CN115274398A - Composite ion source and radio frequency power supply circuit thereof - Google Patents

Composite ion source and radio frequency power supply circuit thereof Download PDF

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Publication number
CN115274398A
CN115274398A CN202210923043.1A CN202210923043A CN115274398A CN 115274398 A CN115274398 A CN 115274398A CN 202210923043 A CN202210923043 A CN 202210923043A CN 115274398 A CN115274398 A CN 115274398A
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torch
discharge tube
vacuum
coil
quadrupole deflection
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CN202210923043.1A
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CN115274398B (en
Inventor
刘广才
李振
李亮
王晶
冯新用
郭宇
曹祥宽
卢会峰
凌星
程文播
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Guoke Xinzhi Tianjin Technology Development Co ltd
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Tianjin Guoke Medical Technology Development Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/022Circuit arrangements, e.g. for generating deviation currents or voltages ; Components associated with high voltage supply
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/26Mass spectrometers or separator tubes

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to a composite ion source and a radio frequency power supply circuit thereof, wherein a torch tube and a torch tube coil of the composite ion source are positioned in a low vacuum region, the torch tube coil is wound on the torch tube, a vacuum slide valve, a photoionization device, a quadrupole deflection device and a focusing lens group are positioned in a high vacuum region, the photoionization device is arranged on the quadrupole deflection device, a vacuum interface and a sample injection capillary tube are connected with the low vacuum region and the high vacuum region through the vacuum slide valve, the torch tube is opposite to the vacuum interface, ions enter the quadrupole deflection region in the quadrupole deflection device through the vacuum interface or the sample injection capillary tube, and the ions discharged from the quadrupole deflection region enter the focusing lens group. According to the invention, through the design of an ion source structure and an electric control system in the mass spectrum, the combination of an inductively coupled plasma ionization source and a photoionization source is realized, so that the instrument can detect volatile organic compounds and heavy metal elements, the multi-substance detection application of the instrument is ensured, and the detection of water quality is more convenient and faster.

Description

Composite ion source and radio frequency power supply circuit thereof
Technical Field
The invention relates to the technical field of ionization, in particular to a composite ion source and a radio frequency power supply circuit thereof.
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 an object to be detected by a certain means and then screen 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 the sample molecules can be effectively ionized can directly influence important indexes such as the type of a detectable substance, the detection limit and the like. There are many types of ion sources, and different types of ion sources can analyze different substances, for example, inductively coupled plasma Ionization (ICP) sources mainly analyze inorganic substances, electron impact ionization (EI) sources and Photoionization (PI) sources mainly analyze Volatile Organic Compounds (VOCs), electrospray ionization (ESI) sources and Atmospheric Pressure Chemical Ionization (APCI) sources mainly analyze macromolecular organic compounds, and the like.
In recent years, with the industrial development, the water pollution of rivers and lakes is serious, water resources are closely related to the survival, the life and the production of people in natural environment, water quality monitoring can provide scientific basis for water environment management, pollution source control, environment planning and the like, and the method has an important role in preventing and treating water pollution. However, the existing detection means can only detect one kind of substances in water, for example, some instruments can detect volatile organic compounds in water, some instruments can detect heavy metal elements in water, and the instruments cannot meet the detection of all water quality parameters.
Disclosure of Invention
To achieve the above object and other advantages in accordance with the present invention, a first object of the present invention is to provide a complex ion source comprising: torch, torch coil, vacuum interface, advance kind capillary, vacuum slide valve, photoionization device, quadrupole deflection device, focusing lens group, the torch coil is located low vacuum region, the torch coil is around on the torch, the vacuum slide valve the photoionization device the quadrupole deflection device the focusing lens group is located high vacuum region, the photoionization device is installed on the quadrupole deflection device, the vacuum interface advance kind capillary all passes through the vacuum slide valve is connected low vacuum region and high vacuum region, the torch with the vacuum interface is relative, the ion warp the vacuum interface or advance kind capillary entering quadrupole deflection region in the quadrupole deflection device, follow the regional exhaust ion of quadrupole deflection gets into the focusing lens group.
Furthermore, the quadrupole deflection device comprises a quadrupole deflection electrode, a quadrupole deflection inlet electrode, an ion repulsion electrode, a neutral particle discharge electrode and an ion extraction electrode; the quadrupole deflection inlet electrode, the ion repulsion electrode, the neutral particle discharge electrode and the ion extraction electrode are arranged around the quadrupole deflection electrode, the quadrupole deflection inlet electrode is opposite to the neutral particle discharge electrode, the ion repulsion electrode is opposite to the ion extraction electrode, the quadrupole deflection inlet electrode is opposite to the vacuum interface, and the ion extraction electrode is opposite to the focusing lens group.
Further, the photoionization device comprises a discharge tube, a discharge tube coil, a discharge tube mounting plate and an insulating column; the discharge tube mounting plate is mounted on the quadrupole deflection electrode through the insulating column, the discharge tube is mounted on the discharge tube mounting plate, and the discharge tube is wound on the discharge tube.
Furthermore, one end of the discharge tube close to the quadrupole deflection device is provided with an optical window which releases photons into the quadrupole deflection region; the discharge tube is made of quartz glass; argon or krypton gas is filled in the discharge tube.
Furthermore, the insulating column is made of a nylon material or a ceramic material.
Further, the vacuum interface is a vacuum interface cone.
Furthermore, the torch tube is made of quartz glass; argon is introduced into the torch tube.
Furthermore, the sample injection capillary tube is made of quartz glass.
A second object of the present invention is to provide an rf power supply circuit for a composite ion source, comprising: the composite ion source comprises a high-power radio-frequency power supply, a power detection circuit, a resonance matching control circuit, a tuning element and a reflected power detection circuit, wherein the power detection circuit is connected with the high-power radio-frequency power supply and the resonance matching control circuit;
the radio frequency signal output by the high-power radio frequency power supply is coupled to the tuning element through the power detection circuit;
the tuning element outputs a signal to the torch coil, the discharge tube coil;
the reflected power detection circuit detects radio frequency signals reflected by the torch coil and the discharge tube coil and inputs the radio frequency signals to the resonance matching control circuit to generate a group of phase error signals and amplitude error signals;
and the resonance matching control circuit generates a control signal according to the phase error signal and the amplitude error signal to drive the tuning element so that the load coil obtains the maximum power output.
Furthermore, the tuning element comprises two motors, the two motors drive the rotating handle, and the rotating handle is respectively connected with the movable piece of the adjustable capacitor to control the capacitance value of the capacitor;
the resonance matching control circuit generates control signals according to the phase error signals and the amplitude error signals to drive the two motors, and adjusts the position of the movable plate of the adjustable capacitor, so that the loop parameters of the capacitor and the inductance of the load coil reach a resonance state, and the load coil obtains the maximum power output.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a composite ion source and a radio frequency power supply circuit thereof, which realize the combination of an inductively coupled plasma ionization source and a photoionization source through the design of an ion source structure and an electric control system in a mass spectrum, so that an instrument can detect volatile organic compounds and heavy metal elements, the multi-substance detection application of the instrument is ensured, and the detection of water quality is more convenient and faster.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings. The detailed description of the present invention is given in detail 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 limiting the invention. In the drawings:
FIG. 1 is a schematic view of a composite ion source of example 1;
fig. 2 is a schematic structural view of a quadrupole deflection apparatus according to embodiment 1;
fig. 3 is a schematic view of a partial structure of a quadrupole deflection unit according to embodiment 1;
fig. 4 is a schematic diagram of an rf power supply circuit of the composite ion source of embodiment 2.
In the figure: 1. a torch tube; 2. a torch tube coil; 3. a vacuum interface cone; 4. sampling a capillary tube; 5. a vacuum slide valve; 6. a quadrupole deflection device; 61. a quadrupole deflection electrode; 62. a quadrupole deflection entrance electrode; 63. an ion-repelling electrode; 64. a neutral particle discharge electrode; 65. an ion extraction electrode; 7. a focusing lens group; 8. a high vacuum region; 9. a photoionization device; 91. a discharge tube; 92. a discharge tube coil; 93. a discharge tube mounting plate; 94. and an insulating column.
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 any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
Example 1
A source of complex ions, as shown in figure 1, comprising: the device comprises a torch tube 1, a coil 2 of the torch tube 1, a vacuum interface, a sample injection capillary tube 4, a vacuum slide valve 5, a photoionization device 9, a quadrupole deflection device 6 and a focusing lens group 7, wherein the torch tube 1 and the coil 2 of the torch tube 1 are positioned in a low vacuum region such as atmospheric pressure, the coil 2 of the torch tube 1 is wound on the torch tube 1, the vacuum slide valve 5, the photoionization device 9, the quadrupole deflection device 6 and the focusing lens group 7 are positioned in a high vacuum region 8, the photoionization device 9 is installed on the quadrupole deflection device 6, the vacuum interface and the sample injection capillary tube 4 are connected with the low vacuum region and the high vacuum region 8 through the vacuum slide valve 5, the torch tube 1 is opposite to the vacuum interface, ions enter the quadrupole deflection region in the quadrupole deflection device 6 through the vacuum interface or the sample injection capillary tube 4, and the ions discharged from the quadrupole deflection region enter the focusing lens group 7. In this embodiment, the vacuum interface is a vacuum interface cone 3.
As shown in fig. 2 and 3, the quadrupole deflection device 6 includes a quadrupole deflection electrode 61, a quadrupole deflection entrance electrode 62, an ion repulsion electrode 63, a neutral particle discharge electrode 64, and an ion extraction electrode 65; the quadrupole deflection entrance electrode 62, the ion repulsion electrode 63, the neutral particle discharge electrode 64 and the ion extraction electrode 65 are arranged around the quadrupole deflection electrode 61, the quadrupole deflection entrance electrode 62 is opposite to the neutral particle discharge electrode 64, the ion repulsion electrode 63 is opposite to the ion extraction electrode 65, the quadrupole deflection entrance electrode 62 is opposite to the vacuum interface, and the ion extraction electrode 65 is opposite to the focusing lens group 7.
As shown in fig. 2, the photoionization device 9 includes a discharge tube 91, a coil 92 of the discharge tube 91, a discharge tube 91 mounting plate 93, and an insulating post 94; an installation plate 93 for the discharge tube 91 is attached to the quadrupole deflection electrode 61 via an insulating column 94, the discharge tube 91 is installed on the installation plate 93 for the discharge tube 91, and a coil 92 for the discharge tube 91 is wound around the discharge tube 91. In this embodiment, the insulating column 94 is made of nylon or ceramic. The discharge tube 91 is made of quartz glass; argon or krypton is filled in the discharge tube 91, photons with different energies can be generated by different gases under the action of radio frequency voltage, and MgF is adopted at one end close to the quadrupole deflection device 6 2 The optical window is used to release photons into the quadrupole deflection region, i.e., the ionization region of the VOCs.
Aiming at the ionization detection of heavy metal samples, the heavy metal samples are atomized and then are led into a torch tube 1, the torch tube 1 is made of quartz glass materials, argon is introduced into the torch tube 1 and used as auxiliary gas and cooling gas, high-power radio frequency is applied to a coil 2 of the torch tube 1, the argon is changed into high-temperature plasma to act with the heavy metal samples to ionize the heavy metal samples under the action of the high-power radio frequency, a vacuum slide valve 5 on one side of a vacuum interface cone 3 is opened at the moment, the heavy metal ions enter a high vacuum area 8 through the vacuum interface cone 3 and are led into a quadrupole deflection area through a quadrupole deflection inlet electrode 62, the ions are deflected under the action of a quadrupole deflection electrode 61, the ions are discharged from an ion leading-out electrode 65 to the quadrupole deflection area, neutral particles are not influenced by an electric field, and are discharged from a neutral particle discharging electrode 64. The ions extracted from the ion extraction electrode 65 are focused and shaped by the focusing lens group 7, and finally enter a mass analyzer of a mass spectrometer for analysis and detection.
When Volatile Organic Compounds (VOCs) sample ionization detection is performed, headspace sampling is performed on a detection sample, the VOCs enter a sampling capillary tube 4, the sampling capillary tube 4 is made of quartz glass, a vacuum slide valve 5 on one side of the sampling capillary tube 4 is opened at the moment, and the VOCs sample enters a quadrupole deflection area, namely a VOCs ionization area. At this time, radio frequency voltage is applied to the coil 92 of the discharge tube 91, and under the action of the radio frequency voltage, the gas in the discharge tube 91 releases photons, and the photons enter the VOCs ionization region to collide with VOCs molecules, so that the VOCs molecules are ionized into ions. The VOCs ions enter the focusing lens group 7 for focusing and shaping under the action of the ion repulsion electrode 63 and the ion leading-out electrode 65, and finally enter the mass analyzer of the mass spectrum for analysis and detection.
Example 2
An rf power supply circuit for a composite ion source, as shown in fig. 4, comprises: the device comprises a high-power radio frequency power supply, a power detection circuit, a resonance matching control circuit, a tuning element and a reflected power detection circuit, wherein the power detection circuit is connected with the high-power radio frequency power supply and the resonance matching control circuit, the power detection circuit and the resonance matching control circuit are connected with the tuning element, the tuning element is connected with a torch tube 1 coil 2 and a discharge tube 91 coil 92 of a composite ion source, the torch tube 1 coil 2 and the discharge tube 91 coil 92 are connected with the reflected power detection circuit, and the reflected power detection circuit is connected with the resonance matching control circuit;
the tuning element comprises two motors, the two motors drive a rotating handle, and the rotating handle is respectively connected with a moving plate of the adjustable capacitor, so that the capacitance value control of the capacitor is realized, and the impedance matching is realized.
The radio frequency signal output by the high-power radio frequency power supply is coupled to the tuning element through the power detection circuit, and finally output to the coil 2 of the torch tube 1 or the coil 92 of the discharge tube 91 through the tuning element. Because the different inductance values of the coil 2 of the torch 1 and the coil 92 of the discharge tube 91 cause different load impedances, the situation that the load is not matched with the radio frequency signal source can be generated for different loads, so that the power obtained by the load is not the maximum, and a signal reflecting back to the radio frequency source is generated. The output radio frequency signal is detected through the reflected power detection circuit, the reflected radio frequency signal is detected through the reflected power detection circuit, the radio frequency signal is input to the resonance matching control board to generate a group of phase error and amplitude error signals, the resonance matching control circuit generates control signals according to the magnitude of the two error signals to drive the two motors, the positions of the moving pieces of the two tuning elements are adjusted, namely the capacitance values of the two capacitors are adjusted, so that the loop parameters of the two capacitors and the inductance of the load coil reach a resonance state, and the load coil obtains the maximum power output. Wherein, two load coils, namely the coil 2 of the torch 1 and the coil 92 of the discharge tube 91 do not work simultaneously, when one coil works, the other coil is disconnected and is not connected into a loop.
According to the invention, through the design of an ion source structure and an electric control system in the mass spectrum, the combination of an inductively coupled plasma ionization source and a photoionization source is realized, so that the instrument can detect volatile organic compounds and heavy metal elements, the multi-substance detection application of the instrument is ensured, and the detection of water quality is more convenient and faster.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising a," "8230," "8230," or "comprising" does not exclude the presence of additional identical elements in the process, method, article, or apparatus comprising the element.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments.
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. A composite ion source, comprising: torch, torch coil, vacuum interface, advance kind capillary, vacuum slide valve, photoionization device, quadrupole deflection device, focusing lens group, the torch coil is located low vacuum region, the torch coil is around on the torch, the vacuum slide valve the photoionization device the quadrupole deflection device the focusing lens group is located high vacuum region, the photoionization device is installed on the quadrupole deflection device, the vacuum interface advance kind capillary all passes through the vacuum slide valve is connected low vacuum region and high vacuum region, the torch with the vacuum interface is relative, the ion warp the vacuum interface or advance kind capillary entering quadrupole deflection region in the quadrupole deflection device, follow the regional exhaust ion of quadrupole deflection gets into the focusing lens group.
2. The composite ion source of claim 1, wherein: the quadrupole deflection device comprises a quadrupole deflection electrode, a quadrupole deflection inlet electrode, an ion repulsion electrode, a neutral particle discharge electrode and an ion extraction electrode; the ion repulsion electrode is arranged on the periphery of the focusing lens group, and the ion repulsion electrode is arranged on the vacuum interface.
3. The source of claim 2, wherein: the photoionization device comprises a discharge tube, a discharge tube coil, a discharge tube mounting plate and an insulating column; the discharge tube mounting plate is mounted on the quadrupole deflection electrode through the insulating column, the discharge tube is mounted on the discharge tube mounting plate, and the discharge tube is wound on the discharge tube.
4. A source of complex ions according to claim 3, wherein: one end of the discharge tube close to the quadrupole deflection device is provided with an optical window which releases photons into a quadrupole deflection area; the discharge tube is made of quartz glass; argon or krypton gas is filled in the discharge tube.
5. A source of complex ions according to claim 3, wherein: the insulating column is made of a nylon material or a ceramic material.
6. A source of complex ions according to claim 1, wherein: the vacuum interface is a vacuum interface cone.
7. The composite ion source of claim 1, wherein: the torch tube is made of quartz glass; argon is introduced into the torch tube.
8. The composite ion source of claim 1, wherein: the sample injection capillary is made of quartz glass.
9. An rf power supply circuit for a composite ion source, comprising: the composite ion source comprises a high-power radio-frequency power supply, a power detection circuit, a resonance matching control circuit, a tuning element and a reflected power detection circuit, wherein the power detection circuit is connected with the high-power radio-frequency power supply and the resonance matching control circuit;
the radio frequency signal output by the high-power radio frequency power supply is coupled to the tuning element through the power detection circuit;
the tuning element outputs a signal to the torch coil, the discharge tube coil;
the reflected power detection circuit detects radio frequency signals reflected by the torch coil and the discharge tube coil and inputs the radio frequency signals to the resonance matching control circuit to generate a group of phase error signals and amplitude error signals;
and the resonance matching control circuit generates a control signal according to the phase error signal and the amplitude error signal to drive the tuning element so that the load coil obtains the maximum power output.
10. The rf power supply circuit of claim 9, wherein: the tuning element comprises two motors, the two motors drive a rotating handle, and the rotating handle is respectively connected with a moving plate of the adjustable capacitor to control the capacitance value of the capacitor;
the resonance matching control circuit generates control signals according to the phase error signals and the amplitude error signals to drive the two motors, and adjusts the position of the movable plate of the adjustable capacitor, so that the loop parameters of the capacitor and the inductance of the load coil reach a resonance state, and the load coil obtains the maximum power output.
CN202210923043.1A 2022-08-02 2022-08-02 Composite ion source and radio frequency power supply circuit thereof Active CN115274398B (en)

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