CN109212113B - Ion trapping gas molecule separation method and device - Google Patents
Ion trapping gas molecule separation method and device Download PDFInfo
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention provides an ion trapping gas molecular separation device, which comprises a device body, wherein the device body comprises a sample gas inlet pipe, an ionization source, an ionization chamber, an ion trapping and neutralizing electrode, an ion repulsive electrode, a gas washing inlet pipe and a gas outlet pipe; the invention also relates to a method for separating the molecules of the ion trapping gas. The invention combines ultraviolet ionization, proton affinity ionization reaction, electric field auxiliary ion trapping (field ion trapping) and ion neutralization reduction technology to realize rapid separation of sample gas molecules; the separation time interval can be adjusted in a linkage way according to the analysis processing speed of a subsequent detection instrument; meanwhile, only small electric power is consumed to ionize and assist ion trapping in the separation treatment process, large-range temperature control is not needed, high-pressure carrier gas is not needed, and the whole device is small in size, light in weight and free of consumable materials. The invention has smart conception, flexible control of separation effect and is convenient for gas detection popularization and application.
Description
Technical Field
The invention relates to the field of pretreatment of complex multi-component gas molecule detection samples, in particular to an ion trapping gas molecule separation method.
Background
The detection of complex multi-component gas molecules is an important part of the gas refinement detection, when a gas sample is analyzed and detected by adopting mass spectrometry or ion mobility spectrometry, samples with less gas molecular types can be directly subjected to sample injection detection, and when the sample to be detected is complex multi-component gas, partial sample molecules can interfere with each other to cause detection omission or false detection, so that the detection of the complex multi-component gas molecules needs to be subjected to gas separation sample pretreatment, such as gas chromatography combined with gas chromatography to separate sample molecules before sample injection.
Gas chromatography is the most widely used sample molecular separation processing technology in mass spectrometry detection at present, a chromatographic column of a separation device uses gas as a mobile phase and solid or liquid as a stationary phase, and the separation of a mixture is realized by utilizing the difference of the boiling point, the polarity and the adsorption property of substances. The gas chromatography has the defects that the temperature control heating is needed for the chromatographic column in the separation process, and meanwhile, high-pressure pure carrier gas is needed for pushing the mobile phase, so that the gas chromatography device or equipment mostly adopts a temperature control box for heating the chromatographic column, and is provided with a high-pressure helium gas and argon gas steel cylinder for pushing the mobile phase, so that the whole device or equipment is large in size, heavy in weight, difficult to portable move and unfavorable for on-site rapid detection, and meanwhile, the heavy carrier gas steel cylinder is replaced along with the consumption of the high-pressure carrier gas, so that inconvenience is brought to the use. Furthermore, the retention time of a chromatographic column is on the order of minutes, and it is typically from a few minutes to tens of minutes to isolate one sample, which is not adequate for detection speeds requiring on-line monitoring on the order of seconds or faster.
In summary, the gas chromatographic device or equipment commonly used for separating and processing the complex multi-component gas sample of the mass spectrum or the ion mobility spectrometry has the defects of large volume, heavy weight, requirement for high-pressure steel bottle carrier gas, low separation processing speed and the like, and along with the development of the portable microminiature mass spectrometer and the ion mobility spectrometer, the gas chromatograph is difficult to meet the application matching requirements of the mass spectrum and the ion mobility spectrometry in the field of portable field fast detection and the field of high-speed on-line detection of second-level frequency. In view of the above, there is a need to develop a new gas molecular separation method for solving the above problems.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method and a device for separating gas molecules trapped by ions, which are combined with ultraviolet light ionization, proton affinity ionization reaction, electric field assisted ion trapping (field ion trapping) and ion neutralization reduction technology to realize rapid separation of gas molecules of a sample; meanwhile, only small electric power is consumed to ionize and assist ion trapping in the separation treatment process, large-range temperature control is not needed, high-pressure carrier gas is not needed, and the whole device is small in size, light in weight and free of consumable materials.
To achieve the above objects and other advantages and in accordance with the purpose of the invention, there is provided an ion trap gas molecular separation method comprising the steps of:
air is introduced, a trapping electric field and an ionization source are started, the excitation power of the ionization source is constant, gas washing is closed, sample injection is started, and sample gas is injected into an ionization reaction cavity; at this time, the number of photons for ionization injected in a unit time of the ionization source is constant, and the number of photons is equal to or greater than the number of molecules of the sample gas; wherein the sample gas molecules comprise at least two substances, and the proton affinity energy of each sample gas molecule is different;
ionization, closing sample introduction, opening gas washing, wherein all sample gas molecules with ionization energy under photon capacity are ionized into positive ions, the positive ions are pushed to an ion trapping and neutralizing electrode under the action of the electric field force of an ion repulsive electrode, neutral molecules are obtained by neutralization, the molecules are separated from the ion trapping and neutralizing electrode and are ionized into positive ions again, the sample gas molecules are always converted between ion states and molecular states and are restrained in an ionization source action area near the ion trapping and neutralizing electrode by a trapping electric field, and then the sample gas cannot pass through the ion repulsive electrode;
the trapping and separation reduce the photon quantity for ionization in unit time, and sample gas molecules with relatively low proton affinity are not ionized again to become neutral molecules, and are carried by the washing gas to pass through an ion repulsive electrode and output; sample gas molecules with relatively high proton affinity cannot pass through the ion-repeller electrode because they are re-ionized.
Preferably, the separation is carried out sequentially, the separation to be trapped is completed, the time is delayed, the detection is completed by the instrument to be detected, and the next trapping and separation are skipped until the sample gas is separated one by one in the sequence from low proton affinity to high.
Preferably, the ionization source is an ultraviolet ionization source.
The ion trapping gas molecular separation device comprises a device body, wherein the device body comprises a sample gas inlet pipe, an ionization source, an ionization chamber, an ion trapping and neutralizing electrode, an ion repulsive electrode, a gas washing inlet pipe and a gas outlet pipe; wherein,,
the ionization source is used for ionizing sample gas to be detected in the ionization chamber to form positively charged ions; a plurality of adjustable power outputs are arranged in the ionization source;
the ionization chamber is used for providing an ionization reaction chamber for ionization of the sample gas to be detected; the ionization chamber is of a three-way structure, wherein a first end is communicated with the ionization source, a second end is provided with the ion trapping and neutralizing electrode, and a third end is provided with the ion repulsive electrode;
the ion trapping and neutralizing electrode is used for neutralizing the electric quantity of positively charged ions and reducing the positively charged ions into neutral molecules; the ion trapping neutralization electrode is communicated with the sample gas inlet pipe and the gas washing inlet pipe;
the ion repulsion electrode is used for providing a trapping electric field for pushing positively charged ions to move towards the ion trapping neutralization electrode; the ion repulsive electrode side is communicated with the air outlet pipe;
the sample gas to be detected enters the ionization chamber through the sample gas inlet pipe and is fully ionized to obtain positively charged ions, positive ions are pushed to the ion trapping and neutralizing electrode and then neutralized to obtain neutral molecules under the action of the electric field force of the trapping electric field of the ion trapping and neutralizing electrode, the molecules are separated from the ion trapping and neutralizing electrode and are ionized to positive ions again, the sample gas molecules are always converted between an ionic state and a molecular state and are restrained in the ionization source action area near the ion trapping and neutralizing electrode by the trapping electric field, and the sample gas cannot pass through the ion trapping electrode again; the photon number for ionization in unit time is reduced, and sample gas molecules with relatively low proton affinity are not ionized again to become neutral molecules, and are carried by the gas washer to pass through the ion repulsion electrode and output; sample gas molecules with relatively high proton affinity cannot pass through the ion-repulsive electrode because they are re-ionized; the gas washing enters the ionization chamber through the gas washing inlet pipe, and carries sample gas molecules with relatively low proton affinity through the hollow structure of the ion repulsion electrode and is output from the gas outlet pipe.
Preferably, the ionization source is an ultraviolet ionization source, and the ultraviolet ionization source comprises an ultraviolet PID lamp, a spiral pipe driving coil and a radio frequency driving power supply; the spiral tube driving coil is wound on the ultraviolet PID lamp body; the two poles of the spiral tube driving coil are connected with the radio frequency driving power supply; and a light-transmitting window of the ultraviolet PID lamp is connected with the ionization chamber.
Preferably, the ion-repelling electrode side is communicated with the air outlet pipe through the air outlet collector; the air outlet collector comprises a funnel-shaped collecting inner surface and a duct; the pore canal is communicated with the converging inner surface and the air outlet pipe.
Preferably, the ionization chamber is of a hollow tee structure, and one end of the inner surface of the ionization chamber is provided with a first step and a second step; the first step geometry is greater than the second step geometry; the first step is used for fixing the ion trapping neutralization electrode; the second step and the ion trapping neutralization electrode form an air guide groove and an air gathering port; a third step is arranged at the other end of the inner surface of the ionization chamber; the third step is used for fixing the ion-repulsive electrode.
Preferably, a fourth step is further arranged on the end face of the inner surface of the ionization chamber at the same end of the third step; the fourth step is used for fixing the air outlet collector.
Preferably, the ion trapping and neutralizing electrode comprises an air inlet diversion trench, an ion neutralizing and trapping plate, a neutralizing electrode lead, a sample air inlet and a gas washing air inlet; connecting the ion neutralization trap plate with a power supply through the neutralization electrode lead; the ion neutralization trapping plate is used for neutralizing the electric quantity of positively charged ions; the sample air inlet and the gas washing air inlet are respectively communicated with the air inlet diversion trench; the sample air inlet hole is communicated with the sample air inlet pipe; the gas washing inlet hole is communicated with the gas washing inlet pipe.
Preferably, the ion-repulsive electrode includes an electrode sheet, a repulsive electrode lead; connecting the electrode plate with a power supply through the repulsive electrode lead; and the electrode plate is provided with a hollowed-out channel.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides an ion trapping gas molecular separation device, which comprises a device body, wherein the device body comprises a sample gas inlet pipe, an ionization source, an ionization chamber, an ion trapping neutralization electrode, an ion repulsion electrode, a gas washing inlet pipe and a gas outlet pipe; the invention also relates to a method for separating the molecules of the ion trapping gas. The invention combines ultraviolet ionization, proton affinity ionization reaction, electric field auxiliary ion trapping (field ion trapping) and ion neutralization reduction technology to realize rapid separation of sample gas molecules; the separation time interval can be adjusted in a linkage way according to the analysis processing speed of a subsequent detection instrument; meanwhile, only small electric power is consumed to ionize and assist ion trapping in the separation treatment process, large-range temperature control is not needed, high-pressure carrier gas is not needed, and the whole device is small in size, light in weight and free of consumable materials. The invention has smart conception, flexible control of separation effect and is convenient for gas detection popularization and application.
Drawings
FIG. 1 is a schematic flow chart of a method for separating molecules of an ion trapping gas according to the present invention;
FIG. 2 is a schematic view of a three-dimensional cross-sectional structure of an ion trap gas molecular separation device according to the present invention;
FIG. 3 is a schematic view of the overall structure of an ionization source of an ion trap gas molecular separation apparatus according to the present invention;
FIG. 4 is a schematic view of a three-dimensional cross-sectional structure of an ionization chamber of an ion trap gas molecular separation device according to the present invention;
FIG. 5 is a schematic view of a three-dimensional cross-sectional structure of an ion trap neutralization electrode of an ion trap gas molecular separation device according to the present invention;
FIG. 6 is a schematic view showing the overall structure of an ion-repulsive electrode of an ion-trapping gas molecular separation device according to the present invention;
fig. 7 is a schematic structural diagram of an air outlet collector of an ion trapping gas molecular separation device according to the present invention.
Reference numerals in the drawings:
the device comprises a device body 100, a sample gas inlet pipe 10, an ionization source 20, an ionization chamber 30, an ion trapping and neutralizing electrode 40, an ion repulsion electrode 50, a gas washing inlet pipe 70, an outlet pipe 80, a driving power supply 90, an ultraviolet PID lamp 201, a spiral tube driving coil 202, a radio frequency driving power supply 203, a light transmission window 204, an upper step 301, a first step 302, a second step 303, a third step 304, a fourth step 305, a gas inlet guide groove 401, a collision plate 402, an ion trapping and neutralizing trap plate 403, a neutralizing electrode lead 404, a sample inlet hole 405, a gas washing inlet hole 406, an electrode plate 501, a repulsion electrode lead 502, a hollowed-out channel 503, a barrel body 601, a flat barrel bottom 602, a converging inner surface 603, a barrel opening 604 and a hole 605.
Detailed Description
The foregoing and other objects, features, aspects and advantages of the present invention will become more apparent to those skilled in the art from the following detailed description, which, taken in conjunction with the annexed drawings, discloses a device for practicing the invention. In the drawings, the shape and size may be exaggerated for clarity, and the same reference numerals will be used throughout the drawings to designate the same or similar components. In the following description, terms such as center, thickness, height, length, front, back, rear, left, right, top, bottom, upper, lower, etc. are based on the orientation or positional relationship shown in the drawings. In particular, "height" corresponds to the top-to-bottom dimension, "width" corresponds to the left-to-right dimension, and "depth" corresponds to the front-to-back dimension. These relative terms are for convenience of description and are not generally intended to require a particular orientation. Terms (e.g., "connected" and "attached") referring to an attachment, coupling, etc., refer to a relationship wherein these structures are directly or indirectly secured or attached to one another through intervening structures, as well as both movable or rigid attachments or relationships, unless expressly described otherwise.
Example 1
Referring to fig. 1, a method for separating molecules of an ion trapping gas includes the steps of:
s1, air inflow, starting a trapping electric field and an ionization source, enabling excitation power of the ionization source to be constant, closing gas washing, starting sample injection, and injecting sample gas into an ionization reaction cavity; at this time, the number of photons for ionization injected in a unit time of the ionization source is constant, and the number of photons is equal to or greater than the number of molecules of the sample gas; wherein the sample gas molecules comprise at least two substances, and the proton affinity energy of each sample gas molecule is different; in one embodiment, the high-voltage trapping electric field and the ultraviolet PID lamp are turned on, the excitation power of the ultraviolet PID lamp is modulated to the maximum, the gas washing is turned off, and the sample gas is turned on to inject the sample gas into the ionization reaction chamber.
S2, ionization, closing sample introduction, starting gas washing, wherein all sample gas molecules with ionization energy under photon capacity are ionized into positive ions, under the action of the electric field force of an ion repulsion electrode, the positive ions are pushed to an ion trapping and neutralizing electrode and then neutralized to obtain neutral molecules, the molecules are separated from the ion trapping and neutralizing electrode and are ionized into positive ions again, the sample gas molecules are always converted between an ionic state and a molecular state and are restrained in an ionization source action area near the ion trapping and neutralizing electrode by a trapping electric field, and then the sample gas is ionized again to obtain the sample gas which cannot pass through the ion repulsion electrode; in one embodiment, after the sample gas fills the ionization reaction chamber, the sample gas is closed to stop sample injection, and then the gas washing is started, so that clean gas washing continuously flows through the ionization reaction chamber, passes through the ion repulsion electrode and flows from the gas outlet collector to the matched detection instrument; at this time, the ultraviolet PID lamp rapidly injects enough high-energy ultraviolet photons into the ionization reaction chamber with the maximum driving excitation power, the sample molecules with ionization energy under the photon capacity are all ionized into positive ions, the positive ions are trapped on the grounded neutralization electrode plate under the pushing of the high-voltage electric field, electrons are obtained on the electrode plate and then are neutralized and reduced into molecules, then the positive ions are ionized again after leaving the neutralization electrode plate and are transported to the trapping neutralization electrode plate again by the electric field force, so that the sample gas molecules are always converted between an ionic state and a molecular state and are confined in an ultraviolet irradiation area near the ion trapping neutralization electrode plate by the high-voltage electric field, and then the sample gas cannot pass through the ion repulsive electrode after being ionized again.
S3, trapping and separating, namely reducing the photon number for ionization in unit time, wherein sample gas molecules with relatively low proton affinity are not ionized again to become neutral molecules, and are carried by the gas washing through an ion repulsion electrode and output; sample gas molecules with relatively high proton affinity cannot pass through the ion-repeller electrode because they are re-ionized. In one embodiment, the drive excitation power of the ultraviolet PID lamp is reduced by one step, i.e., turned down to the next constant power. After sample material ions are obtained from a collecting and neutralizing electrode plate and are neutralized into neutral molecules, as the number of injected high-energy ultraviolet photons in unit time is reduced, the sample material with relatively lowest proton affinity is not ionized again after photoionization and proton affinity ionization reaction to obtain free neutral molecules, and then the free neutral molecules are collected in an air outlet collector by a clean air washing carrying fan-shaped hollow channel passing through an ion repulsive electrode and then are sent to a matched detection instrument.
S4, sequentially separating, waiting for the trapping and separating to be completed, delaying for waiting for the detection of the detecting instrument to be completed, and jumping to the next trapping and separating until the sample gas is separated one by one according to the sequence from low proton affinity to high proton affinity. In one embodiment, after the sample molecules recovered from the ionization reaction chamber are taken away by the gas washing, delaying for a period of time and reserving the sample molecules for a matched detection instrument to detect and analyze the sample molecules separated out in the previous time; and (3) sequentially repeating the steps of S2 and S3 after the time delay is finished until sample molecules in the ionization reaction chamber are separated one by one according to the sequence from low to high of proton affinity.
Example 2
An ion trapping gas molecular separation device comprises a device body 100, wherein the device body 100 comprises a sample gas inlet pipe 10, an ionization source 20, an ionization chamber 30, an ion trapping neutralization electrode 40, an ion repulsion electrode 50, a gas washing inlet pipe 70 and a gas outlet pipe 80; wherein,,
the ionization source 20 is used for ionizing the sample gas to be detected in the ionization chamber 30 to form positively charged ions; a plurality of adjustable power outputs are arranged in the ionization source 20;
the ionization chamber 30 is used for providing an ionization reaction chamber 306 for ionization of the sample gas to be detected; the ionization chamber 30 has a three-way structure, wherein a first end is communicated with the ionization source 20, a second end is provided with the ion trapping neutralization electrode 40, and a third end is provided with the ion repulsion electrode 50;
the ion trap neutralization electrode 40 is used for neutralizing the electric quantity of positively charged ions and reducing the electric quantity into neutral molecules; the ion trapping neutralization electrode 40 communicates the sample gas inlet pipe 10 with the purge gas inlet pipe 70;
the ion-repeller electrode 50 is used to provide an ion-repeller separation electric field that pushes positively charged ions toward the ion-trap neutralization electrode 40; the ion repulsive electrode 50 side is communicated with the air outlet pipe 80;
after the sample gas to be detected enters the ionization chamber 30 through the sample gas inlet pipe 10 and is fully ionized, positively charged ions are obtained, positive ions are pushed to the ion trapping and neutralizing electrode 40 and neutralized under the action of the electric field force of the trapping electric field of the ion trapping and neutralizing electrode 50 to obtain neutral molecules, the molecules are separated from the ion trapping and neutralizing electrode 40 and are ionized again to positive ions, the sample gas molecules are always converted between an ionic state and a molecular state and are restrained in the action area of the ionization source 20 near the ion trapping and neutralizing electrode 40 by the trapping electric field, and then the sample gas cannot pass through the ion trapping electrode; the photon number for ionization in unit time is reduced, and sample gas molecules with relatively low proton affinity are not ionized again to become neutral molecules, and are carried by the gas washer to pass through the ion repulsion electrode and output; sample gas molecules with relatively high proton affinity cannot pass through the ion-repulsive electrode because they are re-ionized; purge gas enters the ionization chamber 30 through the purge gas inlet pipe 70, and the purge gas carries sample gas molecules with relatively low proton affinity through the hollow structure of the ion-repelling electrode 50 and is output from the gas outlet pipe 80.
Proton affinity refers to the energy released during the process of protonating the positive charge of molecules in molecular ion reaction, and reflects the capability of the molecules to abstract positive charge, and according to the data of the national institute of standards and technology National Institute of Standards and Technology, NIST chemical database (SRD 69) for proton affinity testing and recording, almost two thousand molecules can abstract positive charge from the positive ions of substances with lower proton affinity than that of the molecules, the vast majority of gas molecules under normal pressure are covered. In this embodiment, the separation treatment of the complex multicomponent gas molecules is based on the competitive ionization reaction principle, and by utilizing the characteristic that the substance molecules with high proton affinity are easy to exchange charges with the substance ions with low proton affinity to form ion molecule inversion, the sample gas molecules are ionized into positive ions in turn from high proton affinity to low proton affinity with a certain optical power, the ion trapping is restrained near the neutralizing electrode by using the electric field force, so that the ionized molecules cannot escape, and the neutral molecules without charge can be taken out of the ionization chamber by gas washing; gradually reducing the optical power, wherein when the optical power is reduced once, along with the reduction of the high-energy ultraviolet photon injection quantity in unit time, a part of sample substance ions with relatively low proton affinity can not be converted into ion states again after being neutralized and reduced to neutral molecules on the surface of a trapping and neutralizing electrode, and the neutralized and reduced neutral sample molecules are carried out of an ionization chamber by a gas washing air flow and are sent to a matched detection instrument; and (3) reducing the optical power again after the detection of the instrument is finished, repeating the process, and separating the gas molecules of the complex multi-component sample from one to one according to the sequence from low to high of proton affinity. In brief summary, the proton affinity ionization reaction is utilized to convert the material molecules with relatively high proton affinity into an ionic state, the ions are trapped by a high-voltage electric field to prevent the ions from escaping from an electric field region, and the material molecules with relatively low proton affinity are separated in advance in a neutral molecular state by freely passing through the electric field region.
Example 3
As shown in fig. 3, the ionizing ionization source 20 is an ultraviolet ionizing ionization source, and the ultraviolet ionizing ionization source includes an ultraviolet PID lamp 201, a spiral tube driving coil 202, and a radio frequency driving power supply 203; the spiral tube driving coil 202 is wound on the lamp body of the ultraviolet PID lamp 201; the two poles of the spiral tube driving coil 202 are connected with the radio frequency driving power supply 203; the light-transmitting window 204 of the ultraviolet PID lamp 201 is connected to the ionization chamber 30.
In this embodiment, as shown in fig. 3, the ultraviolet PID lamp 201 has a transparent window 204 of magnesium fluoride or lithium fluoride that can transmit high-energy ultraviolet photons, the high-energy ultraviolet photons can exit from the window to the outside of the lamp, and the window end of the ultraviolet PID lamp is connected with the sample inlet guide cover 30.
The ultraviolet light ionization source is a selective ionization source, and uses high-energy ultraviolet light to ionize gaseous molecules. In the embodiment, the PID lamp is an argon lamp, the wavelength of the shortest spectral line is 104.8nm, the energy of the corresponding photon with the highest energy is 11.8eV, gas molecules with ionization energy within 11.8eV can be converted into an ionic state, and carrier gas molecules with higher ionization energy (such as 14.53eV and 13.62eV for the ionization energy of nitrogen and oxygen which are main components of air) are not affected and keep in a neutral molecular state; meanwhile, the energy of the adopted high-energy ultraviolet photons is below 11.8eV, so that the molecular structure is not damaged. In this embodiment, the high energy in the high-energy ultraviolet photon refers to single photon energy. According to Einstein's theory of light quanta, light is composed of a stream of photons, the energy of which is inversely proportional to the wavelength of light, i.e. the shorter the wavelength of light the higher the energy of the corresponding photons, e.g. the photon energy of light with a wavelength of 116.5nm is 10.6eV and the photon energy of light with a wavelength of 50.8nm is 11.8eV. In addition to the energy of a single photon, there is a parameter that the light intensity, i.e. the luminous flux in a unit solid angle, is proportional to the number of photons that directly pass through a unit area in a unit time, i.e. the density distribution of photons in a unit time, and a larger light intensity means a larger number of photons emitted in a unit time.
In the working process, the radio frequency driving power supply 203 generates radio frequency alternating current and supplies the radio frequency alternating current to the spiral tube driving coil 202, the spiral tube driving coil 202 converts the radio frequency alternating current into an induction electromagnetic field to provide excitation energy for the ultraviolet PID lamp 201, the induction electromagnetic field excites thin gas molecules in the lamp to discharge to generate high-energy ultraviolet light, the high-energy ultraviolet light is emitted from the light-transmitting window 204 and irradiates the ionization chamber 30, and although the energy of single photons is determined by characteristic spectral lines of the thin gas filled in the lamp and cannot be regulated in the working process, the luminous intensity of the lamp can be changed through the size of excitation power, namely the quantity of the high-energy ultraviolet photons emitted in unit time can be regulated through the output power of the radio frequency driving power supply 203. When the driving excitation power of the ultraviolet PID lamp 201 is constant, the PID lamp injects high-energy ultraviolet photons into the ionization reaction chamber 306 at a constant speed, and sample molecules which receive the high-energy ultraviolet photons are ionized into positive ions, namely the high-energy ultraviolet photons generate positive ions at a constant speed; when the number of injected high-energy ultraviolet photons in unit time is far more than the number of ionized substance molecules, all the ionized substance molecules can be photoionized; when the number of injected high-energy ultraviolet photons in unit time is reduced, part of sample substance molecules cannot obtain the high-energy ultraviolet photons and are not photoionization, but after the subsequent proton affinity ionization reaction, the substance molecules with high proton affinity can abstract positive charges from substance ions with low proton affinity to generate proton affinity ionization reaction; after proton affinity ionization reaction, the substances with high proton affinity are ionized, and the substances with relatively low proton affinity are in neutral molecular form.
Example 4
As shown in fig. 4, the ionization chamber 30 has a hollow three-way structure, and a first step 302 and a second step 303 are disposed at one end of the inner surface of the ionization chamber 30; the first step 302 geometry is larger than the second step 303 geometry; the first step 302 is used to fix the ion trapping neutralization electrode 40; the second step 303 and the ion trapping neutralization electrode 40 form an air guide groove and an air gathering port; a third step 304 is arranged at the other end of the inner surface of the ionization chamber 30; the third step 304 is used to fix the ion-repeller electrode 50.
In this embodiment, as shown in fig. 4, the upper opening of the ionization chamber 30 is led to the ultraviolet PID lamp 201, a circular upper step 301 is provided around the upper opening for abutting against the end of the light-transmitting window 204 of the ultraviolet PID lamp 201, the high-energy ultraviolet photon light-transmitting window 204 of the PID lamp is attached to the surface of the upper step 301, and the lamp body of the ultraviolet PID lamp 201 is tightly matched with the step wall of the upper step 301. The opening on the left side of the ionization chamber 30 is led to the ion trapping neutralization electrode 40, and two circular steps are arranged on the left side, a first step 302 is used for fixing the ion trapping neutralization electrode 40, and a second step 303 and a groove ring in the middle of the ion trapping neutralization electrode 40 form an air guide groove and an air gathering port for air intake. The right opening of the ionization chamber 30 is open to the ion-repelling electrode 50 and the gas outlet collector 60, and there are two circular steps on the right side, a third step 304 for clamping the ion-repelling electrode 50, and a fourth step 305 for fixing the gas outlet collector 60. The center of the ionization chamber forms a relatively closed cavity, namely an ionization reaction cavity 306, under the surrounding of the light-transmitting window 204 of the upper ultraviolet PID lamp 201, the left ion trapping and neutralizing electrode 40, the right ion repulsive electrode 50 and the inner wall of the ionization chamber in the direction of not being provided with an opening.
Example 5
As shown in fig. 5, the ion capturing neutralization electrode 40 includes an air inlet guide groove 401, an ion neutralization capturing plate 403, a neutralization electrode lead 404, a sample air inlet 405, and a purge air inlet 406; connecting the ion neutralization trap plate 403 to a power supply through the neutralization electrode lead 404; the ion neutralization trap plate 403 is used to neutralize the positively charged ion charge; the sample air inlet 405 and the purge air inlet 406 are respectively communicated with the air inlet diversion trench 401; the sample air inlet hole 405 is communicated with the sample air inlet pipe 10; the purge inlet 406 communicates with the purge inlet conduit 70.
In this embodiment, as shown in fig. 5, the ion trapping neutralization electrode 40 is a circular i-shaped structure made of a corrosion-resistant stainless steel material; an air inlet diversion trench 401 with a circle of trenches at the waist part is used for air inlet diversion, and the air inlet diversion trench 401 is matched with the step wall of the circular step 303 at the left side of the ionization chamber to form a relatively wide air inlet diversion channel; the left circular interference plate 402 is used to be tightly fixed with the left circular first step 302 of the ionization chamber 30; the edge of the ion neutralization trap plate 403 and the step plane of the second step 303 on the left side of the ionization chamber 30 form a circle of relatively narrow air gathering ports; the side wall of the edge of the interference plate 402 is provided with a neutralization electrode lead 404 for connecting with the output power ground of the high-voltage driving power supply 90, and two sample air inlets 405 and gas washing air inlets 406 which are communicated with the air inlet guide groove 401 are arranged near the edge and are respectively used for installing the sample gas inlet pipe 10 and the gas washing inlet pipe 70. The gas washing is in a closed state in the sample injection process, the sample gas flows along a relatively wide groove after entering the gas inlet diversion trench 401, and is uniformly injected into the ionization reaction cavity 306 from the gas gathering port outside the ion neutralization and trapping plate 403 edge after filling the groove; during separation, the sample gas is closed, the gas washing is started, clean gas washing is firstly filled in the gas inlet diversion trench 401, overflows from the gas collecting port and flows into the ionization reaction cavity 306, and neutral sample molecules which are carried by the ionization reaction cavity 306 from left to right and are not ionized pass through the ion repulsion electrode 50 and then flow away from the middle round hole of the gas outlet collector 60. The ion trapping neutralization electrode 40 is always grounded, and the ion neutralization trapping plate 403 on the right side thereof forms a pair of plate electrodes with the pole pieces of the ion repulsive electrode 50.
Example 6
As shown in fig. 6, the ion-repulsive electrode 50 includes an electrode sheet 501, a repulsive electrode lead 502; connecting the electrode pad 501 to a power source through the repulsive electrode lead 502; the electrode plate 501 is provided with a hollowed-out channel 503.
In this embodiment, as shown in fig. 6, a plurality of fan-shaped hollow channels 503 are formed on the circular electrode plate 501 for air flow to pass through, and redundant sample gas during sample injection and washing gas carrying part of sample substance molecules during separation flow out of the fan-shaped hollow channels 503 into an air outlet collector; the electrode plate 501 and the ion trapping neutralization ion neutralization trapping plate 403 form a pair of parallel electrodes, the electrode plate is connected with the output positive high voltage of the high-voltage driving power supply 90 by the repulsive electrode lead 502, when the positive high voltage is started, a trapping electric field formed between the two parallel electrodes passes through the ionization reaction cavity 306 of the ionization chamber, ions formed by photoionization and proton affinity ionization reaction are attracted to the ion neutralization trapping plate 403 under the pushing of electric field force, the ions are neutralized into neutral substance molecules after obtaining electrons on a grounded conductive plate, then the neutral substance molecules are carried into a high-energy ultraviolet light area by a gas washing airflow and are again photo-ionized or subjected to proton affinity ionization reaction to be converted into an ionic state again, then the ionic substance is trapped by the grounded middle electrode plate under the action of electric field force, the cyclic process of ionization and trapping neutralization is repeated repeatedly, and the gaseous substances are limited in the ultraviolet light area near the trapping middle electrode plate in the cyclic process, and cannot reach the ion repulsive electrode to leave the ionization chamber all the time; only when the output power of the rf driving power supply 203 is reduced so that the number of high-energy uv photons emitted by the uv PID lamp 201 in a unit time is reduced, the corresponding number of substance molecules with relatively lowest proton affinity cannot be obtained after leaving the trapping and neutralizing electrode plate, and the photons are not photo-ionized or the ions thereof are reduced into molecules by the positive charges of other substance molecules with high proton affinity, i.e. the substances with relatively low proton affinity are still in a neutral molecular state after leaving the trapping and neutralizing electrode plate due to the reduction of the number of injected photons in a unit time, and then the substance molecules can be carried by the purge gas to reach the gas outlet collector 60 through the fan-shaped hollowed-out channels 503 of the ion-repulsive electrode, so that the opportunity of leaving the ionization chamber is finally obtained.
Note that, the power source connecting the ion trapping neutralization electrode 40 and the ion repulsive electrode 50 may be the same power source, for example, the driving power source 90; the power supply can also be two independent power supplies, and the protection scope of the invention is not limited by the selection of the power supplies.
Example 7
As shown in fig. 7, the ion trapping gas molecular separation device further includes a gas outlet collector 60, and the ion repulsive electrode 50 side and the gas outlet pipe 80 are communicated by the gas outlet collector 60; the outlet collector 60 comprises a funnel-shaped collecting inner surface 603 and a duct 605; the channel 605 communicates the converging inner surface 603 with the outlet tube 80.
In this embodiment, as shown in fig. 7, the air outlet collector 60 is made of an insulating material and is composed of a left circular tub body 601 and a right circular flat tub bottom 602 having a larger area than the tub body. The inner space of the tub 601 is cone-shaped, i.e., converging inner surface 603; the bung hole 604 abuts against the ion-repelling electrode 50, the ion-repelling electrode 50 is pressed against the right third step surface 304 of the ionization chamber 30, and the gas from the fan-shaped hollow hole 503 of the ion-repelling electrode 50 flows into the converging inner surface 603 from the bung hole. The center of the flat barrel bottom 602 is provided with a hole 605 for fixing the air outlet pipe 80, the left side of the hole 605 is communicated with the leak of the converging inner surface 603, and the air collected by the converging inner surface 603 is sent to a matched detection instrument through the air outlet pipe 80.
The invention provides an ion trapping gas molecular separation device, which comprises a device body, wherein the device body comprises a sample gas inlet pipe, an ionization source, an ionization chamber, an ion trapping neutralization electrode, an ion repulsion electrode, a gas washing inlet pipe and a gas outlet pipe; the invention also relates to a method for separating the molecules of the ion trapping gas. The invention combines ultraviolet ionization, proton affinity ionization reaction, electric field auxiliary ion trapping (field ion trapping) and ion neutralization reduction technology to realize rapid separation of sample gas molecules; the separation time interval can be adjusted in a linkage way according to the analysis processing speed of a subsequent detection instrument; meanwhile, only small electric power is consumed to ionize and assist ion trapping in the separation treatment process, large-range temperature control is not needed, high-pressure carrier gas is not needed, and the whole device is small in size, light in weight and free of consumable materials. The invention has smart conception, flexible control of separation effect and is convenient for gas detection popularization and application.
The number of equipment and the scale of processing described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be readily apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (6)
1. An ion trap gas molecule separation device comprising a device body (100), characterized in that: the device body (100) comprises a sample gas inlet pipe (10), an ionization source (20), an ionization chamber (30), an ion trapping and neutralizing electrode (40), an ion repulsive electrode (50), a gas washing inlet pipe (70) and a gas outlet pipe (80); wherein,,
the ionization source (20) is used for ionizing sample gas to be detected in the ionization chamber (30) to form positively charged ions; a plurality of adjustable power outputs are arranged in the ionization source (20);
-said ionization chamber (30) is adapted to provide an ionization reaction chamber (306) for ionization of said sample gas to be detected; the ionization chamber (30) is of a three-way structure, wherein a first end is communicated with the ionization source (20), the second end is provided with the ion trapping and neutralizing electrode (40), and a third end is provided with the ion repulsive electrode (50);
the ion trapping neutralization electrode (40) is used for neutralizing the electric quantity of positively charged ions and reducing the positively charged ions into neutral molecules; the ion trapping neutralization electrode (40) is communicated with the sample gas inlet pipe (10) and the gas washing inlet pipe (70);
the ion-repeller electrode (50) is configured to provide a trapping electric field that pushes positively charged ions toward the ion trapping neutralization electrode (40); the ion repulsive electrode (50) side is communicated with the air outlet pipe (80);
the ion repulsion electrode (50) side is communicated with the air outlet pipe (80) through the air outlet collector (60); the air outlet collector (60) comprises a funnel-shaped collecting inner surface (603) and a pore canal (605); the pore canal (605) is communicated with the converging inner surface (603) and the air outlet pipe (80);
the ionization chamber (30) is of a hollow tee structure, and one end of the inner surface of the ionization chamber (30) is provided with a first step (302) and a second step (303); -the first step (302) geometry is larger than the second step (303) geometry; the first step (302) is used for fixing the ion trapping neutralization electrode (40); the second step (303) and the ion trapping neutralization electrode (40) form an air guide groove and an air gathering port; a third step (304) is arranged at the other end of the inner surface of the ionization chamber (30); the third step (304) is used for fixing the ion-repulsive electrode (50);
the ion trapping neutralization electrode (40) comprises an air inlet diversion trench (401), an ion neutralization trapping plate (403), a neutralization electrode lead (404), a sample air inlet hole (405) and a gas washing air inlet hole (406); connecting the ion neutralization trap plate (403) to a power supply through the neutralization electrode lead (404); the ion neutralization trap plate (403) is used for neutralizing the electric quantity of positively charged ions; the sample air inlet hole (405) and the gas washing air inlet hole (406) are respectively communicated with the air inlet diversion trench (401); the sample air inlet hole (405) is communicated with the sample air inlet pipe (10); the gas washing inlet hole (406) is communicated with the gas washing inlet pipe (70);
after the sample gas to be detected enters the ionization chamber (30) through the sample gas inlet pipe (10) and is fully ionized, positively charged ions are obtained, positive ions are pushed to the ion trapping and neutralizing electrode (40) and neutralized under the action of the electric field force of the trapping electric field of the ion trapping and neutralizing electrode (50) to obtain neutral molecules, the molecules are separated from the ion trapping and neutralizing electrode (40) and are ionized into positive ions again, the sample gas molecules are always converted between an ionic state and a molecular state and are restrained in the action area of the ionization source (20) near the ion trapping and neutralizing electrode (40) by the trapping electric field, and then the sample gas cannot pass through the ion trapping electrode; the photon number for ionization in unit time is reduced, and sample gas molecules with relatively low proton affinity are not ionized again to become neutral molecules, and are carried by the gas washer to pass through the ion repulsion electrode and output; sample gas molecules with relatively high proton affinity cannot pass through the ion-repulsive electrode because they are re-ionized; the gas washing enters the ionization chamber (30) through the gas washing inlet pipe (70), and carries sample gas molecules with relatively low proton affinity through the hollow structure of the ion repulsion electrode (50) and is output from the gas outlet pipe (80).
2. An ion trap gas molecular separation apparatus as defined in claim 1 wherein the ionization source (20) is an ultraviolet ionization source comprising an ultraviolet PID lamp (201), a solenoid drive coil (202), a radio frequency drive power supply (203); the spiral tube driving coil (202) is wound on the ultraviolet PID lamp (201) body; the two poles of the spiral tube driving coil (202) are connected with the radio frequency driving power supply (203); the light-transmitting window (204) of the ultraviolet PID lamp (201) is connected with the ionization chamber (30).
3. An ion trap gas molecular separation apparatus as defined in claim 1 wherein: a fourth step (305) is also arranged on the end surface of the inner surface of the ionization chamber (30) positioned at the same end of the third step (304); the fourth step (305) is used for fixing the outlet collector (60).
4. An ion trap gas molecular separation apparatus as defined in any one of claims 1 to 3 wherein: the ion repulsive electrode (50) comprises an electrode plate (501) and a repulsive electrode lead (502); connecting the electrode sheet (501) with a power supply through the repulsive electrode lead (502); and a hollowed-out channel (503) is arranged on the electrode plate (501).
5. An ion trap gas molecular separation method, characterized in that it uses the ion trap gas molecular separation apparatus according to claim 1, comprising the steps of:
air is introduced, a trapping electric field and an ionization source are started, the excitation power of the ionization source is constant, gas washing is closed, sample injection is started, and sample gas is injected into an ionization reaction cavity; at this time, the number of photons for ionization injected in a unit time of the ionization source is constant, and the number of photons is equal to or greater than the number of molecules of the sample gas; wherein the sample gas molecules comprise at least two substances, and the proton affinity energy of each sample gas molecule is different;
ionization, closing sample introduction, opening gas washing, wherein all sample gas molecules with ionization energy under photon capacity are ionized into positive ions, the positive ions are pushed to an ion trapping and neutralizing electrode under the action of the electric field force of an ion repulsive electrode, neutral molecules are obtained by neutralization, the molecules are separated from the ion trapping and neutralizing electrode and are ionized into positive ions again, the sample gas molecules are always converted between ion states and molecular states and are restrained in an ionization source action area near the ion trapping and neutralizing electrode by a trapping electric field, and then the sample gas cannot pass through the ion repulsive electrode;
the trapping and separation reduce the photon quantity for ionization in unit time, and sample gas molecules with relatively low proton affinity are not ionized again to become neutral molecules, and are carried by the washing gas to pass through an ion repulsive electrode and output; sample gas molecules with relatively high proton affinity cannot pass through the ion-repeller electrode because they are re-ionized.
6. The method of ion trap gas molecular separation of claim 5, further comprising the steps of: sequentially separating, waiting for the completion of trapping and separating, delaying for the completion of detection by a detecting instrument, and jumping to the next trapping and separating until the sample gas is separated one by one according to the sequence from low proton affinity to high proton affinity.
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