CN108760637B - Device for researching molecular photoisomerization - Google Patents
Device for researching molecular photoisomerization Download PDFInfo
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- CN108760637B CN108760637B CN201810832101.3A CN201810832101A CN108760637B CN 108760637 B CN108760637 B CN 108760637B CN 201810832101 A CN201810832101 A CN 201810832101A CN 108760637 B CN108760637 B CN 108760637B
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- 238000007699 photoisomerization reaction Methods 0.000 title claims abstract description 20
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 100
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 150000002500 ions Chemical class 0.000 claims description 131
- 239000007789 gas Substances 0.000 claims description 75
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 230000005684 electric field Effects 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 230000005284 excitation Effects 0.000 description 12
- 238000005452 bending Methods 0.000 description 9
- 150000001793 charged compounds Chemical group 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 5
- 239000007921 spray Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000005283 ground state Effects 0.000 description 3
- 238000001871 ion mobility spectroscopy Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000006303 photolysis reaction Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005281 excited state Effects 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000001720 action spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000012306 spectroscopic technique Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- 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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
Abstract
The invention relates to the field of spectrochemistry, in particular to a device for researching molecular photoisomerization, which comprises an electrospray device, an ion beam condenser, an ion gate, a laser, a deflection electrode group, a linear electrode group, an octupole ion guide, a quadrupole mass filter, a detector, a vacuum cavity, a drift cavity, a gas inlet and a gas outlet, wherein the deflection electrode group is provided with nineteen annular electrodes, the included angle between the adjacent annular electrodes is five degrees, the linear electrode group is provided with twenty annular electrodes, the annular electrode of the deflection electrode group II is provided with a through hole, and laser emitted by the laser III can enter the drift region along the negative z direction through the through hole; the laser beam emitted by the laser I can enter the drift region through the deflection electrode group I, and the laser beam emitted by the laser II can enter the drift region through the linear electrode group II; the electrospray device consists of an outer tube, an inner tube, a baffle, an air inlet and a liquid inlet, wherein the outer tube and the inner tube are cylindrical and are in coaxial nested configuration, and a liquid channel is arranged between the outer tube and the inner tube.
Description
Technical Field
The invention relates to the field of spectrochemistry, in particular to a device for researching molecular photoisomerization with multiple light excitation modes.
Background
Photoisomerization refers to the structural change of a molecule between the isomerism under light excitation, and the influence of photoisomerization on the chemical shift of each group or even each atom in the molecule can be determined by analyzing certain spectral lines, and is usually studied by mass spectrometry or ion mobility spectrometry, in which a sample molecule is usually injected into a drift region in the form of ions, and is moved by an electric field generated by an electrode to perform subsequent measurement. Defect one of the prior art: the prior art cannot realize that laser is overlapped with ion beams from the transverse direction and the longitudinal direction to interact in the same device; the defects of the prior art are as follows: the electrospray method is generally adopted to inject sample molecules into the drift region, the mass flow output of electrospray in the prior art is low, and the device for researching the photoisomerization of the molecules can solve the problem.
Disclosure of Invention
In order to solve the problems, the device for researching the molecular photoisomerization can select the isomer before a mass spectrum stage and identify the isomer in the product, and has various light excitation modes; can be used for researching photodecomposition of molecular ions and can identify charged products thereof from both migration rate and mass; the spray head is provided with the annular liquid channel, and the liquid is applied with high voltage in a thin layer shape, so that relatively uniform atomized liquid drops can be sprayed, and the quality of ion packets entering a drift region is improved.
The technical scheme adopted by the invention is as follows:
the device for researching molecular photoisomerization comprises an electrospray device, an ion beam expander I, an ion gate I, a laser I, a deflection electrode group I, a linear electrode group I, an ion gate II, a laser II, a linear electrode group II, a deflection electrode group II, an ion beam expander II, a laser III, an octapole ion guide, a quadrupole mass filter, a detector, a vacuum chamber, a drift cavity, a gas inlet and a gas outlet, xyz is a three-dimensional coordinate system, the ion beam expander I, the ion gate I, the deflection electrode group I, the linear electrode group I, the ion gate II, the linear electrode group II, the deflection electrode group II and the ion beam expander II are sequentially connected, the ion beam expander I, the ion gate I, the deflection electrode group I, the linear electrode group I, the ion gate II, the linear electrode group II, the deflection electrode group II and the ion beam expander II are all positioned in the drift cavity, the device comprises a deflection electrode group I, a linear electrode group II and a deflection electrode group II, wherein the deflection electrode group I, the linear electrode group II and the deflection electrode group II are all composed of annular electrodes with the inner diameter of forty millimeters, a space formed by the centers of the annular electrodes of the deflection electrode group I, the linear electrode group II and the deflection electrode group II is a drift region, a drift cavity is provided with a starting end and a tail end, the starting end and the tail end are provided with small holes for passing ion beam, a gas inlet is arranged on the side wall of the tail end of the drift cavity, a gas outlet is arranged on the side wall of the starting end of the drift cavity, the gas inlet is sequentially connected with a mass flow controller and a gas storage tank, buffer gas is filled in the gas storage tank, the buffer gas is nitrogen or helium, and the mass flow controller can control the drift cavityThe buffer gas is discharged from a gas outlet into a drift cavity, the buffer gas flow value is 0.3SLM, the SLM is standard gas per liter/min, the buffer gas can form a gas countercurrent which passes through an ion beam expander I, neutral molecules can be prevented from entering the drift region, solvent molecules in electrospray solution can be prevented from entering the drift region, the drift cavity is provided with a release valve, the air pressure in the drift region can be controlled by adjusting the buffer gas flow and the frequency of opening and closing the release valve, the air pressure value is 1000 Pa, the electrospray device is positioned at the outer side of the initial end of the drift cavity, the vacuum cavity is positioned at the outer side of the tail end of the drift cavity, the octupole ion guide, the quadrupole mass filter and the detector are sequentially and linearly arranged in the vacuum cavity, the initial end of the vacuum cavity is provided with a small hole for passing through the ion beam, the vacuum pump is connected with a vacuum pump, and the vacuum degree is superior to 10 -5 When the electrospray device generates ions of molecules to be detected, the ions sequentially pass through the ion beam expander I, the ion gate I, the deflection electrode group I, the linear electrode group I, the ion gate II, the linear electrode group II, the deflection electrode group II, the ion beam expander II, the octupole ion guide and the quadrupole mass filter to reach the detector, so that an ion beam path is formed. In the deflection electrode group I, the centers of the ten annular electrodes through which the ion beam passes are positioned in the yz plane and positioned on the 1/8 circumference with the radius of fifty millimeters, and are arranged at equal intervals in the clockwise direction, the centers of the nine annular electrodes through which the ion beam passes next are positioned in the yz plane and positioned on the 1/8 circumference with the radius of fifty millimeters, and are arranged at equal intervals in the counterclockwise direction, the centers of the ten annular electrodes through which the ion beam passes first are positioned in the yz plane and positioned on the 1/8 circumference with the radius of fifty millimeters, and are arranged at equal intervals in the clockwise direction, and the centers of the nine annular electrodes through which the ion beam passes next are positioned in the yz plane and positioned on the 1/8 circumference with the radius of fifty millimeters, and are arranged at equal intervals in the counterclockwise direction, respectivelyThe needles are arranged at equal intervals in the direction; a megaohm resistor is connected in series between adjacent annular electrodes in the deflection electrode group I and the deflection electrode group II to divide the voltage, and the deflection electrode group I and the deflection electrode group II respectively provide voltages through two high-voltage power supplies; the linear electrode group I and the linear electrode group II are respectively provided with twenty annular electrodes, the annular electrodes are perpendicular to the yz plane, the annular electrodes of the deflection electrode group II are provided with through holes, and laser emitted by the laser III can enter the drift region along the negative z direction through the through holes; the laser beam emitted by the laser I can enter the drift region through the deflection electrode group I, and the laser beam emitted by the laser II can enter the drift region through the linear electrode group II; the ion beam-buncher I consists of fifty metal ring electrodes with the thickness of one millimeter, and comprises ten ring electrodes with the inner diameter of forty millimeters and forty ring electrodes with the inner diameter linearly reduced from forty millimeters to two millimeters along the positive direction z, wherein adjacent metal ring electrodes are separated by insulating sheets with the thickness of one millimeter; the ion beam buncher II connected with the tail end of the drift region consists of forty annular electrodes with the inner diameter of forty millimeters in the positive z direction being linearly reduced to two millimeters; the electric spraying device is composed of an outer tube, an inner tube, a baffle, an air inlet and a liquid inlet, wherein the baffle can seal one side port of the inner tube, the outer tube and the inner tube are cylindrical, the inner diameter of the outer tube is 3000 microns, the outer diameter of the inner tube is 2700 microns, the outer tube and the inner tube are in coaxial nested configuration, a liquid channel is arranged between the outer tube and the inner tube, the air inlet and the liquid inlet are respectively connected with the outer wall of the outer tube and are communicated with the liquid channel, the inner wall of the outer tube is provided with dispersed grooves along the axial direction of the outer tube, and the grooves can enable liquid to locally form protruding shapes to increase a local electric field. The number of grooves on the inner wall of the outer tube is four to twelve, and the cross section of each groove is semicircular, square or triangular.
During the test, ions generated by electrospray accumulate in the ion beam condenser I, and the ion gate I is periodically opened to enable the ion beam to be injected to the front section of the drift region where the deflection electrode group I is positioned, and the ions are acted by a drift electric field to move towards the tail end of the drift cavity and collide with nitrogen or helium filled in the drift region; the ions are collected by the ion beam condenser II after leaving the drift region, and then sequentially pass through the small hole at the tail end of the drift cavity, the small hole at the starting end of the vacuum cavity, the octupole ion guide and the quadrupole mass filter, and finally enter the detector. The ions can be irradiated laterally by the laser when they pass through the ion beam expander I or through the drift region after the ion beam expander II, and can be irradiated axially by the laser when they are in the middle of the drift region, i.e. in different excitation modes.
The principle of the invention is that the device is mainly based on an ion mobility spectrometry method, and the drift region is provided with a bending section, so that a laser beam and drifting ions are overlapped and interacted in the axial direction or the transverse direction to change the isomerism form of the ions, and the drift speed of the ions is changed.
Principle of operation of ion mobility spectrometry: the ion packets formed by electrospray or photoexcitation move in the drift region under the action of the electric field and collide with the buffer gas in the drift region, and the molecular isomer which is compact in configuration moves at a higher speed, so that the molecular isomer which is large in configuration can be spatially and temporally distinguished from the molecular isomer which is large in configuration. In addition, the drift region in the invention has two special bending sections, and the bending sections are composed of a series of annular electrodes and have special arrangement structures, so that the effect of re-converging ions in the drift region can be achieved, and the principle is as follows: in the first bending section, the distance between the ring electrodes on the lower side of the bending section is short, so the electric field intensity is large and the movement path of the ions is short, so the ions near the lower side of the bending section in one ion packet are shorter than the drift distance of the ions near the upper side, so the ions move to the front, while in the second bending section, the distance between the ring electrodes on the lower side of the bending section is long, so the electric field intensity is small and the movement path of the ions is long, so the ions near the lower side of the bending section are longer than the drift distance of the ions near the upper side, so the ions near the upper side and the lower side in the ion packet are recombined. The design has the advantages that the rear end of the ion beam splitter does not need to adopt an ion beam splitter with larger deflection to the direction of deflected ion beams, so that the ion loss in the process of passing through the ion beam splitter is avoided, and the resolution of acquired spectrums is avoided. The invention can measure the photoisomerization spectrum of the isomer with mobility selected, the device detects the change of the ion drift velocity, and the photoisomerization spectrum is obtained by measuring the relation between the signal of the photoisomerization and the laser wavelength used for light excitation. By measuring the yield of the photoisomers as a function of the laser wavelength, a spectrum of action can be obtained which reflects the molecular absorption spectrum and the isomerisation yield phi (lambda) which depends on the wavelength of the light lambda, if this yield phi (lambda) is independent of the wavelength of the light, the photoisomerization spectrum is similar to the optical absorption spectrum, which compensates for the deficiencies of the existing spectroscopic techniques for detecting molecular ions.
The method for researching by using the device for researching the molecular photoisomerization comprises the following steps:
introducing high-purity nitrogen from an air inlet of an electrospray device, wherein the typical flow rate is 1.0SLM (selective vapor deposition) which is standard gas per liter/min, and simultaneously introducing a solution containing molecules to be tested from a liquid inlet of the electrospray device, and the typical flow rate is 2.0 milliliters/min;
applying voltage between an outer tube and an inner tube of the electrospray device, wherein the voltage ranges from 1000V to 5000V, so that part of molecules to be detected in the solution are in an ionic form, atomized liquid drops are formed at an outlet of the electrospray device, the shape of liquid spray can be adjusted by adjusting the voltage, and part of liquid drops enter the drift cavity through a small hole at the starting end of the drift cavity;
when ions entering the drift cavity pass through the ion beam shaper I, only direct current potential is applied to the first annular electrode and the last annular electrode of the ion beam shaper I, direct current potential and alternating current potential are applied to other annular electrodes, the range of the direct current potential is 150V to 300V, the range of the alternating current potential is 30V to 50V, the phases of the alternating current potentials applied to adjacent annular electrodes are opposite, the driving frequency of the alternating current potential is 300kHz, and the direct current potential applied to each annular electrode through a voltage divider is reduced along the positive z direction, so that the ion beams reach the converging effect;
the movement direction of the ion beam in the drift region where the deflection electrode group I is located deviates from the z direction and returns to the z direction, then sequentially passes through the linear electrode group I, the ion gate II and the linear electrode group II, and then deviates from the z direction and returns to the z direction in the drift region where the deflection electrode group II is located;
fifth, the laser irradiates the ion packet in the drift region to excite it, the cross section of the laser beam is larger than 5mm×5mm so that the whole ion packet is irradiated, and three optical excitation modes can be selected:
mode one: the ion is irradiated by the laser pulse emitted by the laser I at the position 30 mm after passing through the ion gate I, and the parent ion, the photoisomer generated by light excitation and the photoinduced fragment ion can be separated in time and space after passing through the drift region, so that the whole ion packet can be irradiated by relatively strong laser before being diffused;
mode two: after the ion packets have been selected for their mobility in the drift region by the ion gate II, they are irradiated by the laser light emitted by the laser II. After the ion gate I is opened and a certain ion packet is transmitted, the ion gate II is opened for 100 microseconds, and the laser pulse emitted by the laser II is overlapped with the selected ions at the position 15mm behind the ion gate II;
mode three: the laser emitted by the laser III irradiates ions along the z direction through the through hole on the annular electrode of the deflection electrode group II, and has the advantages of being applicable to molecular ions excited from a ground state to an excited state and quickly relaxed to the ground state, and under the condition, the laser excitation can be used for establishing optical driving balance between the ground state and the excited state;
the ion beam enters an ion beam condenser II, only DC potential is applied to the first annular electrode and the last annular electrode of the ion beam condenser II, DC and AC potentials are applied to other annular electrodes, the DC potential ranges from 150V to 300V, the AC potential ranges from 30V to 50V, phases of the AC potentials applied to adjacent annular electrodes are opposite, the driving frequency is 500kHz, and the DC potential applied to each annular electrode through a voltage divider linearly decreases, so that the ion beam is further converged;
seventhly, the ion beam sequentially enters the vacuum cavity through a small hole at the tail end of the drift cavity and a small hole at the starting end of the vacuum cavity, and the cross section of the ion beam in the xz plane is reduced after the ion beam passes through the octupole ion guide;
the ion beam passes through a quadrupole mass filter, and the mass selection of the ions can be carried out according to the charge-to-mass ratio difference of the ions by adjusting the voltage value on the quadrupole rods of the quadrupole mass filter and the voltage range from 50V to 200V;
ninth, the ions with the mass selection enter a detector to obtain corresponding signals;
analyzing the data to obtain the intensity and delay time of the ion signals detected by the detector under different laser conditions, obtaining the distribution of the time of each isomer ion packet reaching the detector, obtaining the relation between the time of each isomer ion packet reaching the detector and the charge-to-mass ratio of each isomer ion packet, obtaining the relation between the time of each isomer ion packet reaching the detector and the laser wavelength adopted by light excitation, judging the type of the generated ions and the relation between the generated ions and different laser wavelengths, and obtaining the photoisomerization action spectrum;
eleven, the data were further analyzed to determine the relationship of measured ion mobility to molecular structure.
The beneficial effects of the invention are as follows:
the method is used for researching photoisomerization of molecular ions in gas phase, and has the advantages of being capable of selecting isomers before a mass spectrum stage and identifying the isomers in the product, and having various light excitation modes; the invention can also be used for researching photodecomposition of molecular ions, and can identify charged products thereof from the aspects of migration rate and mass simultaneously; in addition, the spray head is provided with the annular liquid channel, and the liquid is applied with high voltage in a thin layer shape, so that relatively uniform atomized liquid drops can be sprayed, and the quality of an ion packet entering a drift region is improved.
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 a top view of the electrospray device;
fig. 3 is a side view of an electrospray device.
In the drawings, 1. Electrospray device, 1-1. Outer tube, 1-2. Inner tube, 1-3. Baffle, 1-4. Gas inlet, 1-5. Liquid inlet, 2. Ion beam condenser I,3. Ion gate I,4. Laser I,5. Deflection electrode group I,6. Straight electrode group I,7. Ion gate II,8. Laser II,9. Straight electrode group II,10. Deflection electrode group II,11. Ion beam condenser II,12. Laser III,13. Octant ion guide, 14. Quadrupole mass filter, 15. Detector, 16. Vacuum chamber, 17. Drift chamber, 18. Gas inlet, 19. Gas outlet.
Detailed Description
As shown in FIG. 1, the invention is schematically shown, and comprises an electrospray device (1), an ion beam expander I (2), an ion gate I (3), a laser I (4), a deflection electrode group I (5), a linear electrode group I (6), an ion gate II (7), a laser II (8), a linear electrode group II (9), a deflection electrode group II (10), an ion beam expander II (11), a laser III (12), an octant ion guide (13), a quadrupole mass filter (14), a detector (15), a vacuum chamber (16), a drift chamber (17), a gas inlet (18) and a gas outlet (19), xyz is a three-dimensional coordinate system, the ion beam expander I (2), the ion gate I (3), the deflection electrode group I (5), the linear electrode group I (6), the ion gate II (7), the linear electrode group II (9), the deflection electrode group II (10) and the ion beam expander II (11) are sequentially connected, and the ion beam expander I (2), the ion gate I (3), the deflection electrode group I (5), the deflection electrode group I (6), the ion gate II (7), the ion beam expander II (11) are sequentially connected, and the ion beam expander II (17) is located in the three-dimensional coordinate system, the linear electrode group I (6), the linear electrode group II (9) and the deflection electrode group II (10) are all composed of annular electrodes with the inner diameter of forty millimeters, a space formed by the centers of the annular electrodes of the deflection electrode group I (5), the linear electrode group I (6), the linear electrode group II (9) and the deflection electrode group II (10) is a drift region, the drift cavity (17) is provided with a starting end and a tail end, the starting end and the tail end are provided with a small hole for passing ion beam, the gas inlet (18) is positioned on the side wall of the tail end of the drift cavity (17), and the gas outlet is formed(19) The side wall at the beginning end of the drift cavity (17), the gas inlet (18) is sequentially connected with a mass flow controller and a gas storage tank, buffer gas is filled in the gas storage tank, the buffer gas is nitrogen or helium, the flow of the buffer gas in the drift cavity (17) can be controlled through the mass flow controller, the buffer gas is discharged from the gas outlet (19) into the drift cavity (17), the flow value of the buffer gas is 0.3SLM, the SLM is standard gas per liter/minute, the gas countercurrent passing through the ion beam condenser I (2) can be formed, neutral molecules can be prevented from entering the drift region, solvent molecules in an electrospray solution can be prevented from entering the drift region, the drift cavity (17) is provided with a gas release valve, the air pressure in the drift region can be controlled by adjusting the flow rate of the buffer air flow and the frequency of the opening and closing of the air release valve, the air pressure value is 1000 Pa, the electrospray device (1) is positioned at one side outside the initial end of the drift cavity (17), the vacuum cavity (16) is positioned at one side outside the tail end of the drift cavity (17), the octupole ion guide (13), the quadrupole mass filter (14) and the detector (15) are sequentially and linearly arranged inside a Yu Zhen cavity (16), the initial end of the vacuum cavity (16) is provided with a small hole for passing through ion beam, the vacuum cavity (16) is connected with a vacuum pump group, the vacuum pump group can vacuumize the vacuum cavity (16), and the vacuum degree is superior to 10 -5 When the electrospray device (1) generates ions of molecules to be detected, the ions sequentially pass through the ion beam expander I (2), the ion gate I (3), the deflection electrode group I (5), the linear electrode group I (6), the ion gate II (7), the linear electrode group II (9), the deflection electrode group II (10), the ion beam expander II (11), the octupole ion guide (13) and the quadrupole mass filter (14) to reach the detector (15), so that an ion beam path is formed. The deflection electrode group I (5) and the deflection electrode group II (10) are respectively provided with nineteen annular electrodes, the annular electrodes are perpendicular to the yz plane, the included angle between the adjacent annular electrodes is five degrees, in the deflection electrode group I (5), the centers of the ten annular electrodes through which the ion beam passes firstly are positioned in the yz plane and positioned on 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the clockwise direction, the centers of the nine annular electrodes through which the ion beam passes next are positioned in the yz plane and positioned on 1/8 circumference with the radius of fifty millimeters and are arranged in the anticlockwise directionIn the deflection electrode group II (10), the centers of ten annular electrodes through which the ion beam passes are positioned in the yz plane and on the 1/8 circumference with the radius of fifty millimeters, and are arranged at equal intervals in the clockwise direction, and the centers of nine annular electrodes through which the ion beam passes next are positioned in the yz plane and on the 1/8 circumference with the radius of fifty millimeters, and are arranged at equal intervals in the anticlockwise direction; a megaohm resistor is connected in series between adjacent annular electrodes in the deflection electrode group I (5) and the deflection electrode group II (10) to divide the voltage, and the deflection electrode group I (5) and the deflection electrode group II (10) respectively provide voltages through two high-voltage power supplies; the linear electrode group I (6) and the linear electrode group II (9) are respectively provided with twenty annular electrodes, the annular electrodes are perpendicular to the yz plane, the annular electrodes of the deflection electrode group II (10) are provided with through holes, and laser emitted by the laser III (12) can enter a drift region along the negative z direction through the through holes; the laser beam emitted by the laser I (4) can enter the drift region through the deflection electrode group I (5), and the laser beam emitted by the laser II (8) can enter the drift region through the linear electrode group II (9); the ion beam-buncher I (2) consists of fifty metal ring electrodes with the thickness of one millimeter, and comprises ten ring electrodes with the inner diameter of forty millimeters and forty ring electrodes with the inner diameter linearly reduced from forty millimeters to two millimeters along the positive direction z, wherein adjacent metal ring electrodes are separated by insulating sheets with the thickness of one millimeter; the ion beam-buncher II (11) connected with the tail end of the drift region consists of forty annular electrodes with the inner diameter in the positive z direction linearly reduced from forty millimeters to two millimeters; the number of grooves on the inner wall of the outer tube (1-1) is four to twelve, and the cross section of each groove is semicircular, square or triangular.
Referring to fig. 2, which is a top view of an electrospray device, referring to fig. 3, which is a side view of the electrospray device, the electrospray device (1) is composed of an outer tube (1-1), an inner tube (1-2), a baffle (1-3), an air inlet (1-4) and a liquid inlet (1-5), wherein the baffle (1-3) can seal one side port of the inner tube (1-2), the outer tube (1-1) and the inner tube (1-2) are both cylindrical, the inner diameter of the outer tube (1-1) is 3000 micrometers, the outer diameter of the inner tube (1-2) is 2700 micrometers, the outer tube (1-1) and the inner tube (1-2) are in a coaxial nested configuration, a liquid channel is arranged between the outer tube (1-1) and the inner tube (1-2), the air inlet (1-4) and the liquid inlet (1-5) are respectively connected with the outer wall of the outer tube (1-1) and are communicated with the liquid channel, and the inner wall of the outer tube (1-1) is provided with dispersed grooves along the axial direction, and the grooves can enable the liquid to locally increase to form a local electric field.
The device for researching molecular photoisomerization comprises an electrospray device (1), an ion beam expander I (2), an ion gate I (3), a laser I (4), a deflection electrode group I (5), a linear electrode group I (6), an ion gate II (7), a laser II (8), a linear electrode group II (9), a deflection electrode group II (10), an ion beam expander II (11), a laser III (12), an octapole ion guide (13), a quadrupole mass filter (14), a detector (15), a vacuum chamber (16), a drift chamber (17), a gas inlet (18) and a gas outlet (19), xyz is a three-dimensional coordinate system, the ion beam expander I (2), the ion gate I (3), the deflection electrode group I (5), the linear electrode group I (6), the ion gate II (7), the linear electrode group II (9), the deflection electrode group II (10) and the ion beam expander II (11) are sequentially connected, and the ion beam expander I (2), the ion gate I (3), the ion gate I (5), the deflection electrode group I (6), the ion gate II (7), the ion gate II (10) and the ion beam expander II (11) are sequentially connected, and the ion beam expander I (2), the ion gate I (3), the deflection electrode group I (5), the deflection electrode group II (6), the ion gate II (7) and the ion beam expander II (11) are in the three-dimensional coordinate system The linear electrode group I (6), the linear electrode group II (9) and the deflection electrode group II (10) are all composed of annular electrodes with the inner diameter of forty millimeters, a space formed by the centers of the annular electrodes of the linear electrode group I (5), the linear electrode group I (6), the linear electrode group II (9) and the deflection electrode group II (10) is a drift region, the drift chamber (17) is provided with a starting end and a tail end, the starting end and the tail end are respectively provided with a small hole for passing an ion beam, the gas inlet (18) is positioned on the side wall of the tail end of the drift chamber (17), the gas outlet (19) is positioned on the side wall of the starting end of the drift chamber (17), the gas inlet (18) is sequentially connected with a mass flow controller and a gas storage tank, the gas storage tank is filled with buffer gas, the buffer gas is nitrogen or helium, the buffer gas flow in the drift chamber (17) can be controlled through the mass flow controller, the buffer gas is discharged from the gas outlet (19) into the drift chamber (17), the buffer gas flow value is 0.3S, and is standard gas per liter/minute, and the buffer gas flow value can be obtainedCan form a gas countercurrent through the ion beam expander I (2), can prevent neutral molecules from entering a drift region, can prevent solvent molecules in electrospray solution from entering the drift region, a drift chamber (17) is provided with a bleed valve, the gas pressure in the drift region can be controlled by adjusting the flow rate of buffer gas flow and the frequency of opening and closing of the bleed valve, the gas pressure value is 1000 Pa, an electrospray device (1) is positioned at the outer side of the initial end of the drift chamber (17), a vacuum chamber (16) is positioned at the outer side of the tail end of the drift chamber (17), an octapole ion guide (13), a quadrupole mass filter (14) and a detector (15) are sequentially arranged in a Yu Zhen cavity (16), the initial end of the vacuum chamber (16) is provided with a small hole for passing through ion beam, the vacuum chamber (16) is connected with a vacuum pump set, and the vacuum degree is superior to 10 -5 When the electrospray device (1) generates ions of molecules to be detected, the ions sequentially pass through the ion beam expander I (2), the ion gate I (3), the deflection electrode group I (5), the linear electrode group I (6), the ion gate II (7), the linear electrode group II (9), the deflection electrode group II (10), the ion beam expander II (11), the octupole ion guide (13) and the quadrupole mass filter (14) to reach the detector (15), so that an ion beam path is formed. The deflection electrode group I (5) and the deflection electrode group II (10) are respectively provided with nineteen annular electrodes, the annular electrodes are perpendicular to the yz plane, the included angle between the adjacent annular electrodes is five degrees, in the deflection electrode group I (5), the centers of the ten annular electrodes through which the ion beam passes firstly are positioned in the yz plane and are positioned on the 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the clockwise direction, the centers of the nine annular electrodes through which the ion beam passes next are positioned in the yz plane and are positioned on the 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the anticlockwise direction, in the deflection electrode group II (10), the centers of the ten annular electrodes through which the ion beam passes firstly are positioned in the yz plane and are positioned on the 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the clockwise direction, and the centers of the nine annular electrodes through which the ion beam passes next are positioned in the yz plane and are positioned on the 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the anticlockwise direction; the saidA megaohm resistor is connected in series between adjacent annular electrodes in the deflection electrode group I (5) and the deflection electrode group II (10) to divide the voltage, and the deflection electrode group I (5) and the deflection electrode group II (10) respectively provide voltages through two high-voltage power supplies; the linear electrode group I (6) and the linear electrode group II (9) are respectively provided with twenty annular electrodes, the annular electrodes are perpendicular to the yz plane, the annular electrodes of the deflection electrode group II (10) are provided with through holes, and laser emitted by the laser III (12) can enter a drift region along the negative z direction through the through holes; the laser beam emitted by the laser I (4) can enter the drift region through the deflection electrode group I (5), and the laser beam emitted by the laser II (8) can enter the drift region through the linear electrode group II (9); the ion beam-buncher I (2) consists of fifty metal ring electrodes with the thickness of one millimeter, and comprises ten ring electrodes with the inner diameter of forty millimeters and forty ring electrodes with the inner diameter linearly reduced from forty millimeters to two millimeters along the positive direction z, wherein adjacent metal ring electrodes are separated by insulating sheets with the thickness of one millimeter; the ion beam-buncher II (11) connected with the tail end of the drift region consists of forty annular electrodes with the inner diameter in the positive z direction linearly reduced from forty millimeters to two millimeters; the electrospray device (1) comprises an outer tube (1-1), an inner tube (1-2), a baffle (1-3), an air inlet (1-4) and a liquid inlet (1-5), wherein the baffle (1-3) can seal one side port of the inner tube (1-2), the outer tube (1-1) and the inner tube (1-2) are both cylindrical, the inner diameter of the outer tube (1-1) is 3000 micrometers, the outer diameter of the inner tube (1-2) is 2700 micrometers, the outer tube (1-1) and the inner tube (1-2) are in coaxial nested configuration, a liquid channel is arranged between the outer tube (1-1) and the inner tube (1-2), the air inlet (1-4) and the liquid inlet (1-5) are respectively connected with the outer wall of the outer tube (1-1) and are communicated with the liquid channel, and the inner wall of the outer tube (1-1) is provided with dispersed grooves along the axial direction of the outer tube, and the grooves can enable liquid to locally form a protruding shape to increase a local electric field. The number of grooves on the inner wall of the outer tube (1-1) is four to twelve, and the cross section of each groove is semicircular, square or triangular.
During the test, ions generated by electrospray accumulate in the ion beam condenser I (2), the ion gate I (3) is periodically opened to enable the ion beam to be injected into the front section of the drift region where the deflection electrode group I (5) is positioned, and the ions are subjected to the action of a drift electric field, move towards the tail end of the drift cavity (17) and collide with nitrogen or helium filled in the drift region; ions leave the drift region and are collected by the ion beam combiner II (11), then sequentially pass through a small hole at the tail end of the drift cavity (17), a small hole at the starting end of the vacuum cavity (16), the octupole ion guide (13) and the quadrupole mass filter (14), and finally enter the detector (15). The ions can be irradiated laterally by the laser after passing through the ion beam expander I (2) or through the drift region after the ion beam expander II (11), and axially by the laser when in the middle of the drift region, i.e. in different excitation modes.
The invention is used for researching photoisomerization of molecular ions in gas phase, has various light excitation modes, can be used for researching photodecomposition of molecular ions, and can identify charged products thereof from the two aspects of migration rate and quality; in addition, the spray head provided by the invention is provided with the annular liquid channel, so that relatively uniform atomized liquid drops can be sprayed, the quality of an ion packet entering the drift region is improved, and the signal-to-noise ratio of an ion signal obtained by the detector is increased.
Claims (2)
1. The device for researching molecular photoisomerization comprises an electrospray device (1), an ion beam expander I (2), an ion gate I (3), a laser I (4), a deflection electrode group I (5), a linear electrode group I (6), an ion gate II (7), a laser II (8), a linear electrode group II (9), a deflection electrode group II (10), an ion beam expander II (11), a laser III (12), an octapole ion guide (13), a quadrupole mass filter (14), a detector (15), a vacuum chamber (16), a drift chamber (17), a gas inlet (18) and a gas outlet (19), xyz is a three-dimensional coordinate system, the ion beam expander I (2), the ion gate I (3), the deflection electrode group I (5), the linear electrode group I (6), the ion gate II (7), the linear electrode group II (9), the deflection electrode group II (10) and the ion beam expander II (11) are sequentially connected, and the ion beam expander I (2), the ion gate I (3), the ion gate I (5), the deflection electrode group I (6), the ion gate II (7), the ion beam expander II (11) are sequentially connected, and the ion beam expander I (5), the deflection electrode group II (7), the ion gate II (10) and the ion beam expander II (11) are in the three-dimensional coordinate system Linear electrode group I (6), linear electrode group II (9) and deflectionThe electrode group II (10) is composed of annular electrodes with the inner diameter of forty millimeters, the space formed by the centers of the annular electrodes of the deflection electrode group I (5), the straight line electrode group I (6), the straight line electrode group II (9) and the deflection electrode group II (10) is a drift region, the drift cavity (17) is provided with a starting end and a tail end, the starting end and the tail end are respectively provided with a small hole for passing ion beam current, the gas inlet (18) is positioned on the side wall of the tail end of the drift cavity (17), the gas outlet (19) is positioned on the side wall of the starting end of the drift cavity (17), the gas inlet (18) is sequentially connected with a mass flow controller and a gas storage tank, buffer gas is filled in the gas storage tank, and the buffer gas is nitrogen or helium, the flow rate of the buffer gas in the drift cavity (17) can be controlled through a mass flow controller, the buffer gas is discharged from a gas outlet (19) to the drift cavity (17), the flow rate of the buffer gas is 0.3SLM, the reverse flow of the gas passing through the ion beam expander I (2) can be formed, neutral molecules can be prevented from entering the drift region, solvent molecules in electrospray solution can be prevented from entering the drift region, the drift cavity (17) is provided with a deflation valve, the gas pressure in the drift region can be controlled by adjusting the flow rate of the buffer gas and the frequency of opening and closing the deflation valve, the gas pressure is 1000 Pa, the electrospray device (1) is positioned on the outer side of the initial end of the drift cavity (17), the vacuum cavity (16) is positioned on the outer side of the tail end of the drift cavity (17), the eight-pole ion guide (13), the quadrupole mass filter (14) and the detector (15) are sequentially arranged in a Yu Zhen cavity (16) in a linear mode, a small hole is formed in the starting end of the vacuum cavity (16) and used for passing through ion beam current, a vacuum pump set is connected to the vacuum cavity (16), the vacuum pump set can vacuumize the vacuum cavity (16), and the vacuum degree is superior to 10 -5 When the electrospray device (1) generates ions of molecules to be detected, the ions sequentially pass through the ion beam expander I (2), the ion gate I (3), the deflection electrode group I (5), the linear electrode group I (6), the ion gate II (7), the linear electrode group II (9), the deflection electrode group II (10), the ion beam expander II (11), the octupole ion guide (13) and the quadrupole mass filter (14) to reach the detector (15), so that an ion beam path is formed,
the method is characterized in that: the deflection electrode group I (5) and the deflection electrode group II (10) are respectively provided with nineteen annular electrodes, the annular electrodes are perpendicular to the yz plane, the included angle between the adjacent annular electrodes is five degrees, in the deflection electrode group I (5), the centers of the ten annular electrodes through which the ion beam passes firstly are positioned in the yz plane and are positioned on the 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the clockwise direction, the centers of the nine annular electrodes through which the ion beam passes next are positioned in the yz plane and are positioned on the 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the anticlockwise direction, in the deflection electrode group II (10), the centers of the ten annular electrodes through which the ion beam passes firstly are positioned in the yz plane and are positioned on the 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the clockwise direction, and the centers of the nine annular electrodes through which the ion beam passes next are positioned in the yz plane and are positioned on the 1/8 circumference with the radius of fifty millimeters and are arranged at equal intervals in the anticlockwise direction; a megaohm resistor is connected in series between adjacent annular electrodes in the deflection electrode group I (5) and the deflection electrode group II (10) to divide the voltage, and the deflection electrode group I (5) and the deflection electrode group II (10) respectively provide voltages through two high-voltage power supplies; the linear electrode group I (6) and the linear electrode group II (9) are respectively provided with twenty annular electrodes, the annular electrodes are perpendicular to the yz plane, the annular electrodes of the deflection electrode group II (10) are provided with through holes, and laser emitted by the laser III (12) can enter a drift region along the negative z direction through the through holes; the laser beam emitted by the laser I (4) can enter the drift region through the deflection electrode group I (5), and the laser beam emitted by the laser II (8) can enter the drift region through the linear electrode group II (9); the ion beam-buncher I (2) consists of fifty metal ring electrodes with the thickness of one millimeter, and comprises ten ring electrodes with the inner diameter of forty millimeters and forty ring electrodes with the inner diameter linearly reduced from forty millimeters to two millimeters along the positive direction z, wherein adjacent metal ring electrodes are separated by insulating sheets with the thickness of one millimeter; the ion beam-buncher II (11) connected with the tail end of the drift region consists of forty annular electrodes with the inner diameter in the positive z direction linearly reduced from forty millimeters to two millimeters; the electrospray device (1) comprises an outer tube (1-1), an inner tube (1-2), a baffle (1-3), an air inlet (1-4) and a liquid inlet (1-5), wherein the baffle (1-3) can seal one side port of the inner tube (1-2), the outer tube (1-1) and the inner tube (1-2) are both cylindrical, the inner diameter of the outer tube (1-1) is 3000 micrometers, the outer diameter of the inner tube (1-2) is 2700 micrometers, the outer tube (1-1) and the inner tube (1-2) are in coaxial nested configuration, a liquid channel is arranged between the outer tube (1-1) and the inner tube (1-2), the air inlet (1-4) and the liquid inlet (1-5) are respectively connected with the outer wall of the outer tube (1-1) and are communicated with the liquid channel, and the inner wall of the outer tube (1-1) is provided with dispersed grooves along the axial direction of the outer tube, and the grooves can enable liquid to locally form a protruding shape to increase a local electric field.
2. The apparatus for studying molecular photoisomerization of claim 1, further comprising: the number of grooves on the inner wall of the outer tube (1-1) is four to twelve, and the cross section of each groove is semicircular, square or triangular.
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