CN103972018A - Radio-frequency electric field enhanced single photon and chemical ionization source - Google Patents
Radio-frequency electric field enhanced single photon and chemical ionization source Download PDFInfo
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Abstract
The invention relates to a mass spectrometer ionization source, in particular to a radio-frequency electric field enhanced single photon and chemical ionization source comprising a vacuum ultraviolet source, an ion generation and transmission area and a vacuum chamber vacuum cavity. A plurality of transmission electrodes and vacuum differential perforated electrodes are disposed in parallel and at intervals in the ion generation and transmission area. Each electrode is axially provided with a through hole. Ultraviolet emitted by the vacuum ultraviolet source enters the perforated electrodes along the axes. Direct-current voltage is applied to all transmission electrodes and perforated electrodes; radio-frequency voltage is superposed to one transmission electrode. Two different ionization ways are switched by controlling start and stop of the radio-frequency voltage. The radio-frequency electric field enhanced single photon and chemical ionization source comprises the single photon ionization source, the chemical ionization source is obtained through photoelectron ionization reagent gas obtained by means of photoelectric effect, radio-frequency electric field is introduced to the ionization area to enhance chemical ionization triggered by photoelectrons, detection sensitivity is improved, soft ionization of sample molecules with ionization energy higher than the energy of ultraviolet photons can be achieved, and range of analyzable samples is widened.
Description
Technical field
The present invention relates to mass spectrometer ionization source, single photon-chemical ionization source that a kind of rf electric field strengthens specifically.The present invention is on the basis that comprises single photon ionization source, utilize the photoelectron ionization reagents gas that photoelectric effect obtains to obtain chemical ionization source, strengthen by introducing rf electric field in ionized region the chemi-ionization that photoelectron causes, improve detection sensitivity, and can realize the soft ionization of ionization energy higher than the sample molecule of ultraviolet photon energy, widen the scope of analytic sample.By the control to radio-frequency voltage opening and closing, can realize neatly two kinds of switchings between different ionization modes.
Background technology
In traditional organic substance mass spectrum, conventionally adopt electron impact ionization source (EI), it utilizes the electronics of 70eV energy to remove to bombard organic molecule, makes its ionization, and every kind of organic substance can obtain feature spectrogram separately, by spectrogram library searching, mostly can carry out accurately qualitative analysis.But, produce sometimes a large amount of fragment ions, the especially peak overlap in the time of Analysis of Complex mixture, identification of spectrogram difficulty, is unfavorable for quick, the on-line analysis of sample.Vacuum-ultraviolet light can make the organic molecule generation soft ionization of ionization energy (IE) lower than its photon energy, mainly produces molecular ion, almost there is no fragment ion, is suitable for qualitative and quantitative analysis fast.Hou Keyong [Chinese invention patent: 200610011793.2] and Zheng Peichao [Chinese invention patent: 200810022557.X] are combined vacuum ultraviolet light ionization source with mass spectrum, in the organic substance spectrogram obtaining, only comprise organic molecular ion peak, spectrogram is simple, can carry out qualitative and quantitative analysis fast according to molecular weight and signal strength signal intensity.
The optical window materials limitations particularly using in vacuum UV lamp in vacuum ultraviolet light source see through the photon energy of light.The at present known LiF optical window material that only has reaches as high as 11.8eV through photon energy.So, only have ionization energy to utilize 11.8eV photon energy to access effective ionization lower than the organic molecule of 11.8eV, ionization energy is helpless higher than the compound photon of 11.8eV.For addressing this problem, the photoelectron of spending [PCT:201010567193] of heap of stone to adopt vacuum ultraviolet light source to produce in reagent area accelerates ionization reagents gas under electrostatic field, produces reagent ion.Then transmit reagent ion and enter reaction zone and sample molecule generation chemi-ionization.This invention realized the online switching of single photon ionization and chemi-ionization two kinds of soft ionization modes, widened can analyte scope.
But the limited optical density of commercial vacuum ultraviolet (VUV) lamp source, has not only limited the sensitivity of single photon ionization, and has limited photoelectronic quantity, has reduced reagent ion intensity, causes chemi-ionization sensitvity constraint.And, under higher air pressure conditions, electronics and gas molecule frequent impact, after bumping, need to from electrostatic field, regain energy and remove ionization by collision molecule, but electronics one direction rectilinear motion in electrostatic field, movement velocity is fast, electronics is short in the time of staying of ionized region, causes electrostatic field to accelerate the inefficiency of photoelectron ionization reagents gas molecule.
Summary of the invention
Single photon-the chemical ionization source that the object of the present invention is to provide a kind of rf electric field to strengthen, on the basis that comprises single photon ionization source, by introduce rf electric field in ionized region, utilize rf electric field light modulated electronic, reciprocating motion, improve photoelectron motion distance and the time of staying in ionized region, strengthen photoelectron ionization, improve detection sensitivity, and utilize chemical ionization source can realize the soft ionization of ionization energy higher than the sample molecule of ultraviolet photon energy.By the control to radio-frequency voltage opening and closing, can realize flexibly the switching between single photon ionization, two kinds of different ionization modes of single photon-chemi-ionization.
For achieving the above object, the technical solution used in the present invention is:
Single photon-chemical ionization source that a kind of rf electric field strengthens, comprise vacuum ultraviolet light source, ionization chamber cavity, one or more transmission electrode and difference pore electrod, on ionization chamber cavity wall, have sample gas capillary interface, reagent gas capillary interface, vacuum gauge interface and vacuum pump bleeding point;
Transmission electrode is placed in ionization chamber inside cavity, transmission electrode axially have a through hole; In the time being more than one transmission electrode, between more than one transmission electrode, be parallel to each other, interval arrange, through hole is coaxial;
The ionization chamber cavity wall of locating in the through hole top of transmission electrode is provided with ultraviolet light entrance, and ultraviolet light entrance is coaxial with through hole; Below place in transmission electrode is provided with difference pore electrod, and the hole of difference pore electrod is coaxial with through hole, and the ultraviolet light that ultraviolet source sends is radiated at difference pore electrod surface from ultraviolet light entrance, produces photoelectron by photoelectric effect;
On transmission electrode, be applied with direct current transmission voltage; In the time being more than one transmission electrode, on each electrode of more than one transmission electrode, be applied with successively direct current transmission voltage, the voltage applying successively on each electrode reduces successively along light incident direction;
Be superimposed with a radio-frequency voltage in one of them of transmission electrode by capacity coupled mode;
In the time being more than one transmission electrode, on other the every plate electrodes except being superimposed with the transmission electrode of radio-frequency voltage, all pass through capacity earth;
On difference pore electrod, be applied with direct voltage, and by capacity earth, be also connected to ground by resistance simultaneously;
Reagent gas capillary and sample gas capillary enter ionization chamber inside by the reagent gas capillary interface on ionization chamber cavity wall and sample gas capillary interface respectively; Reagent gas capillary and sample gas gas vent capillaceous is between transmission electrode and difference pore electrod or between transmission electrode and transmission electrode; Reagent gas capillary and sample gas gas outlet end capillaceous is perpendicular to ultraviolet light beam.
On each electrode of more than one transmission electrode, be applied with successively direct current transmission voltage, direct current transmission voltage adopts same DC power supply, and the direct voltage applying successively on each electrode carries out dividing potential drop by resistance.
Between transmission electrode and difference pore electrod, separate by insulating material, in the middle of all electrodes, have through hole, coaxial and interval setting between electrode;
In the time being more than one transmission electrode, between adjacent two transmission electrodes, separate by insulating material, in the middle of all transmission electrodes, have through hole, coaxial and interval setting between transmission electrode.
Difference pore electrod middle part has aperture, coaxial with transmission electrode;
Be provided with mass analyzer in difference pore electrod below, the ion that ionization chamber produces enters mass analyzer by aperture; Described mass analyzer is time of flight mass analyzer, level Four bar mass analyzer or ion strap mass analyzer.
Ultraviolet source can be gas-discharge light source, LASER Light Source or synchrotron radiation light source.
Sample is by sample gas capillary sample inlet;
Vacuum gauge interface is connected with vacuum gauge, and vacuum pump bleeding point is connected with vacuum pump through control valve; Ionization chamber vacuum degree, by vacuum pump and control valve control, maintains 1Pa between 500Pa; Ionization chamber vacuum values obtains by vacuum gauge.
Ionization source can be realized the switching of two kinds of different mode of operations;
In the time closing radio-frequency voltage, it is single photon ionization pattern; In the time opening radio-frequency voltage, the photoelectron that photoelectric effect produces obtains energy from radiofrequency field, and photoelectron ionization by collision reagent gas produces reagent ion, obtains the chemical ionization source of soft ionization, and now single photon ionization and chemi-ionization act on simultaneously;
Transmission electrode is sheet or tabular, and middle part (axially refers to the normal direction perpendicular to plate face) vertically and has through hole.
Ionization source provided by the invention, on the basis that comprises single photon ionization source, by introducing rf electric field in ionized region under medium air pressure conditions, utilize the vibration of rf electric field control photoelectron, effectively ionization reagents gas, the reagent ion of generation further with sample molecule generation chemi-ionization.Only, by controlling the opening and closing of radio-frequency voltage, can realize the quick switching of two kinds of soft ionization modes.
Brief description of the drawings
Fig. 1 is single photon-chemical ionization source structural representation that the rf electric field based on vacuum-ultraviolet light of the present invention strengthens.
Fig. 2 is 10ppm benzene in embodiment 1, toluene and dimethylbenzene gaseous sample (O
2for Balance Air) mass spectrogram under different condition, comprise only have ultraviolet light photo from time, while not having ultraviolet light only to have radio-frequency voltage, when ultraviolet light and radio-frequency voltage apply simultaneously.
Fig. 3 is O in embodiment 2
2radiofrequency field chemi-ionization 10ppm chloroform (CHCl during as reagent gas
3) accumulative total 500,000 times obtain mass spectrogram, the ionization energy of chloroform is 11.4eV, is greater than photon energy 10.6eV.
Fig. 4 is O in embodiment 3
2the intensification factor of different ionization energy samples during as reagent gas.
Embodiment
Referring to Fig. 1, is structural representation of the present invention.Ionization source of the present invention by vacuum ultraviolet light source 1, ionization chamber cavity 2, some transmission electrodes 4 and difference pore electrod 5, has sample gas capillary 3 interfaces on ionization chamber cavity 2 walls, reagent gas capillary 9, and vacuum gauge 6 interfaces and vacuum pump 7 bleeding points form.
Reagent gas capillary 9 and sample gas capillary 3 enter ionization chamber inside by reagent gas capillary 9 interfaces on ionization chamber cavity 2 walls and sample gas capillary 3 interfaces respectively; The gas vent of reagent gas capillary 9 and sample gas capillary 3 is between transmission electrode and difference pore electrod or between transmission electrode and transmission electrode; The gas outlet end of reagent gas capillary 9 and sample gas capillary 3 is perpendicular to ultraviolet light beam.
Ionization chamber air pressure is controlled by the control valve 8 that connects vacuum pump 7, and air pressure maintains 1Pa between 500Pa; Atmospheric pressure value obtains by vacuum gauge 6.
Transmission electrode 4 is placed in ionization chamber cavity 2 inside, transmission electrode 4 axially have a through hole; In the time being more than one transmission electrode 4, between more than one transmission electrode 4, be parallel to each other, interval arrange, through hole is coaxial; Ionization chamber cavity 2 walls of locating in the through hole top of transmission electrode 4 are provided with ultraviolet light entrance, and ultraviolet light entrance is coaxial with through hole; Below place in transmission electrode 4 is provided with difference pore electrod 5, and the hole of difference pore electrod 5 is coaxial with through hole, and the ultraviolet light that ultraviolet source 1 sends is radiated at difference pore electrod 5 surfaces from ultraviolet light entrance, produces photoelectron by photoelectric effect; On transmission electrode 4, be applied with direct current transmission voltage; In the time being more than one transmission electrode 4, on each electrode of more than one transmission electrode 4, be applied with successively direct current transmission voltage, the voltage applying successively on each electrode reduces successively along light incident direction; Be superimposed with a radio-frequency voltage in one of them of transmission electrode 4 by capacity coupled mode; In the time being more than one transmission electrode 4, on other the every plate electrodes except being superimposed with the transmission electrode 4 of radio-frequency voltage, all pass through capacity earth; On difference pore electrod 5, be applied with direct voltage, and by capacity earth, be also connected to ground by resistance simultaneously;
The ion that ionization chamber produces enters mass analyzer by aperture; Described mass analyzer is time of flight mass analyzer, level Four bar mass analyzer or ion strap mass analyzer.
Ionization source can be realized the switching of two kinds of different mode of operations.In the time closing radio-frequency voltage, it is single photon ionization pattern; In the time opening radio-frequency voltage, the photoelectron that photoelectric effect produces obtains energy from radiofrequency field, and photoelectron ionization by collision reagent gas generation reagent ion obtains the chemical ionization source of soft ionization, and now single photon ionization and chemi-ionization act on simultaneously;
When ionization source of the present invention works in rf electric field enhancing chemi-ionization pattern, sample gas passes into ionization chamber by sample capillary 3, and reagent gas passes into ionization chamber by reagent capillary 9.Ultraviolet light produces photoelectric effect and discharges photoelectron on difference pore electrod 5.Photoelectron is done oscillating movement at ionization chamber under the effect of rf electric field, and continuous and reagent gas molecular collision, produces a large amount of reagent ions.In the time that reagent gas molecular ionization can be higher than ionized sample molecule energy, the chemi-ionization that sample molecule generation electric charge shifts.The sample ions obtaining, under the effect of transmission electrode 4, enters mass analyzer by difference pore electrod 5.
When ionization source works in single photon ionization pattern, sample gas passes into ionization chamber by sample capillary 3., in the time that photon energy is greater than molecular ionization energy, can there is photo ionization in molecule absorption ultraviolet photon.
Embodiment 1
For the examination of ionization source rf electric field humidification of the present invention, the commercialization Kr lamp that use transmitting photon energy is 10.6eV is as vacuum ultraviolet light source, by this ionization source and the coupling of time of flight mass analyzer.Selecting internal diameter is that Φ 150 μ m, the length quartz capillary that is 30cm is respectively as sample gas sample feeding pipe.Sample gas is benzene (IE=9.24eV), toluene (IE=8.83eV), the paraxylene (IE=8.44eV) of 10ppm, and sample gas is with O
2as balanced gas, this experiment is directly with Balance Air O
2(IE=12.07eV) as reagent gas.Air pressure in adjusting ionization source cavity is to 50Pa, and gas sampling amount is 20mL/min.Transmission electrode adopts two plate electrode compositions at this.First applies direct voltage 12V, and second applies DC power supply 11V, and the peak-to-peak value that superposes on second transmission electrode is 216V, the radio-frequency voltage of frequency 7MHz.On difference pore electrod, apply direct voltage 5V.The spacing of three electrodes is 6mm.First transmission electrode and difference pore electrod ground connection filter capacitor size are all 100 μ F, and on second transmission electrode, RF-coupled capacitance size is 100nF.Situation one: only open uviol lamp, carry out single photon ionized sample molecule; Situation two: only apply rf electric field; Situation three: open uviol lamp, apply rf electric field, chemi-ionization.The mass signal obtaining as shown in Figure 2.As seen from the figure, provide under photoelectronic condition at uviol lamp, after introducing rf electric field, significantly improved signal strength signal intensity.
Embodiment 2
Widen the Performance of analyte ranges for ionization source of the present invention, sample gas is 10ppm chloroform (IE=11.37eV), chooses the O of ionization energy higher than photon energy 10.6eV
2(12.07eV) as balanced gas and reagent gas.Selecting internal diameter is that Φ 150 μ m, the length quartz capillary that is 30cm is as sample gas sample feeding pipe.Air pressure in adjusting ionization source cavity is to 50Pa, and gas sampling amount is 20mL/min.First applies direct voltage 12V, and second applies DC power supply 11V, and the peak-to-peak value that superposes on second transmission electrode is 216V, the radio-frequency voltage of frequency 7MHz.On difference pore electrod, apply direct voltage 5V.The spacing of three electrodes is 6mm.First transmission electrode and difference pore electrod ground connection filter capacitor size are all 100 μ F, and on second transmission electrode, RF-coupled capacitance size is 100nF.Total cumulative number 500,000 times, obtains the mass signal shown in Fig. 3.Wherein, mass-to-charge ratio is that 83,85,87 peak is CHCl
2 +, spectrogram, almost without fragment ion, has been realized the soft ionization of high ionization energy sample chloroform.
Embodiment 3
Under the same condition of work of embodiment 2, change different samples, the intensification factor of testing radio frequency electric field soft ionization source.As shown in Figure 4, (a) be less than the sample of photon energy 10.6eV for ionization energy, multiple is the comparison of radiofrequency field chemi-ionization and single photon ionic activity; (b) be greater than the sample of photon energy 10.6eV for ionization energy, multiple is the comparison that radiofrequency field chemi-ionization and DC fields produce chemi-ionization intensity.The condition of work that DC fields produces chemi-ionization is: transmission voltage first applies direct voltage 150V, and second applies direct voltage 13V, and difference pore electrod applies direct voltage 5V.As seen from the figure, this ionization source, on the basis that comprises single photon ionization pattern, by introducing rf electric field under medium air pressure conditions, is controlled photoelectron vibration, effectively ionization reagents gas, the reagent ion of generation further with sample molecule generation chemi-ionization.This ionization source has not only improved detection sensitivity, and can ionize the sample of ionization energy higher than photon energy, widened can analyzing and testing molecule scope.And only by controlling the opening and closing of radio-frequency voltage, can realize the quick switching of two kinds of soft ionization modes.
Claims (8)
1. single photon-the chemical ionization source that rf electric field strengthens, it is characterized in that: comprise vacuum ultraviolet light source (1), ionization chamber cavity (2), one or more transmission electrode (4) and difference pore electrod (5), on ionization chamber cavity (2) wall, have sample gas capillary (3) interface, reagent gas capillary (9) interface, vacuum gauge (6) interface and vacuum pump (7) bleeding point;
Transmission electrode (4) is placed in ionization chamber cavity (2) inside, transmission electrode (4) axially have a through hole; In the time being more than one transmission electrode (4), more than one transmission electrode is parallel to each other between (4), interval arranges, and through hole is coaxial;
Ionization chamber cavity (2) wall of locating in the through hole top of transmission electrode (4) is provided with ultraviolet light entrance, and ultraviolet light entrance is coaxial with through hole; Be provided with difference pore electrod (5) in the below place of transmission electrode (4), the hole of difference pore electrod (5) is coaxial with through hole, the ultraviolet light that ultraviolet source (1) sends is radiated at difference pore electrod (5) surface from ultraviolet light entrance, produces photoelectron by photoelectric effect;
Transmission electrode is applied with direct current transmission voltage on (4); In the time being more than one transmission electrode (4), on each electrode of more than one transmission electrode (4), be applied with successively direct current transmission voltage, the voltage applying successively on each electrode reduces successively along light incident direction;
Be superimposed with a radio-frequency voltage in one of them of transmission electrode (4) by capacity coupled mode;
In the time being more than one transmission electrode (4), on other the each electrodes except being superimposed with the transmission electrode (4) of radio-frequency voltage, pass through capacity earth;
Difference pore electrod is applied with direct voltage on (5), and by capacity earth, is also connected to ground by resistance simultaneously;
Reagent gas capillary (9) and sample gas capillary (3) enter ionization chamber inside by reagent gas capillary (9) interface on ionization chamber cavity (2) wall and sample gas capillary (3) interface respectively; The gas vent of reagent gas capillary (9) and sample gas capillary (3) is between transmission electrode and difference pore electrod or between transmission electrode and transmission electrode; The gas outlet end of reagent gas capillary (9) and sample gas capillary (3) is perpendicular to ultraviolet light beam.
2. single photon-chemical ionization source according to claim 1, is characterized in that:
On each electrode of more than one transmission electrode (4), be applied with successively direct current transmission voltage, direct current transmission voltage adopts same DC power supply, and the direct voltage applying successively on each electrode carries out dividing potential drop by resistance.
3. single photon-chemical ionization source according to claim 1, is characterized in that:
Between transmission electrode (4) and difference pore electrod (5), separate by insulating material, in the middle of all electrodes, have through hole, coaxial and interval setting between electrode.
4. according to single photon-chemical ionization source described in claim 1 or 3, it is characterized in that:
In the time being more than one transmission electrode (4), between adjacent two transmission electrodes, separate by insulating material, in the middle of all transmission electrodes, have through hole, coaxial and interval setting between transmission electrode.
5. single photon-chemical ionization source according to claim 1, is characterized in that:
Difference pore electrod (5) middle part has aperture, coaxial with transmission electrode;
Be provided with mass analyzer in difference pore electrod (5) below, the ion that ionization chamber produces enters mass analyzer by aperture; Described mass analyzer is time of flight mass analyzer, level Four bar mass analyzer or ion strap mass analyzer.
6. single photon-chemical ionization source according to claim 1, is characterized in that:
Ultraviolet source (1) can be gas-discharge light source, LASER Light Source or synchrotron radiation light source.
7. single photon-chemical ionization source according to claim 1, is characterized in that:
Sample is by sample gas capillary (3) sample introduction;
Vacuum gauge (6) interface is connected with vacuum gauge (6), and vacuum pump (7) bleeding point is connected with vacuum pump (7) through control valve (8); Ionization chamber vacuum degree, by vacuum pump (7) and control valve (8) are controlled, maintains 1Pa between 500Pa; Ionization chamber vacuum values obtains by vacuum gauge (6).
8. single photon-chemical ionization source according to claim 1, is characterized in that:
Ionization source can be realized the switching of two kinds of different mode of operations;
In the time closing radio-frequency voltage, it is single photon ionization pattern; In the time opening radio-frequency voltage, the photoelectron that photoelectric effect produces obtains energy from radiofrequency field, and photoelectron ionization by collision reagent gas produces reagent ion, obtains the chemical ionization source of soft ionization, and now single photon ionization and chemi-ionization act on simultaneously.
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| CN112020760A (en) * | 2018-09-28 | 2020-12-01 | 爱奥尼肯分析股份有限公司 | IMR-MS device |
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