CN108987241B - Molecular light reaction testing device - Google Patents
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- CN108987241B CN108987241B CN201810950833.2A CN201810950833A CN108987241B CN 108987241 B CN108987241 B CN 108987241B CN 201810950833 A CN201810950833 A CN 201810950833A CN 108987241 B CN108987241 B CN 108987241B
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- 238000012360 testing method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 title description 4
- 238000005040 ion trap Methods 0.000 claims abstract description 118
- 239000007788 liquid Substances 0.000 claims abstract description 78
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 48
- 230000003287 optical effect Effects 0.000 claims abstract description 35
- 239000000919 ceramic Substances 0.000 claims abstract description 22
- 238000001196 time-of-flight mass spectrum Methods 0.000 claims abstract description 13
- 150000002500 ions Chemical class 0.000 claims description 37
- 239000007789 gas Substances 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 230000010355 oscillation Effects 0.000 claims description 12
- 239000001307 helium Substances 0.000 claims description 8
- 229910052734 helium Inorganic materials 0.000 claims description 8
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 230000005684 electric field Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 208000002925 dental caries Diseases 0.000 claims 1
- 239000012488 sample solution Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 230000003321 amplification Effects 0.000 description 3
- 238000010494 dissociation reaction Methods 0.000 description 3
- 230000005593 dissociations Effects 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 238000007493 shaping process Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- -1 charge position Chemical class 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001845 vibrational spectrum Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/004—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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Abstract
The invention relates to the field of spectrochemistry, in particular to a molecular photoreaction testing device, which comprises a liquid drop ejector, a vacuum cavity, an ionizer, a deflector I, a mass filter, a detector I, a deflector II, an ion beam shaper I, an ion trap I, an ion beam shaper II, an ion trap II, a time-of-flight mass spectrum, a lens, an optical shutter, an optical parametric oscillator, an oscilloscope and a vacuum pump set, wherein the ion trap II can be filled with buffer gas pulses, and the gas pressure in the ion trap II can be increased in a short time; the liquid drop ejector mainly comprises an ejector shell, a liquid storage tank, an electrode disc and a pulse generator, wherein the liquid storage tank is in an open barrel shape and is positioned in the ejector shell, the electrode disc is contacted with the bottom of the liquid storage tank, and the electrode disc is connected with the pulse generator through a cable; the electrode plate is composed of a group of electrode rings, each electrode ring is composed of a piezoelectric ceramic ring and two electrodes, the center of the electrode plate is symmetrically divided into eight areas, and the voltage of the electrodes applied to each area can be independently controlled.
Description
Technical Field
The invention relates to the field of spectrochemistry, in particular to a molecular photoreaction testing device for efficiently performing infrared light dissociation on ions by adopting optical parametric oscillation.
Background
Mass spectrometry is a common means for researching mass characteristics of different molecules in a material, and generally needs to enable a solution containing a sample to be detected to enter a vacuum environment after being atomized, and adopt devices such as a charge detector and the like to research ion beam current of the molecule to be detected in the vacuum environment. The mass spectrum is combined with the adjustable infrared laser, the vibration spectrum of the ions after the mass selection can be recorded through the infrared multiphoton dissociation spectrum depending on the wavelength, and the change of the charge-to-mass ratio of the ions is required to be detected in a test experiment. Optical parametric oscillation is a coherent light source with tunable wavelength, which can be tuned in a wide frequency range, and is generally used for obtaining chemical related information of ions, such as charge position, ion symmetry, and stretching of hydrogen bonds. Defect one of the prior art: the output of the optical parametric oscillation is difficult to realize a multiphoton absorption process, for the pulse optical parametric oscillation, a short pulse with nanosecond magnitude prevents the vibration redistribution process in a molecule, so that the number of photons which can be absorbed is limited, and for the continuous wave band optical parametric oscillation, the photon absorption rate is limited by relatively weak power, and due to the limitation, the infrared light dissociation efficiency of ions by adopting the optical parametric oscillation is lower; the defects of the prior art are as follows: in some experiments, only the components near the liquid level in the sample solution need to be analyzed, and a common spraying method can lead to the mixing of the samples with different structures in the solution, so that the subsequent experiments are interfered; defects three in the prior art: in some prior arts, the direction of the liquid drop of the sample solution is difficult to change by using the vibration of the piezoelectric ceramic material, and in some experiments, the position of the ejector needs to be continuously adjusted to achieve the purpose of changing the jet direction of the liquid drop, the operation is complex, and the defects of the prior art are four: the voltage driving circuit of the ion trap in the prior art is easily influenced by factors such as fluctuation of gain of an amplifier, temperature drift and the like, so that the vibration frequency of ions in the ion trap is fluctuated, the experimental precision is influenced, and the molecular light reaction testing device can solve the problem.
Disclosure of Invention
In order to solve the problems, the invention adopts the ion trap capable of rapidly filling and discharging buffer gas, can increase the air pressure in the ion trap in a very short time, cool ions, and can rapidly extract the ion trap, thereby increasing the efficiency of photoreaction; secondly, the droplet ejector can only form droplets of the solution near the liquid level and eject the droplets, and is suitable for analyzing the sample solution of the multilayer component; furthermore, the injection direction of the liquid drop injector is controllable, the injection direction can be changed for many times in the same experiment without an adjusting device, and finally, a special circuit is adopted to sample and rectify the high-voltage pulse voltage for driving the ion trap, so that the purpose of stabilizing the vibration frequency of ions in the ion trap can be realized.
The technical scheme adopted by the invention is as follows:
the molecular photoreaction testing device comprises a liquid drop ejector, a vacuum cavity, an ionizer, a deflector I, a mass filter, a detector I, a deflector II, an ion beam expander I, an ion trap I, an ion beam expander II, an ion trap II, a time-of-flight mass spectrum, a lens, an optical shutter, an optical parametric oscillator, an oscilloscope, an ion trap voltage driving circuit and a vacuum pump set, wherein the ion trap voltage driving circuit consists of a comparator, an integrating circuit, a radio frequency oscillator, a mixer, a rectifier, an amplifier, an antenna, a resonator and a capacitive voltage divider, and the vacuum cavity is formed by the liquid drop ejector, the vacuum cavity, the ionizer I, the deflector I, the mass filter, the detector I, the ion beam expander II, the ion trap II, the time-of-flight mass spectrum, the lens, the optical shutter, the optical parametric oscillator, the oscilloscope, the ion trap voltage driving circuit and the vacuum pump setVacuum degree 10 -7 Pa, the vacuum cavity is provided with a starting end and a tail end and is formed by vertically connecting two sections of cavities, an ionizer, a deflector I, a mass filter, a deflector II, an ion beam buncher I, an ion trap I, an ion beam buncher II, an ion trap II and a time-of-flight mass spectrum are sequentially arranged in the vacuum cavity from the starting end to the tail end, the deflector II is positioned at the vertical connection position of the vacuum cavity, light emitted by the optical parametric oscillator can sequentially pass through an optical shutter and a lens and then irradiate into the ion trap II, the optical parametric oscillator is connected with an oscilloscope cable, the droplet ejector is connected to one side of the starting end of the vacuum cavity, a small hole is formed in one side of the starting end of the vacuum cavity, droplets ejected by the droplet ejector can enter the vacuum cavity through the small hole and form an ion packet under the action of the ionizer, then an ion beam current is formed under the action of a vacuum pump set after the ion beam current passes through the mass filter and is deflected by the deflector II, and then sequentially passes through the ion beam buncher I, the ion beam buncher II and reaches the ion trap II, and the ion current is irradiated by the optical oscillator to the ion trap II; the ion trap II, the resonator, the capacitive voltage divider, the rectifier, the comparator, the integrating circuit, the mixer and the amplifier are sequentially connected, the amplifier is inductively coupled with the resonator through an antenna, the antenna can enable impedance matching between the ion trap voltage driving circuit and a circuit formed by the resonator and an electrode of the ion trap II, the mixer is provided with an I port, an LO port and an RF port, the I port, the LO port and the RF port are respectively used for inputting intermediate frequency signals, inputting local oscillation signals and outputting radio frequency signals, the integrating circuit is connected with an I port cable, the radio frequency oscillator is connected with an LO port cable, and the amplifier is connected with an RF port cable; the ion trap II can be filled with buffer gas pulses, the buffer gas is a mixture of nitrogen and helium, the mass ratio of the nitrogen to the helium is 1:9, the air pressure value in the ion trap II can be increased within two milliseconds, and the vacuum degree of the ion trap II is 10 -7 Pa reaches 10 - 3 Pa, the ion trap II is a linear radio frequency ion trap, and a two-dimensional radio frequency quadrupole electric field can be generated to limit ions entering the ion trap II byThe electrode of the ion trap II is connected with an ion trap voltage driving circuit; the detector I is positioned outside the vacuum cavity and is collinear with the ion beam expander I and the deflector II; the liquid drop ejector comprises an ejector shell, a liquid storage tank, an electrode disc and a pulse generator, wherein the liquid storage tank is of a barrel-shaped structure and is positioned in the ejector shell, the barrel-shaped structure is provided with an opening, the electrode disc is in contact with the bottom of the liquid storage tank, and the electrode disc is connected with the pulse generator through a cable; the electrode disk consists of a group of electrode rings, each electrode ring consists of a piezoelectric ceramic ring and two electrodes, the two electrodes are respectively attached to the upper surface and the lower surface of the piezoelectric ceramic ring, the electrode rings are arranged according to a Fresnel half-wave band, the size of each electrode ring depends on the vibration wavelength of vibration of the electrode disk in liquid and a preset focal length, and the size of the electrode ring meets the condition thatWhere n=1, 3,5, n is the order, λ l For the wavelength of the vibration wave in the liquid, F is the focal length, which is the distance from the focus of the vibration wave to the center of the ring electrode, r n Radius of the nth electrode ring; the electrode pad is divided equally into eight areas centrally, and the voltages applied to the electrodes in each area can be controlled individually. The radio frequency oscillator generates a radio frequency signal with the frequency of 20MHz and the power of-9 dBm, the radio frequency signal enters the mixer through the LO port, the radio frequency signal output by the RF port of the mixer enters the amplifier, the gain of the amplifier is 40dB, the radio frequency signal amplified by the amplifier is coupled into the resonator through the antenna, the signal output by the resonator is sampled by the capacitive voltage divider, the sampled signal enters the comparator after being subjected to direct current shaping in the rectifier, the sampled signal is compared with a preset stable voltage signal in the comparator, the voltage difference of the two signals is output to the integrating circuit by the comparator, and the voltage difference is input into the I port of the mixer after being subjected to integral amplification of the integrating circuit so as to regulate the amplitude of the radio frequency oscillation output by the RF port of the mixer.
Principle of droplet ejection: the electrode disk consists of a group of electrode rings, each electrode ring consists of a piezoelectric ceramic ring and two electrodes, and the electrodes are attachedThe electrode rings are arranged on the upper surface and the lower surface of the piezoelectric ceramic ring according to the Fresnel half-wave band, after voltage is applied to the electrodes, the piezoelectric ceramic ring can vibrate, vibration waves emitted by the piezoelectric ceramic ring propagate in liquid and interfere with each other, and as the shape of the annular electrode is the Fresnel half-wave band, the vibration waves interfere with each other and generate an enhanced vibration pressure vertical to the surface of the liquid at a focus, liquid drops are generated and are ejected out of the liquid surface in a direction vertical to the plane of the electrode disc, and parts, far away from the focus of the vibration waves, of the liquid are not ejected. Most of the vibration waves collide with the liquid surface, and the vibration energy dissipates and breaks the liquid surface, which in turn generates a free droplet, eventually causing the droplet to be ejected. The energy satisfies the following equilibrium equation:wherein E is oc Is applied vibration energy, E re Is the reflection energy, 4σ pi r 2 Is the energy of the surface tension and,the kinetic energy of the ejected droplet, r, σ, ρ, v are the radius of the droplet, the liquid level tension, the mass density and velocity of the ejected droplet, respectively. When a part of the electrode ring does not vibrate, the vibration pressure of the vibration wave at the focus of the liquid surface is unbalanced, so that the direction of liquid drop emission is not perpendicular to the liquid surface.
The reason that the electrode disc adopts a group of electrode rings instead of a whole piezoelectric ceramic disc is that the vibration of the area with the electrodes attached can be influenced by the area without the electrodes attached in the whole piezoelectric ceramic disc, so that a larger voltage is required to reach the preset frequency, and the vibration among different rings in the group of electrode rings is not interfered with each other, and larger voltage driving is not required.
The purpose of filling buffer gas pulse in the ion trap is as follows:
before the ions are trapped in the ion trap, the ion trap is filled with a cooled buffer gas, so that the ions are cooled through collision of buffer gas molecules and ions in the ion beam, and when the ions are trapped in the ion trap, the excessive buffer gas influences the photoreaction efficiency, so that the buffer gas needs to be rapidly extracted, and therefore, the buffer gas filling pulse is more suitable for the test than a method of continuously filling the buffer gas.
The step of testing by using the molecular light reaction testing device comprises the following steps:
firstly, injecting a sample solution to be detected into a liquid storage tank, wherein the flow rate value is 0.05-0.25 ml/min;
according to the type of the sample solution and the focus position, applying voltage to electrodes in different areas on the electrode plate to make the piezoelectric ceramic ring corresponding to the electrodes vibrate, wherein the vibration frequency value is 20-80 MHz;
thirdly, enabling the liquid drops ejected by the liquid drop ejector to enter a vacuum cavity and form an ion packet under the action of an ionizer, wherein the ion packet is deflected in a deflector I, then forms an ion beam current under the action of a vacuum pump set, and the ion beam current is deflected again by a deflector II after passing through a mass filter and then sequentially passes through an ion beam buncher I, an ion trap I and an ion beam buncher II to reach an ion trap II;
filling buffer gas pulse into the ion trap II, and increasing the air pressure in the ion trap II in a short time, wherein a typical value is two milliseconds of the buffer gas pulse time;
fifthly, after the buffer gas pulse is finished, after a delay time of 0.5 millisecond, the light emitted by the optical parametric oscillator irradiates ions in the ion trap II, and the ions react with light;
and sixthly, enabling the product of the ion photoreaction to enter a time-of-flight mass spectrum, and analyzing according to data obtained by the time-of-flight mass spectrum to obtain photoreaction related information.
The beneficial effects of the invention are as follows:
the invention adopts the ion trap capable of rapidly filling and discharging the buffer gas, can increase the air pressure in the ion trap in a very short time, cool the ions, and can be rapidly extracted when the laser is injected into the ion trap, thereby increasing the efficiency of photoreaction; secondly, the liquid drop ejector adopts a method of focusing vibration waves to form liquid drops only from the solution near the liquid level and eject the liquid drops, so that the liquid drop ejector is suitable for sample solutions with multiple layers of components; furthermore, the ejection direction of the droplet ejector is controllable, and the droplet ejection direction can be changed conveniently in the same experiment.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic illustration of the present invention;
FIG. 2 is an enlarged schematic view of a droplet ejector;
FIG. 3 is an enlarged schematic side view of an electrode disk;
FIG. 4 is an enlarged schematic top view of an electrode disk;
fig. 5 is a schematic diagram of an ion trap voltage drive circuit.
In the figure, 1 drop ejector, 1-1 ejector housing, 1-2 reservoir, 1-3 electrode disk, 1-3-1 electrode, 1-3-2 piezoceramic ring, 1-4 pulser, 2 vacuum chamber, 3 ionizer, 4 deflector I,5 mass filter, 6 detector I,7 deflector II,8 ion beam-forming device I,9 ion trap I,10 ion beam-forming device II,11 ion trap II,12 time-of-flight mass spectrum, 13 lens, 14 optical shutter, 15 optical parametric oscillator, 16 oscilloscope, 17 comparator, 18 integrating circuit, 19 radio frequency oscillator, 20 mixer, 21 rectifier, 22 amplifier, 23 antenna, 24 resonator, 25 capacitive divider.
Detailed Description
Referring to FIG. 1, an xyz is a three-dimensional space coordinate system, which comprises a droplet ejector (1), a vacuum chamber (2), an ionizer (3), a deflector I (4), a mass filter (5), a detector I (6), a deflector II (7), an ion beam expander I (8), an ion trap I (9), an ion beam expander II (10), an ion trap II (11), a time-of-flight mass spectrum (12), a lens (13), an optical shutter (14), an optical parametric oscillator (15) and an oscilloscope (16), wherein the vacuum chamber (2) is connected with a vacuum pump group, and the vacuum degree 10 of the vacuum chamber (2) -7 Pa, the vacuum cavity (2) is provided with a starting end and a tail end and is formed by vertically connecting two sections of cavities, an ionizer (3), a deflector I (4), a mass filter (5), a deflector II (7), an ion beam expander I (8), an ion trap I (9), an ion beam expander II (10), an ion trap II (11) and a time-of-flight mass spectrum (12) are sequentially arranged in the vacuum cavity (2) from the starting end to the tail end, and the deflector II (7) is positioned in the vacuum cavity (2) verticallyThe junction, light that optical parametric oscillator (15) sent can be in the ion trap II (11) through optical shutter (14) and lens (13) back shining in proper order, optical parametric oscillator (15) is connected with oscilloscope (16) cable, drop ejector (1) is connected in the starting end one side of vacuum chamber (2), and the starting end one side of vacuum chamber (2) has the aperture, and the drop that drop ejector (1) jetted can get into vacuum chamber (2) through the aperture and under the effect of ionizer (3) forms the ion packet, after the ion packet deflects in deflector I (4), then forms the ion beam under the effect of vacuum pump group, after the ion beam passes through mass filter (5), is deflected by deflector II (7) again, then loops through ion beam expander I (8), ion trap I (9), ion beam expander II (10) reach ion trap II (11), ion beam is at ion trap II
(11) The ion trap II (11) can be filled with buffer gas pulse, the buffer gas is a mixture of nitrogen and helium, the mass ratio of the nitrogen to the helium is 1:9, the air pressure value in the ion trap II (11) can be increased within two milliseconds, and the vacuum degree of the ion trap II (11) is 10 -7 Pa reaches 10 -3 Pa, the ion trap II (11) is a linear radio frequency ion trap, and a two-dimensional radio frequency quadrupole electric field can be generated to limit ions entering the ion trap II (11), and the ion trap II (11) is connected with an ion trap voltage driving circuit through electrodes; the detector I (6) is positioned in the vacuum cavity
(2) In addition, the ion beam expander I (8) and the deflector II (7) are collinear.
As shown in fig. 2, which is an enlarged schematic view of a droplet ejector, the droplet ejector (1) includes an ejector housing (1-1), a liquid reservoir (1-2), an electrode plate (1-3), and a pulse generator (1-4), the liquid reservoir (1-2) is in a barrel-like structure having an opening, the electrode plate (1-3) is in contact with the bottom of the liquid reservoir (1-2), and the electrode plate (1-3) is connected to the pulse generator (1-4) by a cable.
FIG. 3 is an enlarged schematic side view of the electrode plate, FIG. 4 is an enlarged schematic top view of the electrode plate, the electrode plate (1-3) is composed of a set of electrode rings each composed of a piezoelectric ceramic ring (1-3-2) and two electrodes (1-3-1), the two electrodes (1-3-1) being respectively attached to the upper and lower surfaces of the piezoelectric ceramic rings (1-3-2), the electrode rings being arranged in accordance with a fresnel half-wave band, the size of each electrode ring depending on the vibration wavelength of vibration of the electrode plate (1-3) in the liquid and a preset focal length, the electrode ring size satisfying the condition thatWhere n=1, 3,5, n is the order, λ l For the wavelength of the vibration wave in the liquid, F is the focal length, which is the distance from the focus of the vibration wave to the center of the ring electrode, r n Radius of the nth electrode ring; the electrode plate (1-3) is divided equally into eight areas in central symmetry, and the voltage applied to the electrode (1-3-1) in each area can be controlled individually.
Fig. 5 is a schematic diagram of an ion trap voltage driving circuit, which comprises a comparator (17), an integrating circuit (18), a radio frequency oscillator (19), a mixer (20), a rectifier (21), an amplifier (22), an antenna (23), a resonator (24) and a capacitive voltage divider (25), wherein an electrode of an ion trap II (11), the resonator (24), the capacitive voltage divider (25), the rectifier (21), the comparator (17), the integrating circuit (18), the mixer (20) and the amplifier (22) are sequentially connected, the amplifier (22) and the resonator (24) are inductively coupled through the antenna (23), the antenna (23) can enable impedance matching between the ion trap voltage driving circuit and a circuit formed by the electrodes of the resonator (24) and the ion trap II (11), the mixer (20) is provided with an I port, an LO port and an RF port, the I port, the LO port and the RF port are respectively used for signal input, local oscillator signal input and radio frequency signal output, the integrating circuit (18) and the I port are connected through an antenna cable, the radio frequency oscillator (19) is connected with the LO port cable, and the amplifier (22) is connected with the RF port.
The radio frequency oscillator (19) generates a radio frequency signal with the frequency of 20MHz and the power of-9 dBm, the radio frequency signal enters the mixer (20) through the LO port, the radio frequency signal output by the RF port of the mixer (20) enters the amplifier (22), the gain of the amplifier (22) is 40dB, the amplified radio frequency signal output by the amplifier (22) is coupled into the resonator (24) through the antenna (23), the capacitor divider (25) samples 1% of the signal output by the resonator (24), the sampled signal enters the comparator (17) after being subjected to direct current shaping in the rectifier (21), and is compared with a preset stable voltage signal in the comparator (17), the voltage difference of the two signals is output to the integrating circuit (18) by the comparator (17), and the voltage difference is input into the I port of the mixer after being subjected to integral amplification of the integrating circuit (18) so as to adjust the amplitude of the radio frequency oscillation output by the RF port of the mixer (20).
Principle of droplet ejection: the electrode disc (1-3) consists of a group of electrode rings, each electrode ring consists of a piezoelectric ceramic ring (1-3-2) and two electrodes (1-3-1), the electrodes (1-3-1) are attached to the upper surface and the lower surface of the piezoelectric ceramic ring (1-3-2), the electrode rings are arranged according to a Fresnel half-wave band, after voltage is applied to the electrodes (1-3-1), the piezoelectric ceramic rings (1-3-2) vibrate, vibration waves emitted by the piezoelectric ceramic rings propagate in liquid and interfere with each other, and because the shape of the annular electrodes is the Fresnel half-wave band, the vibration waves interfere and generate an enhanced vibration pressure perpendicular to the surface of the liquid at a focus, liquid drops are generated and are ejected in the direction perpendicular to the plane where the electrode disc (1-3) is located, and the part of the liquid away from the focus of the vibration waves cannot be ejected. Most of the vibration waves collide with the liquid surface, and the vibration energy dissipates and breaks the liquid surface, which in turn generates a free droplet, eventually causing the droplet to be ejected. The energy satisfies the following equilibrium equation:wherein E is oc Is applied vibration energy, E re Is the reflection energy, 4σ pi r 2 Is surface tension energy, < >>The kinetic energy of the ejected droplet, r, σ, ρ, v are the radius of the droplet, the liquid level tension, the mass density and velocity of the ejected droplet, respectively. When a part of the electrode ring does not vibrate, the vibration pressure of the vibration wave at the focus of the liquid surface is unbalanced, so that the direction of liquid drop emission is not perpendicular to the liquid surface.
The reason why the electrode plates (1-3) adopt a group of electrode rings instead of a whole piezoelectric ceramic plate is that since the vibration of the region where the electrodes are attached is affected by the region where the electrodes are not attached in a whole piezoelectric ceramic plate, a larger voltage is required to reach the preset frequency, and the vibration between different rings in a group of electrode rings does not interfere with each other, and a larger voltage driving is not required.
The purpose of filling buffer gas pulse in the ion trap is as follows:
before the ions are trapped in the ion trap, the ion trap is filled with a cooled buffer gas, so that the ions are cooled through collision of buffer gas molecules and ions in the ion beam, and when the ions are trapped in the ion trap, the excessive buffer gas influences the photoreaction efficiency, so that the buffer gas needs to be rapidly extracted, and therefore, the buffer gas filling pulse is more suitable for the test than a method of continuously filling the buffer gas.
The molecular photoreaction testing device comprises a liquid drop ejector (1), a vacuum cavity (2), an ionizer (3), a deflector I (4), a mass filter (5), a detector I (6), a deflector II (7), an ion beam expander I (8), an ion trap I (9), an ion beam expander II (10), an ion trap II (11), a time-of-flight mass spectrum (12), a lens (13), an optical shutter (14), an optical parametric oscillator (15), an oscilloscope (16), an ion trap voltage driving circuit and a vacuum pump set, wherein the ion trap voltage driving circuit consists of a comparator (17), an integrating circuit (18), a radio frequency oscillator (19), a mixer (20), a rectifier (21), an amplifier (22), an antenna (23), a resonator (24) and a capacitive voltage divider (25), xyz is a three-dimensional space coordinate system, the vacuum cavity (2) is connected with the vacuum pump set, and the vacuum degree (10) of the vacuum cavity (2) -7 Pa, the vacuum cavity (2) is provided with a starting end and a tail end and is formed by vertically connecting two sections of cavities, in the vacuum cavity (2), an ionizer (3), a deflector I (4), a mass filter (5), a deflector II (7), an ion beam expander I (8), an ion trap I (9), an ion beam expander II (10), an ion trap II (11) and a time-of-flight mass spectrum (12) are sequentially arranged from the starting end to the tail end, the deflector II (7) is positioned at the vertical connection position of the vacuum cavity (2), light emitted by the optical parametric oscillator (15) can sequentially pass through an optical shutter (14) and a lens (13) and then irradiate the ion trap II (11), and the optical parametric oscillator (15) and an oscilloscope (16)The liquid drop ejector (1) is connected to one side of the starting end of the vacuum cavity (2), a small hole is formed in one side of the starting end of the vacuum cavity (2), liquid drops ejected by the liquid drop ejector (1) can enter the vacuum cavity (2) through the small hole and form an ion packet under the action of the ionizer (3), the ion packet is deflected in the deflector I (4) and then forms an ion beam under the action of the vacuum pump set, the ion beam is deflected again by the deflector II (7) after passing through the mass filter (5), then sequentially passes through the ion beam buncher I (8), the ion trap I (9) and the ion beam buncher II (10) to reach the ion trap II (11), the ion beam is irradiated by light emitted by the optical parameter oscillator (15) in the ion trap II (11), and the ion trap II (11) is provided with an electrode; the ion trap II (11), the resonator (24), the capacitive voltage divider (25), the rectifier (21), the comparator (17), the integrating circuit (18), the mixer (20) and the amplifier (22) are sequentially connected, the amplifier (22) is inductively coupled with the resonator (24) through the antenna (23), the antenna (23) can enable impedance matching between an ion trap voltage driving circuit and a circuit formed by the resonator (24) and electrodes of the ion trap II (11), the mixer (20) is provided with an I port, an LO port and an RF port, the I port, the LO port and the RF port are respectively used for intermediate frequency signal input, local oscillation signal input and radio frequency signal output, the integrating circuit (18) is connected with an I port cable, the radio frequency oscillator (19) is connected with an LO port cable, and the amplifier (22) is connected with an RF port cable; the ion trap II (11) can be filled with buffer gas pulses, the buffer gas is a mixture of nitrogen and helium, the mass ratio of the nitrogen to the helium is 1:9, the air pressure value in the ion trap II (11) can be increased within two milliseconds, and the vacuum degree of the ion trap II (11) is 10 -7 Pa reaches 10 -3 Pa, the ion trap II (11) is a linear radio frequency ion trap, and a two-dimensional radio frequency quadrupole electric field can be generated to limit ions entering the ion trap II (11), and the ion trap II (11) is connected with an ion trap voltage driving circuit through electrodes; the liquid drop ejector (1) comprises an ejector shell (1-1), a liquid storage tank (1-2), an electrode disc (1-3) and a pulse generator (1-4), wherein the liquid storage tank (1-2) is of a barrel-shaped structure and is positioned in the ejector shell (1-1), the barrel-shaped structure is provided with an opening, the electrode disc (1-3) is contacted with the bottom of the liquid storage tank (1-2), and the electrode disc (1-3) is connected with the pulse generator through a cable1-4); the electrode disk (1-3) is composed of a group of electrode rings, each electrode ring is composed of a piezoelectric ceramic ring (1-3-2) and two electrodes (1-3-1), the two electrodes (1-3-1) are respectively attached to the upper surface and the lower surface of the piezoelectric ceramic ring (1-3-2), the electrode rings are arranged according to a Fresnel half-wave band, the size of each electrode ring depends on the vibration wavelength of vibration of the electrode disk (1-3) in liquid and a preset focal length, and the size of the electrode ring meets the condition thatWhere n=1, 3,5, n is the order, λ l For the wavelength of the vibration wave in the liquid, F is the focal length, which is the distance from the focus of the vibration wave to the center of the ring electrode, r n Radius of the nth electrode ring; the electrode disk (1-3) is divided into eight areas symmetrically at the center, and the voltage of the electrode (1-3-1) applied to each area can be controlled individually; the radio frequency oscillator (19) generates a radio frequency signal with the frequency of 20MHz and the power of-9 dBm, the radio frequency signal enters the mixer (20) through the LO port, the radio frequency signal output by the RF port of the mixer (20) enters the amplifier (22), the gain of the amplifier (22) is 40dB, the amplified radio frequency signal output by the amplifier (22) is coupled into the resonator (24) through the antenna (23), the capacitor divider (25) samples 1% of the signal output by the resonator (24), the sampled signal enters the comparator (17) after being subjected to direct current shaping in the rectifier (21), and is compared with a preset stable voltage signal in the comparator (17), the voltage difference of the two signals is output to the integrating circuit (18) by the comparator (17), and the voltage difference is input into the I port of the mixer after being subjected to integral amplification of the integrating circuit (18) so as to adjust the amplitude of the radio frequency oscillation output by the RF port of the mixer (20).
The ion trap adopted by the invention can rapidly charge and discharge buffer gas, can increase the air pressure in the ion trap in a very short time to cool ions, and can rapidly discharge the buffer gas out of the ion trap so that the photoreaction efficiency is not affected; secondly, the liquid drop ejector can only form liquid drops from the solution near the liquid level and eject the liquid drops, and the liquid at other parts of the liquid storage tank is not affected, so that different components are not easy to mix up when the sample solution with multiple layers of components is analyzed; furthermore, the ejection direction of the droplet ejectors is controllable, and the droplet ejection direction can be easily changed without adjusting the device.
Claims (1)
1. A molecular photoreaction testing device comprises a liquid drop ejector (1), a vacuum cavity (2), an ionizer (3), a deflector I (4), a mass filter (5), a detector I (6), a deflector II (7), an ion beam expander I (8), an ion trap I (9), an ion beam expander II (10), an ion trap II (11), a time-of-flight mass spectrum (12), a lens (13), an optical shutter (14), an optical parametric oscillator (15), an oscilloscope (16), an ion trap voltage driving circuit and a vacuum pump set, wherein the ion trap voltage driving circuit consists of a comparator (17), an integrating circuit (18), a radio frequency oscillator (19), a mixer (20), a rectifier (21), an amplifier (22), an antenna (23), a resonator (24) and a capacitive voltage divider (25), xyz is a three-dimensional space coordinate system, the vacuum cavity (2) is connected with the vacuum pump set, and the vacuum degree (10) of the vacuum cavity (2) -7 Pa, vacuum chamber (2) have beginning and end and by two sections of cavitys perpendicular connection form, in vacuum chamber (2) have ionization ware (3) from beginning to end in proper order, deflector I (4), mass filter (5), deflector II (7), ion beam expander I (8), ion trap I (9), ion beam expander II (10), ion trap II (11) and time of flight mass spectrum (12), deflector II (7) are located vacuum chamber (2) vertical junction, light that optical parametric oscillator (15) sent can pass through optical shutter (14) and lens (13) in proper order and shine in ion trap II (11) behind, optical parametric oscillator (15) and oscilloscope (16) cable junction, liquid drop ejector (1) are connected in vacuum chamber (2)'s beginning one side, liquid drop that liquid drop ejector (1) jetted can get into vacuum chamber (2) through aperture and form ion packet under the effect of ionization ware (3), deflection ware I is in vacuum chamber (4) after passing through deflection filter I, deflection ware (8) are formed behind ion beam expander I, ion beam expander I is formed in proper order, ion beam expander I is deflected in proper order behind ion beam expander I (8), the ion beam expander II (10) reaches the ion trap II (11), and the ion beam current is optically referenced in the ion trap II (11)The ion trap II (11) has electrodes, which are irradiated with light from the volume oscillator (15),
the method is characterized in that: the ion trap II (11), the resonator (24), the capacitive voltage divider (25), the rectifier (21), the comparator (17), the integrating circuit (18), the mixer (20) and the amplifier (22) are sequentially connected, the amplifier (22) is inductively coupled with the resonator (24) through the antenna (23), the antenna (23) can enable impedance matching between an ion trap voltage driving circuit and a circuit formed by the resonator (24) and electrodes of the ion trap II (11), the mixer (20) is provided with an I port, an LO port and an RF port, the I port, the LO port and the RF port are respectively used for intermediate frequency signal input, local oscillation signal input and radio frequency signal output, the integrating circuit (18) is connected with an I port cable, the radio frequency oscillator (19) is connected with an LO port cable, and the amplifier (22) is connected with an RF port cable; the ion trap II (11) can be filled with buffer gas pulses, the buffer gas is a mixture of nitrogen and helium, the mass ratio of the nitrogen to the helium is 1:9, the air pressure value in the ion trap II (11) can be increased within two milliseconds, and the vacuum degree of the ion trap II (11) is 10 -7 Pa reaches 10 -3 Pa, the ion trap II (11) is a linear radio frequency ion trap, and a two-dimensional radio frequency quadrupole electric field can be generated to limit ions entering the ion trap II (11), and the ion trap II (11) is connected with an ion trap voltage driving circuit through electrodes; the liquid drop ejector (1) comprises an ejector shell (1-1), a liquid storage tank (1-2), an electrode disc (1-3) and a pulse generator (1-4), wherein the liquid storage tank (1-2) is of a barrel-shaped structure and is positioned in the ejector shell (1-1), the barrel-shaped structure is provided with an opening, the electrode disc (1-3) is in contact with the bottom of the liquid storage tank (1-2), and the electrode disc (1-3) is connected with the pulse generator (1-4) through a cable; the electrode disk (1-3) is composed of a group of electrode rings, each electrode ring is composed of a piezoelectric ceramic ring (1-3-2) and two electrodes (1-3-1), the two electrodes (1-3-1) are respectively attached to the upper surface and the lower surface of the piezoelectric ceramic ring (1-3-2), the electrode rings are arranged according to a Fresnel half-wave band, the size of each electrode ring depends on the vibration wavelength of vibration of the electrode disk (1-3) in liquid and a preset focal length, and the size of the electrode ring meets the condition thatWhere n=1, 3,5, n is the order, λ l For the wavelength of the vibration wave in the liquid, F is the focal length, which is the distance from the focus of the vibration wave to the center of the ring electrode, r n Radius of the nth electrode ring; the electrode plate (1-3) is divided equally into eight areas in central symmetry, and the voltage applied to the electrode (1-3-1) in each area can be controlled individually.
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