CN109192648A - A kind of free radical photoproduct test method - Google Patents
A kind of free radical photoproduct test method Download PDFInfo
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- CN109192648A CN109192648A CN201810950831.3A CN201810950831A CN109192648A CN 109192648 A CN109192648 A CN 109192648A CN 201810950831 A CN201810950831 A CN 201810950831A CN 109192648 A CN109192648 A CN 109192648A
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Abstract
The present invention relates to spectrochemistry field, a kind of free radical photoproduct test method, helium is passed through drift chamber II, and nitrogen is passed through cushion chamber, flow speed value 80SCCM；Mass flow controller is controlled, testing sample solution injects liquid storage tank, and flow velocity is 0.02 ml/min to 0.2 ml/min；It is separately turned on driver I and driver II, it can be there are two types of operating mode；Drop enters vacuum chamber, and forms ion packet, then forms ion beam current, and ion beam current reaches ion bunch device II by ion bunch device I；It adjusts to be applied to respectively and extracts grid, imprison grid and enter the potential on grid, so that a part of ion in ion beam current is trapped in the section IV of ion bunch device II；Laser is injected section IV and is irradiated on ion, and light reaction occurs and generates photoproduct；Potential is adjusted, projects the charged particle in photoproduct from the section V of ion bunch device II, and eventually enter into detector after passing sequentially through ion bunch device III, ion bunch device IV and quadrupole rod.
Description
Technical field
The present invention relates to spectrochemistry fields, especially a kind of to have particular sample solution atomization method and examine
Compared with a kind of free radical photoproduct test method of the light reaction product of the free radical of multiple types.
Background technique
The device of the light reaction product of research molecule or free radical etc. studied usually in vacuum environment testing molecule from
Beamlet stream, it usually needs so that entering vacuum environment, prior art defect one: existing skill after the solution atomization containing sample to be tested
Certain devices are come with method of electrospraying so that the solution atomization containing sample to be tested, has certain want to solvent in solution in art
It asks, i.e., must be polar solvent, and high voltage must be applied to liquid when electron spray work, which has limited method of electrospraying to be applicable in
Sample type；Prior art defect two: certain devices are made by directly applying stressed method to liquid in the prior art
Liquid sprays and is formed drop, the size-constrained internal diameter in drop spout of the drop of this method generation, i.e., can not be formed compared with
Small drop；Prior art defect three: in ion beam current test device in the prior art, multi-stage vacuum pump group is generallyd use
Different chambers is vacuumized, the vacuum difference between different cavity will lead to ion beam current and form sinuous flow, to influence final spy
Efficiency is surveyed, a kind of free radical photoproduct test method is able to solve problem.
Summary of the invention
To solve the above-mentioned problems, a kind of free radical photoproduct test method of the present invention is sprayed using the method for liquid resonant
Drop is projected, and cushion chamber is added in the vacuum chamber, reduces influence of the draught head to ion beam current of different cavity, special designing
Ion bunch device reduces the volume of device, and can reduce the pumping speed of vacuum pump group.
The technical scheme adopted by the invention is that:
Free radical photoproduct test device mainly includes laser, liquid drop ejector, vacuum chamber, ion bunch device I, ion
Beam buncher II, ion bunch device III, ion bunch device IV, quadrupole rod, detector, vacuum pump group I, vacuum pump group II, vacuum pump
There is starting point and end successively to have in vacuum chamber from starting point to end for group III and ionization device, the vacuum chamber
Sample cavity, drift chamber I, drift chamber II, cushion chamber and collision chamber, the sample cavity, cushion chamber and collision chamber are connected separately with very
Empty pump group III, vacuum pump group II and vacuum pump group I；The ion bunch device I, ion bunch device II, ion bunch device III, from
Sub- beam buncher IV and quadrupole rod are respectively positioned in the vacuum chamber, and ion bunch device I is connected between sample cavity and drift chamber I, from
Sub- beam buncher II is connected between drift chamber I and drift chamber II, ion bunch device III be connected to drift chamber II and cushion chamber it
Between, ion bunch device IV is connected between cushion chamber and collision chamber, and it is intracavitary that quadrupole rod is located at collision；The liquid drop ejector connection
Ionization device is installed in sample cavity, the sample cavity, sample cavity side cavity wall has aperture, what liquid drop ejector ejected
Drop can be entered sample cavity by the aperture and form ion packet under the action of the ionization device, then in vacuum pump
Ion beam current is formed under the action of group III, the sample cavity has window, and the laser of laser transmitting can pass through the window
Into vacuum chamber；The detector connection collision chamber, the cavity wall for colliding chamber have through-hole, and the ion beam current collided in chamber can lead to
It crosses the through-hole and enters detector；Cushion chamber has buffer gas entrance, and drift chamber II has drift carrier gas inlet；Ion bunch
Device I, ion bunch device III and ion bunch device IV are made of 20 annular electrodes with a thickness of 0.4 millimeter respectively, adjacent
0.5 millimeter is divided between annular electrode, 20 annular electrode internal diameters are linearly to reduce along z positive direction from 45 millimeters
To two millimeters, 100 kilo-ohms of resistance is in series between each annular electrode respectively.Liquid drop ejector mainly includes mass flow control
Device, inlet tube, cavity, liquid storage tank, driver I, driver II and jet port processed, the cavity are cylinder, are had in cavity
The liquid storage tank and jet port, the liquid storage tank are cylinder, and the upper bottom surface and bottom surface of liquid storage tank are connected separately with driver I
With driver II, when driver I and driver II works, the volume of the liquid storage tank can generate minor change, the injection
The pore diameter range of mouth is 40 to 400 microns, and the liquid storage pool volume range is four to eight milliliters, mass flow controller
Outlet end connects liquid storage tank by inlet tube, arrival end is connected with sample solution fluid reservoir；Have along z just in ion bunch device II
The annular electrode for the different pore size that direction is arranged successively, the annular electrode is with a thickness of between 0.4 millimeter and adjacent annular electrode
Between be divided into 0.5 millimeter, ion bunch device II successively has five sections, is a section I, section II, section III, section IV and section V respectively；I is by seven for section
A internal diameter is 50 millimeters of annular electrode composition, and section II is made of eight annular electrodes, the internal diameter of eight annular electrodes
It is respectively 45 millimeters, 40 millimeters, 35 millimeters, 33 millimeters, 30 millimeters, 27 millimeters, 24 millimeters and 21 millimeters along z positive direction, section III
It is made of three annular electrodes, the internal diameter of three annular electrodes is respectively 28 millimeters, 33 millimeters and 38 millis along z positive direction
Rice, section IV are made of the annular electrode that five internal diameters are 50 millimeters, and section V is made of six annular electrodes, six annulars
The internal diameter of electrode is respectively 46 millimeters, 42 millimeters, 38 millimeters, 34 millimeters, 30 millimeters and 26 millimeters along z positive direction, ion bunch
Have in device II and extract grid, imprison grid, into grid and jet disturbance device, into grid, imprison grid and extracts grid
It is sequentially located in section IV along z positive direction, jet disturbance device is located in section I；Section I can receive the free ion beam of rapid divergence
Stream, section II can be by ion focusings, and the space of section III, section IV and section V composition can be used in trapped ion, section V be it is final from
Son convergence region and the outlet with ion.
The ejector principle of liquid drop ejector: jet port is parallel with liquid storage tank liquid level plane under original state；Opening driver I
After driver II, driver is vibrated with certain frequency, is moved back and forth with certain period to liquid storage tank outside and inside,
Driver is to during liquid storage tank movement outside, liquid storage tank volume enlargement under the action of driver, the liquid level at jet port
It is bent into liquid storage tank, liquid level the degree of bending constantly increases with the expansion of liquid storage pool volume；In driver into liquid storage tank
During side moves, liquid storage tank volume under the action of driver reduces, and curved liquid level receives liquid in liquid storage tank
Active force, for liquid storage tank during volume continues reduction under the action of driver, curved liquid level center will form one
A superfine liquid jet；In next vibration period of driver, driver is to liquid storage tank movement outside, liquid storage pool volume
Start to expand, most of liquid in the liquid jet for having gone out jet port plane be retracted in liquid storage tank, in the liquid
The small amount of liquids at the tip of body jet stream will form a very small drop, so that drop goes out liquid storage tank.
A kind of the step of free radical photoproduct test method, is as follows:
Helium is passed through drift chamber II by one, nitrogen is passed through cushion chamber, typical flow value is 80SCCM；
Two, control mass flow controller, testing sample solution are injected liquid storage tank, flow velocity representative value is 0.02 to 0.2
Ml/min；
Three, are separately turned on driver I and driver II, operating mode one, the vibration frequency one of driver I and driver II
It causes, representative value is 0.8 to 1.5kHz；The vibration frequency of operating mode two, driver I and driver II are inconsistent, driver I's
Representative value is 0.7 to 1.0kHz, and the representative value of driver II is 1.3 to 1.6kHz；
The drop that four, liquid drop ejectors eject enters vacuum chamber, and forms ion under the action of the ionization device
Packet, then forms ion beam current under the action of vacuum pump group III, and ion beam current reaches ion bunch by ion bunch device I
Device II；
Five, are adjusted to be applied to respectively and are extracted grid, imprison grid and enter the potential on grid, so that in ion beam current
A part of ion is trapped in the section IV of ion bunch device II；
The laser of six, lasers transmitting is injected section IV and is irradiated on ion, and light reaction occurs and generates photoproduct；
Seven, are adjusted to be applied to respectively and are extracted grid, imprison grid and enter the potential on grid, so that the band in photoproduct
Charged particle is projected from the section V of ion bunch device II, and after passing sequentially through ion bunch device III, ion bunch device IV and quadrupole rod
Eventually enter into detector；
Eight, analyze the data of detector acquisition, obtain the relevant information of the light reaction product of free radical.
The beneficial effects of the present invention are:
Special droplet discharge method in the present invention is capable of forming the size drop more much smaller than drop jet port internal diameter,
And the polarity no requirement (NR) to solvent, without applying high voltage when injection, applicable sample type is more, secondly, being added in vacuum chamber
Cushion chamber, can reduce the loss of ion beam current, furthermore, the ion bunch device of special designing can carry out respectively drawing for ion
Enter, imprison and project operation, so that device volume reduces, and can reduce the pumping speed of vacuum pump group.
Detailed description of the invention
It is further illustrated below with reference to figure of the invention:
Fig. 1 is schematic diagram of the present invention；
Fig. 2 is liquid drop ejector enlarged diagram；
Fig. 3 is the top view of Fig. 2；
Fig. 4 is ion bunch device II internal cross section enlarged diagram；
Fig. 5 to Figure 10 is the jet port enlarged diagram and ejector principle schematic diagram of liquid drop ejector.
In figure, 1. lasers, 2. liquid drop ejectors, 2-1. mass flow controller, 2-2. inlet tube, 2-3. cavity, 2-
4. liquid storage tank, 2-5. driver I, 2-6. driver II, 2-7. jet port, 3. vacuum chambers, 3-1. sample cavity, 3-2. drift chamber I,
3-3. drift chamber II, 3-4. cushion chamber, 3-5. collide chamber, 4. ion bunch device I, 5. ion bunch device II, 5-1. section I, 5-2.
Section II, 5-3. sections of III, 5-4. sections of IV, 5-5. sections of V, 5-6. extraction grid, 5-7. imprison grid, and 5-8. enters grid, and 5-9. is penetrated
Interference unit is flowed, 6. ion bunch device III, 7. ion bunch device IV, 8. quadrupole rods, 9. detectors, 10. vacuum pump group I, 11. is true
Empty pump group II, 12. vacuum pump group III.
Specific embodiment
If Fig. 1 is schematic diagram of the present invention, xyz is three-dimensional coordinate system, mainly includes laser (1), liquid drop ejector
(2), vacuum chamber (3), ion bunch device I (4), ion bunch device II (5), ion bunch device III (6), ion bunch device IV
(7), quadrupole rod (8), detector (9), vacuum pump group I (10), vacuum pump group II (11), vacuum pump group III (12) and ionization dress
It sets, the vacuum chamber (3) has starting point and end, in vacuum chamber (3), successively has sample cavity from starting point to end
(3-1), drift chamber I (3-2), drift chamber II (3-3), cushion chamber (3-4) and collision chamber (3-5), the sample cavity (3-1) are delayed
It rushes chamber (3-4) and collision chamber (3-5) is connected separately with vacuum pump group III (12), vacuum pump group II (11) and vacuum pump group I
(10)；The ion bunch device I (4), ion bunch device II (5), ion bunch device III (6), ion bunch device IV (7) and four
Pole bar (8) is respectively positioned in the vacuum chamber (3), ion bunch device I (4) be connected to sample cavity (3-1) and drift chamber I (3-2) it
Between, ion bunch device II (5) is connected between drift chamber I (3-2) and drift chamber II (3-3), ion bunch device III (6) connection
Between drift chamber II (3-3) and cushion chamber (3-4), ion bunch device IV (7) is connected to cushion chamber (3-4) and collision chamber (3-
5) between, quadrupole rod (8) is located in collision chamber (3-5)；The liquid drop ejector (2) is connected to sample cavity (3-1), the sample introduction
Ionization device is installed, sample cavity (3-1) side cavity wall has aperture, the drop that liquid drop ejector (2) ejects in chamber (3-1)
Sample cavity (3-1) can be entered by the aperture and form ion packet under the action of the ionization device, then in vacuum
Ion beam current is formed under the action of pump group III (12), the sample cavity (3-1) has window, the laser energy of laser (1) transmitting
Vacuum chamber (3) are enough entered by the window；Detector (9) connection collision chamber (3-5), the cavity wall tool of collision chamber (3-5)
There is through-hole, the ion beam current in collision chamber (3-5) can be entered detector (9) by the through-hole；Cushion chamber (3-4) has slow
Gas access is rushed, drift chamber II (3-3) has drift carrier gas inlet；Ion bunch device I (4), ion bunch device III (6) and from
Sub- beam buncher IV (7) is made of 20 annular electrodes with a thickness of 0.4 millimeter respectively, and adjacent annular electrode gap is 0.5
Millimeter, 20 annular electrode internal diameters be along z positive direction from 45 millimeters it is linear reduce to two millimeters, each annular
100 kilo-ohms of resistance is in series between electrode respectively.
If Fig. 2 is liquid drop ejector enlarged diagram, if Fig. 3 is the top view of Fig. 2, liquid drop ejector (2) mainly includes
Mass flow controller (2-1), inlet tube (2-2), cavity (2-3), liquid storage tank (2-4), driver I (2-5), driver II
(2-6) and jet port (2-7), the cavity (2-3) are cylinder, have the liquid storage tank (2-4) in cavity (2-3) and spray
Mouth (2-7), the liquid storage tank (2-4) are cylinder, and the upper bottom surface and bottom surface of liquid storage tank (2-4) are connected separately with driver I
(2-5) and driver II (2-6), when driver I (2-5) and driver II (2-6) works, the appearance of the liquid storage tank (1-4)
Product can generate minor change, and the pore diameter range of the jet port (2-7) is 40 to 400 microns, and the liquid storage tank (2-4) is held
Product range is four to eight milliliters, the outlet end of mass flow controller (2-1) by inlet tube (2-2) connection liquid storage tank (2-4),
Arrival end is connected with sample solution fluid reservoir.
If Fig. 4 is ion bunch device II internal cross section enlarged diagram, have in ion bunch device II (5) along z positive direction
The annular electrode for the different pore size being arranged successively, the annular electrode are spaced with a thickness of between 0.4 millimeter and adjacent annular electrode
It is 0.5 millimeter, it is a section I (5-1), section II (5-2), section III (5-3), section respectively that ion bunch device II (5), which successively has five sections,
IV (5-4) and section V (5-5)；Section I (5-1) is made of the annular electrode that seven internal diameters are 50 millimeters, and section II (5-2) is by eight
Annular electrode composition, the internal diameter of eight annular electrodes respectively are 45 millimeters, 40 millimeters, 35 millimeters, 33 along z positive direction
Millimeter, 30 millimeters, 27 millimeters, 24 millimeters and 21 millimeters, section III (5-3) is made of three annular electrodes, three annular electros
The internal diameter of pole respectively is 28 millimeters, 33 millimeters and 38 millimeters along z positive direction, and section IV (5-4) is 50 millis by five internal diameters
The annular electrode composition of rice, section V (5-5) is made of six annular electrodes, the internal diameters of six annular electrodes along z positive direction according to
Secondary is respectively 46 millimeters, 42 millimeters, 38 millimeters, 34 millimeters, 30 millimeters and 26 millimeters, has in ion bunch device II (5) and extracts
Grid (5-6) imprisons grid (5-7), into grid (5-8) and jet disturbance device (5-9), into grid (5-8), imprison grid
(5-7) and extraction grid (5-6) are sequentially located in a section IV (5-4) along z positive direction, and jet disturbance device (5-9) is located at section I (5-1)
It is interior；Section I (5-1) can receive the free ion line of rapid divergence, section II (5-2) can by ion focusing, section III (5-3),
The space of section IV (5-4) and section V (5-5) composition can be used in trapped ion, section V (5-5) for final focusing ions region and
Outlet with ion.
If Fig. 5 to Figure 10 is the jet port enlarged diagram and ejector principle schematic diagram of liquid drop ejector, jet port (2-7)
Lower section is the liquid of liquid storage tank (2-4), and arrow indicates the active force of liquid internal in figure, such as jet port (2- under Fig. 5 original state
7) parallel with liquid storage tank (2-4) liquid level plane；After opening driver I (2-5) and driver II (2-6), driver is with certain
Frequency vibration, is moved back and forth with certain period on the outside of liquid storage tank (2-4) and inside, driver to liquid storage tank (2-4) outside
Side move during, liquid storage tank (2-4) volume enlargement under the action of driver, as the liquid level at Fig. 6 jet port (2-7) to
Bending in liquid storage tank (2-4), as Fig. 7 liquid level the degree of bending constantly increases with the expansion of liquid storage tank (2-4) volume；It is driving
To during liquid storage tank (2-4) medial motion, liquid storage tank (2-4) volume under the action of driver reduces device, as Fig. 8 is bent
Liquid level receive the active force of liquid in liquid storage tank (2-4), liquid storage tank (2-4) volume under the action of driver continues to reduce
During, as the curved liquid level center Fig. 9 will form a superfine liquid jet；In next vibration of driver
In period, driver starts to expand to liquid storage tank (2-4) movement outside, liquid storage tank (2-4) volume, will go out jet port (2-
7) most of liquid in the liquid jet of plane retracts in liquid storage tank (2-4), in the small of the tip of the liquid jet
Partially liq will form a very small drop, such as Figure 10 to which drop goes out liquid storage tank (2-4).The present invention is using driving
The direction of vibration of device is vertical with the direction that drop sprays, and advantage is response time of the drop injection to the open and close of driver
It is shorter, in addition, liquid can be sprayed with a variety of vibration modes with the driver of different frequency and amplitude vibration by using two
Drop, to meet different needs, two drivers are in operating mode one with identical frequency and amplitude vibration, in operating mode two
When two drivers are with different frequency and amplitude vibration, the droplet size ejected is not consistent, and the smallest drop can compare
The drop that operating mode one ejects wants small, can be by controlling the pumping speed of vacuum pump group come so that biggish drop and vacuum chamber
Wall collision, so that lesser drop is left in the vacuum chamber, the lesser ion beam current of Formation cross-section product.
Free radical photoproduct test device mainly includes that laser (1), liquid drop ejector (2), vacuum chamber (3), ion are poly-
Beam device I (4), ion bunch device II (5), ion bunch device III (6), ion bunch device IV (7), quadrupole rod (8), detector
(9), vacuum pump group I (10), vacuum pump group II (11), vacuum pump group III (12) and ionization device, xyz are three dimensional space coordinate
System, the vacuum chamber (3) have starting point and end, in vacuum chamber (3), successively have sample cavity from starting point to end
(3-1), drift chamber I (3-2), drift chamber II (3-3), cushion chamber (3-4) and collision chamber (3-5), the sample cavity (3-1) are delayed
It rushes chamber (3-4) and collision chamber (3-5) is connected separately with vacuum pump group III (12), vacuum pump group II (11) and vacuum pump group I
(10)；The ion bunch device I (4), ion bunch device II (5), ion bunch device III (6), ion bunch device IV (7) and four
Pole bar (8) is respectively positioned in the vacuum chamber (3), ion bunch device I (4) be connected to sample cavity (3-1) and drift chamber I (3-2) it
Between, ion bunch device II (5) is connected between drift chamber I (3-2) and drift chamber II (3-3), ion bunch device III (6) connection
Between drift chamber II (3-3) and cushion chamber (3-4), ion bunch device IV (7) is connected to cushion chamber (3-4) and collision chamber (3-
5) between, quadrupole rod (8) is located in collision chamber (3-5)；The liquid drop ejector (2) is connected to sample cavity (3-1), the sample introduction
Ionization device is installed, sample cavity (3-1) side cavity wall has aperture, the drop that liquid drop ejector (2) ejects in chamber (3-1)
Sample cavity (3-1) can be entered by the aperture and form ion packet under the action of the ionization device, then in vacuum
Ion beam current is formed under the action of pump group III (12), the sample cavity (3-1) has window, the laser energy of laser (1) transmitting
Vacuum chamber (3) are enough entered by the window；Detector (9) connection collision chamber (3-5), the cavity wall tool of collision chamber (3-5)
There is through-hole, the ion beam current in collision chamber (3-5) can be entered detector (9) by the through-hole；Cushion chamber (3-4) has slow
Gas access is rushed, drift chamber II (3-3) has drift carrier gas inlet；Ion bunch device I (4), ion bunch device III (6) and from
Sub- beam buncher IV (7) is made of 20 annular electrodes with a thickness of 0.4 millimeter respectively, and adjacent annular electrode gap is 0.5
Millimeter, 20 annular electrode internal diameters be along z positive direction from 45 millimeters it is linear reduce to two millimeters, each annular
100 kilo-ohms of resistance is in series between electrode respectively；Liquid drop ejector (2) mainly includes mass flow controller (2-1), feed liquor
Manage (2-2), cavity (2-3), liquid storage tank (2-4), driver I (2-5), driver II (2-6) and jet port (2-7), the chamber
Body (2-3) is cylinder, has the liquid storage tank (2-4) and jet port (2-7) in cavity (2-3), the liquid storage tank (2-4) is
Cylinder, the upper bottom surface and bottom surface of liquid storage tank (2-4) are connected separately with driver I (2-5) and driver II (2-6), work as drive
When dynamic device I (2-5) and driver II (2-6) work, the volume of the liquid storage tank (1-4) can generate minor change, the injection
The pore diameter range of mouth (2-7) is 40 to 400 microns, and liquid storage tank (2-4) the volume range is four to eight milliliters, quality stream
The outlet end of amount controller (2-1) is connected with sample solution liquid storage by inlet tube (2-2) connection liquid storage tank (2-4), arrival end
Tank；There is the annular electrode for the different pore size being arranged successively along z positive direction, the annular electrode is thick in ion bunch device II (5)
0.5 millimeter is divided between spending between 0.4 millimeter and adjacent annular electrode, ion bunch device II (5) successively has five sections, respectively
It is a section I (5-1), section II (5-2), section III (5-3), section IV (5-4) and section V (5-5)；Section I (5-1) is 50 by seven internal diameters
The annular electrode composition of millimeter, section II (5-2) are made of eight annular electrodes, and the internal diameter of eight annular electrodes is along z pros
To respectively being 45 millimeters, 40 millimeters, 35 millimeters, 33 millimeters, 30 millimeters, 27 millimeters, 24 millimeters and 21 millimeters, section III (5-
3) be made of three annular electrodes, the internal diameters of three annular electrodes along z positive direction respectively be 28 millimeters, 33 millimeters and
38 millimeters, section IV (5-4) is made of the annular electrode that five internal diameters are 50 millimeters, and section V (5-5) is by six annular electrode groups
At the internal diameter of six annular electrodes respectively is 46 millimeters, 42 millimeters, 38 millimeters, 34 millimeters, 30 millis along z positive direction
Rice and 26 millimeters have in ion bunch device II (5) and extract grid (5-6), imprison grid (5-7), into grid (5-8) and penetrate
It flows interference unit (5-9), is sequentially located at a section IV along z positive direction into grid (5-8), imprison grid (5-7) and extraction grid (5-6)
In (5-4), jet disturbance device (5-9) is located in section I (5-1)；Section I (5-1) can receive the free ion line of rapid divergence,
The space formed ion focusing, section III (5-3), section IV (5-4) and section V (5-5) can be used in imprisoning by section II (5-2)
Ion, section V (5-5) are final focusing ions region and the outlet with ion.
The ejector principle of liquid drop ejector: jet port (2-7) is parallel with liquid storage tank (2-4) liquid level plane under original state；
After opening driver I (2-5) and driver II (2-6), driver is vibrated with certain frequency, with certain period to liquid storage tank
On the outside of (2-4) and inside moves back and forth, and during driver is to liquid storage tank (2-4) movement outside, liquid storage tank (2-4) is being driven
Volume enlargement under the action of dynamic device, liquid level bending into liquid storage tank (2-4) at jet port (2-7), liquid level the degree of bending with
The expansion of liquid storage tank (2-4) volume and constantly increase；During driver is to liquid storage tank (2-4) medial motion, liquid storage tank
(2-4) volume under the action of driver reduces, and curved liquid level receives the active force of liquid in liquid storage tank (2-4), liquid storage
Pond (2-4) is during volume continues reduction under the action of driver, curved liquid level center will form one it is superfine
Liquid jet；In next vibration period of driver, driver is to liquid storage tank (2-4) movement outside, liquid storage tank (2-4)
Volume starts to expand, and most of liquid in the liquid jet for having gone out jet port (2-7) plane is retracted liquid storage tank (2-
4) in, the small amount of liquids at the tip of the liquid jet will form a very small drop, so that drop goes out liquid storage tank
(2-4)。
A kind of the step of free radical photoproduct test method, is as follows:
Helium is passed through drift chamber II (3-3) by one, and nitrogen is passed through cushion chamber (3-4), and typical flow value is 80SCCM；
Two, control mass flow controller (2-1), testing sample solution are injected liquid storage tank (2-4), flow velocity representative value is
0.02 to 0.2 ml/min；
Three, are separately turned on driver I (2-5) and driver II (2-6), operating mode one, driver I (2-5) and driving
The vibration frequency of device II (2-6) is consistent, and representative value is 0.8 to 1.5kHz；Operating mode two, driver I (2-5) and driver II
The vibration frequency of (2-6) is inconsistent, and the representative value of driver I (2-5) is 0.7 to 1.0kHz, the representative value of driver II (2-6)
It is 1.3 to 1.6kHz；
The drop that four, liquid drop ejectors (2) eject enters vacuum chamber (3), and the shape under the action of ionization device
At ion packet, ion beam current is then formed under the action of vacuum pump group III (12), ion beam current passes through ion bunch device I (4)
It reaches ion bunch device II (5)；
Five, are adjusted to be applied to respectively and are extracted grid (5-6), imprison grid (5-7) and enter the potential on grid (5-8),
So that a part of ion in ion beam current is trapped in the section IV (5-4) of ion bunch device II (5)；
The laser of six, lasers (1) transmitting is injected section IV (5-4) and is irradiated on ion, and light reaction occurs and generates light
Product；
Seven, are adjusted to be applied to respectively and are extracted grid (5-6), imprison grid (5-7) and enter the potential on grid (5-8),
So that the charged particle in photoproduct is projected from the section V (5-5) of ion bunch device II (5), and pass sequentially through ion bunch device III
(6), detector (9) are eventually entered into after ion bunch device IV (7) and quadrupole rod (8)；
Eight, analyze the data of detector (9) acquisition, obtain the relevant information of the light reaction product of free radical.
The present invention generates using the method for liquid resonant and ejects drop, and the direction of vibration and drop of driver spray
Direction it is vertical, be capable of forming the lesser drop of size, be suitable for compared with multiple types free radical sample, secondly, cushion chamber can be reduced
The loss of ion beam current in the vacuum chamber guarantees the quality of detector acquisition signal, furthermore, the ion bunch body of special designing
Product is small, and can reduce the pumping speed of vacuum pump group.
Claims (1)
1. a kind of free radical photoproduct test method, free radical photoproduct test device mainly includes laser (1), drop injection
Device (2), vacuum chamber (3), ion bunch device I (4), ion bunch device II (5), ion bunch device III (6), ion bunch device IV
(7), quadrupole rod (8), detector (9), vacuum pump group I (10), vacuum pump group II (11), vacuum pump group III (12) and ionization dress
Set, xyz is three-dimensional coordinate system, and the vacuum chamber (3) has starting point and end, in the vacuum chamber (3), from starting point to
End successively has sample cavity (3-1), drift chamber I (3-2), drift chamber II (3-3), cushion chamber (3-4) and collision chamber (3-5),
The sample cavity (3-1), cushion chamber (3-4) and collision chamber (3-5) are connected separately with vacuum pump group III (12), vacuum pump group II
(11) and vacuum pump group I (10)；The ion bunch device I (4), ion bunch device II (5), ion bunch device III (6), ion
Beam buncher IV (7) and quadrupole rod (8) are respectively positioned in the vacuum chamber (3), ion bunch device I (4) be connected to sample cavity (3-1) and
Between drift chamber I (3-2), ion bunch device II (5) is connected between drift chamber I (3-2) and drift chamber II (3-3), and ion is poly-
Beam device III (6) is connected between drift chamber II (3-3) and cushion chamber (3-4), and ion bunch device IV (7) is connected to cushion chamber (3-
4) between collision chamber (3-5), quadrupole rod (8) is located in collision chamber (3-5)；The liquid drop ejector (2) is connected to sample cavity
(3-1), ionization device is equipped in the sample cavity (3-1), and sample cavity (3-1) side cavity wall has aperture, liquid drop ejector
(2) drop ejected can enter sample cavity (3-1) by the aperture and formed under the action of the ionization device from
Attached bag, then forms ion beam current under the action of vacuum pump group III (12), and the sample cavity (3-1) has window, laser
(1) laser emitted can be entered vacuum chamber (3) by the window；Detector (9) connection collision chamber (3-5), collision
The cavity wall of chamber (3-5) has through-hole, and the ion beam current in collision chamber (3-5) can be entered detector (9) by the through-hole；It is slow
Chamber (3-4) is rushed with buffer gas entrance, drift chamber II (3-3) has drift carrier gas inlet；Ion bunch device I (4), ion are poly-
Beam device III (6) and ion bunch device IV (7) is made of 20 annular electrodes with a thickness of 0.4 millimeter respectively, adjacent annular
Electrode gap is 0.5 millimeter, and 20 annular electrode internal diameters are linearly to reduce from 45 millimeters to two along z positive direction
Millimeter, 100 kilo-ohms of resistance is in series between each annular electrode respectively；Liquid drop ejector (2) mainly includes mass flow control
Device (2-1), inlet tube (2-2), cavity (2-3), liquid storage tank (2-4), driver I (2-5), driver II (2-6) and injection processed
Mouth (2-7), the cavity (2-3) are cylinder, have the liquid storage tank (2-4) and jet port (2-7), institute in cavity (2-3)
Liquid storage tank (2-4) is stated as cylinder, the upper bottom surface and bottom surface of liquid storage tank (2-4) are connected separately with driver I (2-5) and driving
Device II (2-6), when driver I (2-5) and driver II (2-6) works, the volume of the liquid storage tank (1-4) can generate small
Variation, the pore diameter range of the jet port (2-7) are 40 to 400 microns, liquid storage tank (2-4) the volume range be four to
Eight milliliters, the outlet end of mass flow controller (2-1) is connected with by inlet tube (2-2) connection liquid storage tank (2-4), arrival end
Sample solution fluid reservoir；There is the annular electrode for the different pore size being arranged successively along z positive direction, institute in ion bunch device II (5)
Annular electrode is stated with a thickness of being divided into 0.5 millimeter between 0.4 millimeter and adjacent annular electrode, ion bunch device II (5) successively has
There are five sections, is a section I (5-1), section II (5-2), section III (5-3), section IV (5-4) and section V (5-5) respectively；Section I (5-1) is by seven
Internal diameter is 50 millimeters of annular electrode composition, and section II (5-2) is made of eight annular electrodes, eight annular electrodes it is interior
Diameter respectively is 45 millimeters, 40 millimeters, 35 millimeters, 33 millimeters, 30 millimeters, 27 millimeters, 24 millimeters and 21 millis along z positive direction
Rice, section III (5-3) are made of three annular electrodes, and the internal diameter of three annular electrodes respectively is 28 millis along z positive direction
Rice, 33 millimeters and 38 millimeters, section IV (5-4) is made of the annular electrode that five internal diameters are 50 millimeters, and section V (5-5) is by six
Annular electrode composition, the internal diameter of six annular electrodes respectively are 46 millimeters, 42 millimeters, 38 millimeters, 34 along z positive direction
Millimeter, 30 millimeters and 26 millimeters, have in ion bunch device II (5) extract grid (5-6), imprison grid (5-7), into grid
(5-8) and jet disturbance device (5-9), into grid (5-8), imprison grid (5-7) and extraction grid (5-6) along z positive direction according to
Secondary to be located in section IV (5-4), jet disturbance device (5-9) is located in section I (5-1)；Section I (5-1) can receive oneself of rapid divergence
By ion beam current, section II (5-2) can be by ion focusing, the space energy of section III (5-3), section IV (5-4) and section V (5-5) composition
It is enough in trapped ion, section V (5-5) is final focusing ions region and the outlet with ion,
It is characterized in that: a kind of the step of free radical photoproduct test method, is as follows:
Helium is passed through drift chamber II (3-3) by one, and nitrogen is passed through cushion chamber (3-4), and typical flow value is 80SCCM；
Two, control mass flow controller (2-1), and testing sample solution is injected liquid storage tank (2-4), and flow velocity representative value is 0.02
To 0.2 ml/min；
Three, are separately turned on driver I (2-5) and driver II (2-6), operating mode one, driver I (2-5) and driver II
The vibration frequency of (2-6) is consistent, and representative value is 0.8 to 1.5kHz；Operating mode two, driver I (2-5) and driver II (2-
6) vibration frequency is inconsistent, and the representative value of driver I (2-5) is 0.7 to 1.0kHz, and the representative value of driver II (2-6) is
1.3 to 1.6kHz；
The drop that four, liquid drop ejectors (2) eject enters vacuum chamber (3), and formed under the action of the ionization device from
Attached bag, then forms ion beam current under the action of vacuum pump group III (12), and ion beam current is reached by ion bunch device I (4)
Ion bunch device II (5)；
Five, are adjusted to be applied to respectively and are extracted grid (5-6), imprison grid (5-7) and enter the potential on grid (5-8), so that
A part of ion in ion beam current is trapped in the section IV (5-4) of ion bunch device II (5)；
The laser of six, lasers (1) transmitting is injected section IV (5-4) and is irradiated on ion, and light reaction occurs and generates photoproduct；
Seven, are adjusted to be applied to respectively and are extracted grid (5-6), imprison grid (5-7) and enter the potential on grid (5-8), so that
Charged particle in photoproduct is projected from the section V (5-5) of ion bunch device II (5), and pass sequentially through ion bunch device III (6),
Detector (9) are eventually entered into after ion bunch device IV (7) and quadrupole rod (8)；
Eight, analyze the data of detector (9) acquisition, obtain the relevant information of the light reaction product of free radical.
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