultraviolet light source system is used for generating vacuum ultraviolet light;
the ionization system is used for enabling a sample and a protonating agent to generate association ionization reaction under the action of the vacuum ultraviolet light to generate ions of an object to be detected;
a metal mesh and a differential plate are arranged between an ionizer in the ionization system and the ion migration system;
the metal net is attached to the center of one side, close to the ionization system, of the differential plate and covers a through hole in the center of the differential plate;
the ion migration system is used for transmitting and focusing the ions of the to-be-detected object through the ion lens I, the octupole ion guide rod and the ion lens II, and the transmitted and focused ions of the to-be-detected object enter the mass spectrum detection system;
the mass spectrum detection system is used for detecting the ions of the object to be detected.
2. The apparatus of claim 1, wherein the vacuum ultraviolet light source system comprises a vacuum ultraviolet light tube and a radio frequency generator.
3. The apparatus of claim 2, wherein a magnesium fluoride lens or a lithium fluoride lens is disposed between the vacuum ultraviolet lamp and the ionizer of the ionization system, and vacuum ultraviolet light is transmitted through the magnesium fluoride lens or the lithium fluoride lens into the ionizer.
4. The apparatus of claim 1, wherein the ionization system comprises a sample introduction tube, a resolving device, a sample introduction tube, and an ionizer connected in sequence;
one end of the sample introducing pipe is connected with one end of the analyzing device, the other end of the analyzing device is connected with one end of the sample introducing pipe, and the other end of the sample introducing pipe is communicated with the ionizer.
5. The apparatus of claim 4, wherein the sample introduction tube of the ionization system is oriented perpendicular to the direction of vacuum ultraviolet light irradiation.
6. The apparatus of claim 1, wherein the ion transfer system and the mass spectrometry detection system are in communication via a slit; and the transmitted and focused object ions enter the reflection type mass spectrum device of the mass spectrum detection system through the slit.
7. The apparatus of claim 1, wherein the mass spectrometry detection system comprises a reflection mass spectrometry device, an ion detection device, and a data acquisition device;
the ion detection device is arranged at the outlet of the reflection type mass spectrum device and is connected with the data acquisition device.
8. The apparatus of claim 1, wherein the ionization system, the ion mobility system, and the mass spectrometry detection system are disposed in separate vacuum chambers, and wherein a molecular pump is disposed on a sidewall of the vacuum chamber for maintaining a vacuum environment required for the ionization system, the ion mobility system, and the mass spectrometry detection system.
9. An ionization system in an apparatus according to any one of claims 1 to 8.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202320078316.7U CN219066754U (en) | 2023-01-10 | 2023-01-10 | Device for effectively inhibiting generation and transmission of water cluster ions in associated ionization mass spectrometer |
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| CN202320078316.7U CN219066754U (en) | 2023-01-10 | 2023-01-10 | Device for effectively inhibiting generation and transmission of water cluster ions in associated ionization mass spectrometer |
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