CN110289203B - Corona discharge ionization source structure and ion mobility spectrometer - Google Patents
Corona discharge ionization source structure and ion mobility spectrometer Download PDFInfo
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- CN110289203B CN110289203B CN201910477779.9A CN201910477779A CN110289203B CN 110289203 B CN110289203 B CN 110289203B CN 201910477779 A CN201910477779 A CN 201910477779A CN 110289203 B CN110289203 B CN 110289203B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/18—Ion sources; Ion guns using spark ionisation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/24—Vacuum systems, e.g. maintaining desired pressures
Abstract
The utility model provides a corona discharge ionization source structure and ion mobility spectrometer, this corona discharge ionization source structure includes the ionization chamber, sets up first electrode and second electrode in the ionization chamber, first electrode with apply the high pressure between the second electrode with form corona discharge in the ionization chamber, be provided with the air inlet and the gas outlet that are used for carrying the purge gas on the ionization chamber, first electrode sets to needle type electrode, air inlet and gas outlet make through setting up the gas flow direction in the ionization chamber is along the axis direction of needle type electrode blows through the pointed end of needle type electrode. The ionization source structure of the invention can enhance the working stability of the corona discharge ionization source, so that the corona discharge ionization source can continuously and stably discharge, and the high-efficiency and stable ion yield is kept.
Description
Technical Field
The invention relates to the field of ion mobility spectrometry, in particular to a corona discharge ionization source structure and an ion mobility spectrometer.
Background
An Ion Mobility Spectrometry (IMS) technique is a technique for detecting trace-quantified substances, and is a technique for characterizing chemical substances based on differences in migration speeds of gas-phase ions in an electric field, so as to separate and detect different substances. After the sample is carried into the ionization region by the carrier gas, carrier gas molecules and sample molecules generate a series of ionization reactions and ion-molecule reactions under the action of the ion source to form various product ions. Under the drive of an electric field in an ionization region, a flaky ion cluster is cut out through an ion gate, different types of ions in the cluster start to directionally migrate at different speeds in a drift tube (a voltage-dividing resistor is used for a migration tube to generate a uniform electric field), then an ion signal is detected on a Faraday disc to form an ion migration spectrogram, and substances to be detected are distinguished and distinguished from the final spectrogram information.
The ionization source of an ion mobility spectrometer is one of the important components, and the generation of sample ions in the ion mobility spectrometer has been completed by the reaction of sample molecules with ion clusters in an ionization region. Corona Discharge (DC) ionization source is a commonly used ionization source, and its basic principle is that uneven Discharge in a narrow space causes it to have a strong electric field and a tiny current channel in a certain space, which causes the atmospheric gas in the area to undergo proton transfer reaction, thereby forming a plasma gathering area, and when sample molecules enter the ion area, a series of charge transfer reactions occur, and ionization occurs, thereby forming ions.
Corona discharge can form a certain amount of nitrogen oxides, when certain nitrogen oxides are accumulated in the ionization chamber, the corona discharge can be interfered, even the corona is extinguished, and the problem is to be relieved. How to optimize the purging mode of the ionized region purging gas through the structural design, keep the plasma environment of the discharge region as stable as possible, and obtain the corona discharge which is stable and continuous as possible is the problem faced by the prior art.
Disclosure of Invention
The invention mainly aims to overcome the defects of the prior art and provide a corona discharge ionization source structure and an ion mobility spectrometer with the same, so that the working stability of the corona discharge ionization source is enhanced, the corona discharge ionization source can continuously and stably discharge, and the high-efficiency and stable ion yield is kept.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a corona discharge ionization source structure, is in including ionization chamber, setting first electrode and second electrode in the ionization chamber, first electrode with apply the high pressure between the second electrode in order form corona discharge in the ionization chamber, be provided with the air inlet and the gas outlet that are used for carrying the purge gas on the ionization chamber, first electrode sets up to needle type electrode, air inlet and gas outlet make through setting up the gas flow direction in the ionization chamber is along the axis direction of needle type electrode blows the pointed end of needle type electrode.
Further:
the air inlet comprises a pair of air inlets symmetrically arranged relative to the axial direction of the needle-shaped electrode, the air outlet comprises a pair of air outlets symmetrically arranged relative to the axial direction of the needle-shaped electrode, the projection positions of the pair of air inlets and the pair of air outlets in the axial direction of the needle-shaped electrode are staggered with each other, and the tip of the needle-shaped electrode is positioned between the projection positions of the pair of air inlets and the pair of air outlets in the axial direction of the needle-shaped electrode.
The pair of air inlets and the pair of air outlets are provided perpendicularly to the axial direction of the needle-type electrode.
The axis direction of the needle-shaped electrode is along the horizontal direction, and the pair of air inlets and the pair of air outlets are arranged along the vertical direction.
The air inlet is arranged on the front side of the tip of the needle electrode, and the air outlet is arranged on the rear side of the tip of the needle electrode.
Corona discharge ionization source structure is still including the needle type electrode fixed bolster and the air inlet ring structure that have the cavity, the ionization chamber form by needle type electrode fixed bolster with the air inlet ring structure encloses the inside of synthetic cavity, needle type electrode is worn to establish by outer to interior on the cavity diapire of needle type electrode fixed bolster, the second electrode is the loop type electrode, the loop type electrode clamp is established needle type electrode fixed bolster with between the air inlet ring structure, the air inlet sets up on the needle type electrode fixed bolster, the gas outlet sets up on the air inlet ring structure.
The needle-shaped electrode fixing support and the air inlet ring structure are made of Teflon materials.
The first electrode is made of tungsten steel materials, and the second electrode is made of stainless steel materials.
The air inlet with the gas outlet include with the radius 1 mm's that ionization chamber meets through-hole, preferably, the external diameter is connected to the outer end of through-hole than the screw hole of through-hole expansion.
An ion mobility spectrometer is provided with the corona discharge ionization source structure.
The invention has the following beneficial effects:
the invention provides a corona discharge ionization source structure, wherein a first electrode for discharging in an ionization cavity is set as a needle-shaped electrode, and a gas inlet and a gas outlet for conveying purge gas on the ionization cavity are arranged, so that the gas flow direction in the ionization cavity blows over the tip of the needle-shaped electrode along the axial direction of the needle-shaped electrode.
Compared with the prior art, the corona discharge ionization source structure can obtain stable and continuous corona discharge, and the corona discharge ionization source has stronger ionization capacity, obtains higher ionized ion density and can continuously generate high ion current signals. Under the same experimental conditions, the signal intensity obtained by using the corona discharge ionization source structure can reach more than 10 times of that of an ultraviolet ionization source.
Drawings
FIG. 1a is a cross-sectional view of a corona discharge ionization source configuration in accordance with one embodiment of the present invention;
FIG. 1b is a schematic diagram of the corona discharge ionization source configuration of one embodiment of the present invention;
FIG. 2 is an air flow field simulation modeling diagram using one embodiment of the present invention;
FIG. 3 is a simulation of an airflow field using one embodiment of the present invention;
FIG. 4 shows a spectrum of an ultraviolet ionization source and a corona discharge ionization source using an embodiment of the present invention.
Detailed Description
The embodiments of the present invention will be described in detail below. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Referring to fig. 1a to 1b, in an embodiment, a corona discharge ionization source structure includes an ionization chamber, a first electrode 1 and a second electrode 2 disposed in the ionization chamber, a high voltage is applied between the first electrode 1 and the second electrode 2 to form corona discharge in the ionization chamber, an air inlet 3 and an air outlet 4 for conveying purge air are disposed on the ionization chamber, the first electrode 1 is disposed as a needle electrode, and the air inlet 3 and the air outlet 4 are disposed such that a gas flow direction in the ionization chamber blows through a tip of the needle electrode along an axial direction of the needle electrode.
In a preferred embodiment, the gas inlet 3 includes a pair of gas inlets 3 disposed symmetrically with respect to the axial direction of the needle electrode, the gas outlet 4 includes a pair of gas outlets 4 disposed symmetrically with respect to the axial direction of the needle electrode, and the projection positions of the pair of gas inlets 3 and the pair of gas outlets 4 in the axial direction of the needle electrode are shifted from each other, and the tip of the needle electrode is located between the projection positions of the pair of gas inlets 3 and the pair of gas outlets 4 in the axial direction of the needle electrode.
In a more preferred embodiment, the pair of air inlets 3 and the pair of air outlets 4 are provided perpendicularly to the axial direction of the needle electrode.
In a further preferred embodiment, the axial direction of the needle electrode is in the horizontal direction, and the pair of air inlets 3 and the pair of air outlets 4 are arranged in the up-down direction.
In a preferred embodiment, the air inlet 3 is disposed at a front side of a tip of the needle electrode, and the air outlet 4 is disposed at a rear side of the tip of the needle electrode.
In a preferred embodiment, the corona discharge ionization source structure further includes a needle-shaped electrode fixing support 5 and an air inlet ring structure 6, the ionization chamber is formed inside a cavity surrounded by the needle-shaped electrode fixing support 5 and the air inlet ring structure 6, the needle-shaped electrode is arranged on the bottom wall of the cavity of the needle-shaped electrode fixing support 5 in a penetrating manner from outside to inside, the second electrode 2 is a ring-shaped electrode, the ring-shaped electrode is arranged between the needle-shaped electrode fixing support 5 and the air inlet ring structure 6 in a clamping manner, the air inlet 3 is arranged on the needle-shaped electrode fixing support 5, and the air outlet 4 is arranged on the air inlet ring structure 6.
In a preferred embodiment, the needle-shaped electrode fixing support 5 and the air inlet ring structure 6 are made of teflon material.
In a preferred embodiment, the first electrode 1 is made of tungsten steel material, and the second electrode 2 is made of stainless steel material.
In a preferred embodiment, the air inlet 3 and the air outlet 4 comprise through holes with a radius of 1mm, which are connected with the ionization chamber, and more preferably, the outer ends of the through holes are connected with threaded holes with an outer diameter larger than that of the through holes.
In a preferred embodiment, the flow rate of the sample gas is set to 100ml/min and the flow rate of the purge gas of each inlet hole is set to 200 ml/min.
In other embodiments, an ion mobility spectrometer has the corona discharge ionization source structure of any of the preceding embodiments.
The following description of exemplary embodiments and the operation of the present invention will be further described with reference to the accompanying drawings.
As shown in fig. 1a, the corona discharge ionization source structure of one embodiment includes a needle-shaped electrode 1, a needle-shaped electrode fixing bracket 5, a ring-shaped electrode 2, and an air inlet ring structure 6. The needle electrode 1 and the ring electrode 2 form a discharge structure of the corona discharge ionization source. High voltage is applied between the needle-shaped electrode and the annular electrode to form corona, and the air inlet 3 and the air outlet 4 which are symmetrical are respectively designed on the air inlet ring and the needle-shaped electrode fixing support 5 to ensure that the air flowing direction in the structure is along the axis direction of the needle-shaped electrode to blow through the needle-shaped electrode.
Two symmetrical air inlets 3 are arranged on the front side of the ring-shaped electrode; symmetrical air outlets 4 are arranged behind the tip of the needle electrode. The symmetry mode of the present embodiment is symmetrical up and down. But the symmetry is not limited to the upper and lower symmetry.
The needle-shaped electrode 1 is manufactured from a piece of tungsten steel with a radius of curvature of the order of 0.01 mm. The ring-shaped electrode 2 is machined using a piece of stainless steel.
The needle-shaped electrode fixing support 5 and the air inlet ring structure 6 are made of teflon.
Two symmetrical through holes with the radius of 1mm are arranged on the air inlet ring structure 6 and are used as air inlets 3, and 1/4-inch threaded holes are arranged outside the through holes. The needle-shaped electrode fixing bracket 5 is also provided with two symmetrical air outlets 4. Thereby, the direction of the air flow is blown from the ring-shaped electrode to the needle-shaped electrode.
In addition, a 1/4-inch threaded hole is formed in the bottom wall of the cavity of the ring-shaped electrode facing the needle-shaped electrode fixing bracket 5, and a through hole with the radius of 1mm is formed inside the threaded hole and used for installing the needle-shaped electrode 1.
The needle electrode can be clamped by using an 1/4 inch hand tight fitting with a bevel edge ring and the inlet tube can be clamped by using a 1/4 inch hand tight fitting with a bevel edge ring. The air inlet pipe can be filled with high-purity nitrogen for symmetrical air inlet.
High voltage is applied to two ends of the needle electrode 1 and the ring electrode 2 to form a corona discharge process, and a stable and continuous ion signal is obtained.
The flow of the tail gas is set to 1000ml/min, the flow of the sample gas is set to 100ml/min, the flow of the purge gas is set to 200ml/min (each gas inlet), simulation software is used to verify the gas circuit design of the embodiment of the invention, and the obtained flow chart is shown in figure 3.
An ion mobility spectrometer of an embodiment includes: the corona discharge ionization source, the ultraviolet ionization source, the migration tube part assembled by stainless steel and insulating materials in a cross stacking mode, the ion gate mechanical structure and the detection base made of stainless steel, the high-voltage power supply for providing a uniform migration electric field, the high-voltage power supply for providing corona discharge voltage, the voltage division circuit powered by the ultraviolet lamp, the gate control circuit for controlling the ion gate and the signal generator for providing external input signals for the gate control circuit are arranged in the ion gate.
The high-voltage power supply for providing the high voltage of the migration tube selects the output voltage to be 5500V, the corona discharge ring-shaped electrode is connected in a voltage dividing circuit of the migration tube to obtain the potential of 5500V, the first ring of the migration tube obtains the potential of 5000V, namely the ion migration spectrum migration region in the working state obtains the migration voltage of 5000V, and the migration electric field intensity is 40V/cm. The output voltage of the high-voltage power supply for providing corona discharge is 9000V, namely the corona discharge voltage in the working state is 3500V.
The comparison example is ion mobility spectrometry of an ultraviolet ionization source, under the condition that the high-voltage power supply selects the output voltage to be 5250V, and the ultraviolet lamp is divided into a starting voltage of 1200V and a maintaining voltage of 250V by a voltage division circuit. Namely 5000V migration voltage is divided in an ion migration spectrum migration region in a working state, and the migration electric field intensity is 40V/cm.
The access reference voltage of the ion gate is 3850V, the voltage of the gate closing is 80V, and the time of the gate opening is 120 mus. The micro-current amplifier is used for amplification, the oscilloscope is used for signal receiving, a spectrum peak is obtained, and the spectrograms of the two ionization sources are obtained and are shown in figure 4.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and these substitutions and modifications should be considered to fall within the scope of the invention.
Claims (10)
1. A corona discharge ionization source structure, comprising an ionization chamber, a first electrode and a second electrode arranged in the ionization chamber, wherein a high voltage is applied between the first electrode and the second electrode to form corona discharge in the ionization chamber, and the ionization chamber is provided with an air inlet and an air outlet for conveying purge air, wherein the first electrode is arranged as a needle-shaped electrode, and the air inlet and the air outlet are arranged to blow the gas flowing direction in the ionization chamber along the axial direction of the needle-shaped electrode through the tip of the needle-shaped electrode; the air inlet comprises a pair of air inlets symmetrically arranged relative to the axial direction of the needle-shaped electrode, the air outlet comprises a pair of air outlets symmetrically arranged relative to the axial direction of the needle-shaped electrode, the projection positions of the pair of air inlets and the pair of air outlets in the axial direction of the needle-shaped electrode are staggered with each other, and the tip of the needle-shaped electrode is positioned between the projection positions of the pair of air inlets and the pair of air outlets in the axial direction of the needle-shaped electrode.
2. The corona discharge ionization source structure of claim 1 wherein said pair of inlet openings and said pair of outlet openings are disposed perpendicular to the axial direction of said needle electrodes.
3. The corona discharge ionization source structure of claim 2 wherein said needle electrode axis direction is in a horizontal direction and said pair of inlet openings and said pair of outlet openings are arranged in an up and down direction.
4. The corona discharge ionization source structure of any one of claims 1 to 3, wherein said air inlet is disposed on a front side of a tip of said needle electrode and said air outlet is disposed on a rear side of said tip of said needle electrode.
5. The corona discharge ionization source structure according to any one of claims 1 to 3, further comprising a needle-shaped electrode fixing support having a cavity, and an air inlet ring structure, wherein said ionization chamber is formed inside a cavity surrounded by said needle-shaped electrode fixing support and said air inlet ring structure, said needle-shaped electrode is disposed through a bottom wall of said cavity of said needle-shaped electrode fixing support from outside to inside, said second electrode is a ring-shaped electrode, said ring-shaped electrode is sandwiched between said needle-shaped electrode fixing support and said air inlet ring structure, said air inlet is disposed on said needle-shaped electrode fixing support, and said air outlet is disposed on said air inlet ring structure.
6. The corona discharge ionization source structure of claim 5 wherein said needle electrode mounting bracket and said air inlet ring structure are of teflon material.
7. The corona discharge ionization source structure of any one of claims 1 to 3, wherein said first electrode is made of tungsten steel material and said second electrode is made of stainless steel material.
8. The corona discharge ionization source structure of any one of claims 1 to 3, wherein said gas inlet and said gas outlet comprise a through hole of radius 1mm bordering said ionization chamber.
9. The corona discharge ionization source structure of claim 8 wherein said through hole has an outer end connected to a threaded hole having an outer diameter that is enlarged relative to said through hole.
10. An ion mobility spectrometer having a corona discharge ionization source structure as claimed in any one of claims 1 to 9.
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| CN113198629B (en) * | 2021-04-27 | 2023-01-06 | 宁波立成涂装技术有限公司 | Powder electrostatic spray gun and assembly thereof |
| CN114864373B (en) * | 2022-04-25 | 2023-08-11 | 苏州大学 | Corona discharge ion source |
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