CN111199864B - Radio frequency enhanced reaction photochemical ionization source - Google Patents
Radio frequency enhanced reaction photochemical ionization source Download PDFInfo
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- CN111199864B CN111199864B CN201811381275.9A CN201811381275A CN111199864B CN 111199864 B CN111199864 B CN 111199864B CN 201811381275 A CN201811381275 A CN 201811381275A CN 111199864 B CN111199864 B CN 111199864B
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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
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/062—Ion guides
- H01J49/063—Multipole ion guides, e.g. quadrupoles, hexapoles
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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
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/161—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission using photoionisation, e.g. by laser
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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
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/161—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission using photoionisation, e.g. by laser
- H01J49/164—Laser desorption/ionisation, e.g. matrix-assisted laser desorption/ionisation [MALDI]
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Abstract
The invention relates to a mass spectrometer, in particular to a radio frequency enhanced reaction photochemical ionization source for mass spectrometer, which mainly comprises an ultraviolet light source, a convergent lens, a reagent molecule sample inlet pipe, an ion generation area, a sample molecule sample inlet pipe, a conical radio frequency three-pole ion reaction area, an ion extraction electrode and the like. The ionization utilizes an ultraviolet light source to generate reagent ions, can flexibly select the reagent ions, and has good universality; the conical radio frequency three-pole rod improves ion collision frequency under medium air pressure, enhances performances such as focusing and the like, can improve the transmission efficiency of ions and the probability of molecular ion reaction, realizes the enhancement of ionization efficiency of a photochemical ionization source, and further improves the detection sensitivity of an instrument.
Description
Technical Field
The invention relates to a mass spectrometry instrument, in particular to a radio frequency enhanced reaction photochemical ionization source. According to the ionization device, the ultraviolet light source is utilized to generate reagent ions, the ion collision frequency is improved under the medium air pressure through the conical radio frequency three-pole rod, the performances such as focusing and the like are enhanced, the transmission efficiency of the ions and the probability of molecular ion reaction are improved, the ionization efficiency of the photo-induced chemical ionization source is enhanced, and the detection sensitivity of the instrument is improved.
Background
The soft ionization mass spectrometry technology gradually becomes one of the main technologies for online monitoring and rapid analysis of VOCs in complex samples due to the advantages of simple spectrogram, few overlapped peaks and the like. Photoionization is a commonly used mass spectrometry soft ionization technique, and the commonly used light source is a vacuum ultraviolet light source.
Li et al (anal. chem.2016,88, 5028-. The ionization technology generates dibromomethane reagent gas through photoionization of VUV Kr lamp (photon energy is 10.6eV)High strength and pure CH2Br2 +Reagent ion, CH2Br2 +Carrying out charge transfer reaction or ion association reaction with sample molecules to generate molecular ions M+Or addition of an ion [ M + CH ]2Br2]+The lowest detection limit of common Volatile Sulfur Compounds (VSCs) can reach 10 pptv. Has higher detection sensitivity, and the specific addition ions are beneficial to spectrogram recognition.
However, the ionization source ion generation region and the ion-molecule reaction region for sample molecule ionization are in the same region, and the conditions (pressure, voltage, etc.) for reagent ion generation and sample molecule chemical ionization cannot be optimized separately; in addition, the ion-molecule reaction area adopts a uniform electrostatic field transmission design, the divergence caused by ion collision is serious along with the increase of air pressure, the electrostatic field is difficult to effectively restrict the ion-molecule reaction area, and the ion transmission efficiency is low.
The radio frequency multipole rod transmission technology has excellent focusing performance, repeatedly collides with neutral gas under the action of a charged ion alternating electric field, and is gradually cooled to the axis of the multipole rod, so that the utilization rate and the transmission efficiency of ions are greatly improved. If the ion source is used in a chemical ionization source, the collision frequency of the sample and reagent ions can be increased, and the ionization efficiency is improved.
Disclosure of Invention
The invention aims to generate reagent ions by utilizing an ultraviolet light source, improve ion collision frequency under medium air pressure by a conical radio frequency three-pole rod, enhance performances such as focusing and the like, improve ion transmission efficiency and the probability of molecular ion reaction, and realize enhancement of ionization efficiency of a photochemical ionization source, thereby improving detection sensitivity of an instrument.
In order to achieve the purpose, the invention adopts the technical scheme that:
the radio frequency enhanced reaction photochemical ionization source for mass spectrometry comprises an ultraviolet light source, a convergent lens, a clean gas sample inlet pipe, a reagent ion generation source cavity, a reagent ion repulsion electrode, a reagent ion transmission hole, a sample inlet pipe, an ion molecule reaction zone cavity, a conical three-pole rod and an ion extraction electrode; the upward direction is the Y direction, and the rightward direction is the X direction;
the reagent ion generating source cavity is a hollow closed cavity, a plate-shaped reagent ion repulsion electrode with a through hole in the middle and a plate-shaped reagent ion transmission electrode with a through hole in the middle are arranged in parallel in the cavity, and the reagent ion repulsion electrode and the through hole in the middle of the reagent ion transmission electrode are coaxial;
the right side of the cavity of the reagent ion generation source is provided with an ion molecule reaction area cavity which is a hollow closed cavity, and the right side wall surface of the cavity of the reagent ion generation source is provided with an ion transmission hole communicated with the cavity of the ion molecule reaction area;
the ultraviolet light source is fixed above the reagent ion generation source cavity, the converging lens is fixed in a through hole at the top of the reagent ion generation source cavity and is opposite to the position under the ultraviolet light source, the peripheral edge of the converging lens is hermetically connected with the inner wall surface of the through hole at the top, and ultraviolet light emitted by the ultraviolet light source irradiates between the reagent ion repulsion electrode at the left side and the reagent ion transmission electrode at the right side after being converged by the converging lens; the clean gas sample inlet pipe penetrates through the upper part of the reagent ion generation source cavity from the outside and enters the cavity, and the outlet of the clean gas sample inlet pipe faces the lower surface of the convergent lens; the reagent gas sample inlet pipe penetrates through the left side wall surface of the reagent ion generation source cavity from the outside to enter the inside, the position of the reagent gas sample inlet pipe is arranged between the inner wall of the reagent ion generation source cavity and the reagent ion repulsion electrode, and the outlet of the pipeline faces to the axis of the through hole in the middle of the reagent ion repulsion electrode; the cavity of the ion molecule reaction area is connected with the mass analyzer through an ion through hole in the middle of the ion extraction electrode;
the reagent ion repulsion electrode, the reagent ion transmission electrode and the reagent ion transmission hole are all flat plate structures with through holes in the middle, and are arranged in parallel along the X direction and coaxially with the central through hole;
a conical three-pole rod is arranged in the cavity of the ion molecule reaction area;
the sample inlet pipe penetrates through the ion molecule reaction zone cavity from the outside to the inside, and the position of the sample inlet pipe is arranged between the reagent ion transmission hole and the conical tripolar rod;
the conical three-pole rod consists of three cylindrical long electrodes with the same diameter and length, the three cylindrical long electrodes are symmetrically and uniformly distributed along a center, three central points of the end surfaces of the left side and the right side are respectively connected to form an equilateral triangle, and the side length of the equilateral triangle formed by the end surfaces of one side close to the ion extraction electrode is smaller than that of the side close to the sample inlet pipe; the central symmetry axes of the three cylindrical long electrodes are coaxial with the central through hole of the ion extraction electrode.
The diameter of the outlet of the reagent gas sample inlet pipe is 1-10 mm; the diameter of the reagent ion transmission hole is 0.5-5 mm; the diameter of the through hole in the middle of the extraction electrode is 0.5-2 mm; the distance between the reagent ion repulsion electrode and the reagent ion transmission electrode is 2-10 mm.
Different voltages V1, V2, V3 and V4 are sequentially loaded on the reagent ion repulsion electrode, the reagent ion transmission hole and the extraction electrode from high to low, and an ion transmission electric field with the size of 1-50V/cm is formed in the axial direction.
The three cylindrical long electrodes are all applied with radio frequency voltage with the same frequency and peak value, the peak value of the radio frequency voltage is 40-1000V, the radio frequency is 0.1-5 MHz, and the radio frequency phases are different by 120 degrees; the applied radio frequency voltage is superposed with a direct current voltage V5, and the voltage of V5 is between V3 and V4, so as to ensure the smooth extraction of ions.
The clean gas sample inlet pipe, the reagent gas sample inlet pipe and the sample inlet pipe can be metal capillary tubes, PEEK capillary tubes or quartz capillary tubes, and can be one or more; the length is 0.05-5 m and the inner diameter is 25-500 μm.
The extraction electrode is connected with a mass analyzer, wherein the mass analyzer is a flight time mass analyzer, a quadrupole rod mass analyzer or an ion trap mass analyzer.
The ultraviolet light source is a gas discharge lamp light source, a laser light source or a synchrotron radiation light source.
The invention utilizes the ultraviolet light source to generate reagent ions, can flexibly select the reagent ions and has good universality; the ion collision frequency is improved through the conical radio frequency three-pole rod under the medium air pressure, the performances such as focusing and the like are enhanced, the ionization efficiency of the photo-induced chemical ionization source is enhanced, and therefore the detection sensitivity of the instrument is improved. The whole set of ionization source is small in size and compact in structure, can be connected with analyzers with different masses, and has wide application prospect in the aspect of high-sensitivity rapid detection.
Drawings
FIG. 1 is a diagram of an RF-enhanced reactive photochemical ionization source of the present invention.
Detailed Description
Referring to fig. 1, the present invention provides a radio frequency enhanced reaction photo-chemical ionization source for mass spectrometry, including an ultraviolet light source 1, a converging lens 2, a clean gas sample inlet tube 3, a reagent gas sample inlet tube 6, a reagent ion generation source cavity 8, a reagent ion repulsion electrode 7, a reagent ion transmission electrode 9, a reagent ion transmission hole 16, a sample inlet tube 11, sample molecules 10, an ion molecule reaction region cavity 12, a conical three-pole rod 13, and an ion extraction electrode 14;
the upward direction is the Y direction, and the rightward direction is the X direction;
the reagent ion generation source cavity 8 is a hollow closed cavity, a plate-shaped reagent ion repulsion electrode 7 with a through hole in the middle and a plate-shaped reagent ion transmission electrode 9 with a through hole in the middle are arranged in parallel in the cavity, and the through holes in the middle of the reagent ion repulsion electrode 7 and the reagent ion transmission electrode 9 are coaxial;
an ion molecule reaction area cavity 12 is arranged on the right side of the reagent ion generation source cavity 8 and is a hollow closed cavity, and an ion transmission hole 16 communicated with the ion molecule reaction area cavity 12 is arranged on the wall surface of the right side of the reagent ion generation source cavity 8;
the ultraviolet light source 1 is fixed above the reagent ion generation source cavity 8, the convergent lens 2 is fixed in a through hole at the top of the reagent ion generation source cavity 8 and is opposite to the position under the ultraviolet light source 1, the peripheral edge of the convergent lens 2 is hermetically connected with the inner wall surface of the through hole at the top, and ultraviolet light emitted by the ultraviolet light source 1 is converged by the convergent lens 2 and then irradiates between the reagent ion repulsion electrode 7 at the left side and the reagent ion transmission electrode 9 at the right side; the clean gas sample inlet pipe 3 penetrates through the upper part of the reagent ion generation source cavity 8 from the outside to enter the cavity, and the outlet of the clean gas sample inlet pipe faces the lower surface of the convergent lens 2; the reagent gas sample inlet pipe 6 penetrates through the left side wall surface of the reagent ion generation source cavity 8 from the outside to enter the inside, the position of the reagent gas sample inlet pipe is arranged between the inner wall of the reagent ion generation source cavity 8 and the reagent ion repulsion electrode 7, and the outlet of the pipeline faces to the axis of the through hole in the middle of the reagent ion repulsion electrode 7; the reagent ion generation source cavity 8 is connected with the ion molecule reaction area cavity 12 through a reagent ion transmission hole 16, the right side wall surface of the ion molecule reaction area cavity 12 is provided with an ion extraction electrode 14, and the ion molecule reaction area cavity 12 is connected with a connection mass analyzer 15 through an ion through hole in the middle of the ion extraction electrode 14;
the reagent ion repulsion electrode 7, the reagent ion transmission electrode 9, the reagent ion transmission hole 16 and the ion leading-out electrode 14 are all flat plate structures with through holes in the middle and are parallel along the X direction and coaxially arranged with the central through hole;
a conical three-pole rod 13 is arranged in the ion molecule reaction zone cavity 12;
the sample inlet pipe 11 penetrates through the ion molecule reaction area cavity 12 from the outside to the inside, and the position of the sample inlet pipe is arranged between the reagent ion transmission hole 16 and the conical three-pole rod 13;
the conical three-pole rod 13 is composed of three cylindrical long electrodes 18 with the same diameter and length, the three cylindrical long electrodes 18 are symmetrically and uniformly distributed along a center, three central points of the end surfaces of the left side and the right side are respectively connected to form an equilateral triangle, and the side length of the equilateral triangle formed by the end surfaces of one side close to the ion leading-out electrode 14 is smaller than that of one side close to the sample molecules 10; the central symmetry axes of the three cylindrical long electrodes 18 are coaxial with the central through hole of the ion extraction electrode 14.
The diameter of the outlet of the reagent gas sample inlet pipe 6 is 1-10 mm; the diameter of the reagent ion transmission hole 16 is 0.5-5 mm; the diameter of the through hole in the middle of the extraction electrode 14 is 0.5-2 mm; the distance between the reagent ion repulsion electrode 7 and the reagent ion transmission electrode 9 is 2-10 mm.
Different voltages V1, V2, V3 and V4 are sequentially applied to the reagent ion repulsion electrode 7, the reagent ion transmission electrode 9, the reagent ion transmission hole 16 and the extraction electrode 14 from high to low, and an ion transmission electric field with the size of 1-50V/cm is formed in the axial direction.
The three cylindrical long electrodes 18 are all applied with radio frequency voltages with the same frequency and peak value, the peak value of the radio frequency voltage is 40-1000V, the radio frequency is 0.1-5 MHz, and the radio frequency phases are different by 120 degrees; the applied radio frequency voltage is superposed with a direct current voltage V5, and the voltage of V5 is between V3 and V4, so as to ensure the smooth extraction of ions.
The clean gas sample inlet pipe 3, the reagent gas sample inlet pipe 6 and the sample inlet pipe 11 can be metal capillary, PEEK capillary or quartz capillary, and can be one or more; the length is 0.05-5 m and the inner diameter is 25-500 μm.
The extraction electrode 14 is connected to a mass analyser 15 which may be a time of flight mass analyser, a quadrupole mass analyser or an ion trap mass analyser. The ultraviolet light source 1 is a gas discharge lamp light source, a laser light source or a synchrotron radiation light source.
In specific implementation, the reagent gas 5 enters the reagent ion generation source cavity 8 through the reagent gas sampling tube 6, and ultraviolet light generated by the ultraviolet light source 1 irradiates the reagent gas 5 in the reagent ion generation source cavity 8 through the convergent lens 2 to generate reagent ions; clean gas 4 enters the reagent ion generation source cavity 8 through the clean gas sample inlet pipe 3 and sweeps the surface of the lens, so that the pollution of organic matters on the surface of the lens is avoided, and the yield of reagent ions is prevented from being influenced; reagent ions enter the ion molecule reaction zone cavity 12 through the reagent ion transmission holes 16 under the combined action of the reagent ion repulsion electrode 7 and the reagent ion transmission electrode 9; sample molecules 10 enter an ion molecule reaction zone cavity 12 through a sample inlet pipe 11, and are subjected to high-efficiency ion molecule reaction ionization with reagent ions entering the ion reaction zone cavity under the action of a radio frequency conical three-pole rod 13; the same amplitude of rf voltage is applied to the multipole rods with a phase difference of 120 °, a dc voltage is superimposed on the applied rf voltage and the resulting reagent ions are propelled by the dc voltage through the extraction electrode 14 into the mass analyser.
Claims (7)
1. The radio frequency enhanced reaction photochemical ionization source for mass spectrometry comprises an ultraviolet light source (1), a convergent lens (2), a clean gas sample inlet pipe (3), a reagent gas sample inlet pipe (6), a reagent ion generation source cavity (8), a reagent ion repulsion electrode (7), a reagent ion transmission electrode (9), a reagent ion transmission hole (16), a sample inlet pipe (11), sample molecules (10), an ion molecule reaction zone cavity (12), a conical three-pole rod (13) and an ion extraction electrode (14); the method is characterized in that:
the upward direction is the Y direction, and the rightward direction is the X direction;
the reagent ion generation source cavity (8) is a hollow closed cavity, a plate-shaped reagent ion repulsion electrode (7) with a through hole in the middle and a plate-shaped reagent ion transmission electrode (9) with a through hole in the middle are arranged in parallel in the cavity, and the through holes in the middle of the reagent ion repulsion electrode (7) and the reagent ion transmission electrode (9) are coaxial;
an ion molecule reaction area cavity (12) which is a hollow closed cavity is arranged on the right side of the reagent ion generation source cavity (8), and an ion transmission hole (16) communicated with the ion molecule reaction area cavity (12) is arranged on the right side wall surface of the reagent ion generation source cavity (8);
the ultraviolet light source (1) is fixed above the reagent ion generation source cavity (8), the converging lens (2) is fixed in a through hole at the top of the reagent ion generation source cavity (8) and is right below the ultraviolet light source (1), the peripheral edge of the converging lens (2) is hermetically connected with the inner wall surface of the through hole at the top, and ultraviolet light emitted by the ultraviolet light source (1) is converged by the converging lens (2) and then irradiates between the reagent ion repulsion electrode (7) at the left side and the reagent ion transmission electrode (9) at the right side; the clean gas sample inlet pipe (3) penetrates through the upper part of the reagent ion generation source cavity (8) from the outside to enter the cavity, and the outlet of the clean gas sample inlet pipe faces the lower surface of the convergent lens (2); the reagent gas sample inlet pipe (6) penetrates through the left side wall surface of the reagent ion generation source cavity (8) from the outside to enter the inside, the position of the reagent gas sample inlet pipe is arranged between the inner wall of the reagent ion generation source cavity (8) and the reagent ion repulsion electrode (7), and the outlet of the pipeline faces to the axis of the through hole in the middle of the reagent ion repulsion electrode (7); the reagent ion generation source cavity (8) is connected with the ion molecule reaction area cavity (12) through a reagent ion transmission hole (16), an ion extraction electrode (14) is arranged on the right side wall surface of the ion molecule reaction area cavity (12), and the ion molecule reaction area cavity (12) is connected with a connection mass analyzer (15) through an ion through hole in the middle of the ion extraction electrode (14);
the reagent ion repulsion electrode (7), the reagent ion transmission electrode (9), the reagent ion transmission hole (16) and the ion leading-out electrode (14) are all of a flat plate structure with a through hole in the middle, and are parallel along the X direction and coaxially arranged with the central through hole;
a conical three-pole rod (13) is arranged in the ion molecule reaction zone cavity (12);
sample molecules (10) enter the ion molecule reaction area cavity (12) through the sample inlet pipe (11); the sample inlet pipe (11) penetrates through the ion molecule reaction zone cavity (12) from the outside to the inside, and the position of the sample inlet pipe is arranged between the reagent ion transmission hole (16) and the conical three-pole rod (13);
the conical three-pole rod (13) consists of three cylindrical long electrodes (18) with the same diameter and length, the three cylindrical long electrodes (18) are symmetrically and uniformly distributed along a center, three central points of the end surfaces of the left side and the right side are respectively connected to form an equilateral triangle, and the side length of the equilateral triangle formed by the end surfaces of one side close to the ion extraction electrode (14) is smaller than that of one side close to the sample inlet tube (11); the central symmetry axes of the three cylindrical long electrodes (18) are coaxial with the central through hole of the ion extraction electrode (14).
2. The photochemical ionization source as claimed in claim 1, characterized in that:
the diameter of the outlet of the reagent gas sample inlet pipe (6) is 1-10 mm; the diameter of the reagent ion transmission hole (16) is 0.5-5 mm; the diameter of the through hole in the middle of the leading-out electrode (14) is 0.5-2 mm; the distance between the reagent ion repulsion electrode (7) and the reagent ion transmission electrode (9) is 2-10 mm.
3. The photochemical ionization source as claimed in claim 1, characterized in that:
different voltages V1, V2, V3 and V4 are sequentially applied to the reagent ion repulsion electrode (7), the reagent ion transmission electrode (9), the reagent ion transmission hole (16) and the extraction electrode (14) from high to low, and an ion transmission electric field with the size of 1-50V/cm is formed in the axial direction.
4. The photochemical ionization source as claimed in claim 1, characterized in that:
the three cylindrical long electrodes (18) are all applied with radio frequency voltages with the same frequency and peak value, the peak value of the radio frequency voltage is 40-1000V, the radio frequency is 0.1-5 MHz, and the radio frequency phases are different by 120 degrees; the applied radio frequency voltage is superposed with a direct current voltage V5, and the voltage of V5 is between V3 and V4, so as to ensure the smooth extraction of ions.
5. The photochemical ionization source as claimed in claim 1, characterized in that:
the clean gas sample inlet pipe (3), the reagent gas sample inlet pipe (6) and the sample inlet pipe (11) are one or more metal capillary tubes, PEEK capillary tubes or quartz capillary tubes; the length is 0.05-5 m and the inner diameter is 25-500 μm.
6. The photochemical ionization source as claimed in claim 1, characterized in that:
the extraction electrode (14) is connected to a mass analyser (15) which may be a time of flight mass analyser, a quadrupole mass analyser or an ion trap mass analyser.
7. The photochemical ionization source as claimed in claim 1, characterized in that:
the ultraviolet light source (1) is a gas discharge lamp light source, a laser light source or a synchrotron radiation light source.
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| DE102009050040B4 (en) * | 2009-08-28 | 2014-10-30 | Bruker Daltonik Gmbh | Inlet of ions in mass spectrometer through Laval nozzles |
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