CN101592628B - Device and method for increasing photoionization efficiency - Google Patents
Device and method for increasing photoionization efficiency Download PDFInfo
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- CN101592628B CN101592628B CN200910054219.9A CN200910054219A CN101592628B CN 101592628 B CN101592628 B CN 101592628B CN 200910054219 A CN200910054219 A CN 200910054219A CN 101592628 B CN101592628 B CN 101592628B
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Abstract
The invention relates to a method and a device for increasing photoionization efficiency. The device comprises a light source for generating photons, an optical resonator in which the photons move, an electric field applied on the optical resonator, and an introduction port communicated with the optical resonator; and because the photons are vibrated repeatedly in the resonator, the action opportunities of the photons and sample molecules can be greatly improved so as to improve the photoionization efficiency. The direction of the photon resonance in the optical resonator, the direction of feeding a sample from the introduction port and the motion direction of ions formed by the electric field form an orthogonal structure in three-dimensional space so as to reduce pollution and prolong the service life.
Description
Technical field
The present invention relates to a kind of photoionization field, relate in particular to a kind of device and method that strengthens photoionization efficiency.
Background technology
Mass spectrum is to analysis of the molecular structure one of the most accurate method, is commonly used to unknown material carry out qualitative analysis and known component in potpourri is quantitatively detected.Ion gun is mass spectrographic gordian technique, and the most frequently used classics are EI source (electron ionization), and it adopts high-power electron beam bombardment sample, thereby make sample that ionization occur, produces electronics and molion.Principle is as follows:
M+e→M
++2e
M
+the fracture or the intramolecular rearrangement that continue to be subject to electronics bombardment and cause chemical bond, moment produces multiple fragmention.The use in EI source and extensive, ionizing efficiency is high, and spectrum storehouse is the most complete.Yet the electron energy using due to EI source is very high, in spectrogram, fragment peak accounts for morely, and molion peak intensity is very weak and be subject to the interference of other sample fragment peaks, and spectrogram is complicated, very difficult for the spectrum unscrambling that mixes unknown material.
In order to address this problem, produced a series of soft ionization (soft ionization) method.
CI source (chemical ionization).Sample molecule is before bearing electronics bombardment, and by a kind of reaction gas (normally methane etc.) dilution, so the collision probability of sample molecule and electronics is minimum, and the sample molecule ion of the face of giving birth to is mainly produced by reaction gas molecular ionization.The ionization energy in CI source is little, and the mass spectra peak number of generation is few, and very strong molecular ion peak can be provided, and can determine easily molecular weight.But the factors such as the fragmention that CI source produces and the temperature of reaction, Ion source pressure, reaction gas are relevant, do not have standard spectrum not have comparability, and larger to vacuum system consumption.
Utilize Proton-Transfer Reactions (proton transfer reaction) also can produce more complete molecular ion peak, especially small organic molecule is had to outstanding effect.Its shortcoming is, device is complicated, and vacuum consumption is large.
In order to make up these shortcomings, developed photoionization technology.Photoionization and EI source are very similar, and just electron beam is replaced by 5～15eV vacuum ultraviolet photon, and the sample molecule that it can make ionization energy be less than photon energy is ionized.The reaction mechanism of photoionization is:
M+hv→M
++e
Photoionization both can obtain molecular ion peak, can obtain minority fragment ion peak again, significant to the evaluation of unknown material.Photoionization can be divided into atmospheric pressure photoionization (APPI) and vacuum ultraviolet photoionization (VUV-PI).What but classic method was used is vacuum UV lamp (as deuterium lamp) direct irradiation, and photoion stream is inadequate.The EBEL lamp or the ultraviolet laser (UV-SPI) that use rare gas to excite can obtain higher light intensity, solve such problem.But volume is large, cost is higher, the life-span is shorter.
Optical resonator is the light wave cavity that thereby back reflective provides luminous energy to feed back therein.It is the necessary component of laser instrument, conventionally two planes vertical with actuating medium axis or concave spherical mirror, consists of.The effect of resonator cavity is to select frequency light certain, that direction is consistent to do prepreerence amplification, and the light of other frequencies and direction is suppressed.All photons not moving along resonator axis are all overflowed outside chamber very soon, no longer contact with actuating medium; Photon along axial-movement will move in chamber, and constantly come and go operation generation vibration through the reflection of two catoptrons, during operation constantly be excited particle and meet and produce stimulated radiation, photon along axis operation will constantly be bred, in chamber, form the strong beam that the direction of propagation is consistent, frequency is identical with phase place, i.e. laser.For laser is drawn outside chamber, catoptron can be made to part transmission, transmissive portion becomes available laser, and reflecting part is stayed and in chamber, is continued propagation photon.
Optical resonator has been used in and has strengthened infrared optics absorption field.In resonator cavity, be filled with gas, gas molecule has stopped the propagation of photon, and a part is absorbed.This absorption meets Lambert-Beer's law, that is:
The effect of optical resonator in absorption process has:
1, provide longer absorption light path 1;
2, reflection photon, provides more multiaction chance, improves quantum efficiency
Given this, now propose a kind of simple in structure, cheap and can significantly strengthen the device and method of the efficiency of photoionization.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of device and method that strengthens photoionization efficiency, optical resonator will be introduced after sample vaporization, due to photon concussion repeatedly in resonator cavity, can increase substantially the effect chance of photon and sample molecule, thereby improve the efficiency of photoionization.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of device that strengthens photoionization efficiency, this device comprises
Light source, for generation of photon;
The optical resonator adjacent with light source, the photon that light source produces enters rear generation resonance;
Be applied to the electric field on optical resonator, for drawing ion, this electric field comprises repulsion electrode and arranges in opposite directions and be provided with the ground electrode of through hole with repulsion electrode;
Described optical resonator, repulsion electrode and ground electrode surround a host cavity;
Injection port, is communicated with optical resonator for entering the sample molecule after vaporization.
As one of optimal way of the present invention, focus place and described sample molecule approach axis that described injection port is positioned at optical resonator are vertical with photon resonance directions and Ion Extraction.
As one of optimal way of the present invention, described optical resonator is arranged and forms in opposite directions by semi-transparent reflection mirror and completely reflecting mirror.
As one of optimal way of the present invention, the position adjacent at the ground electrode with being provided with through hole is provided with focusing electrode, and described focusing electrode is provided with the second through hole communicating with the through hole of ground electrode.
As one of optimal way of the present invention, described focusing electrode remotely a side of electrode be provided with the intrusion utmost point, the described intrusion utmost point is provided with the third through-hole communicating with the second through hole of focusing electrode.
As one of optimal way of the present invention, described injection port is capillary sample inlet mouth.
As one of optimal way of the present invention, described light source is Kr gas vacuum UV lamp.
As one of optimal way of the present invention, described semi-transparent reflection mirror adopts the BeF of double-sided coating
2lens.
As one of optimal way of the present invention, described optical resonator is hemicon-focal resonator, hemi-concentric resonator, Confocal Resonator or concentric resonator.
The present invention also comprises a kind of method that strengthens photoionization, and the method comprises the following steps:
1>, the photon that light source produces enters concussion repeatedly in optical resonator by catoptron;
2>, the sample molecule after vaporization enters in optical resonator by injection port;
3>, two common electric fields that form of electrode are drawn positive ion or negative ion from the through hole of ground electrode, and wherein photon concussion direction, sample molecule approach axis and Ion Extraction direction are orthogonal.
The present invention strengthens method and the device of photoionization efficiency.Can increase substantially the effect chance of photon and sample molecule, thereby improve the efficiency of photoionization.The ion motion direction that the direction that in optical resonator, the direction of photon resonance, sample enter from injection port and electric field form, is polluted thereby reduce in orthohormbic structure at three dimensions, increases the service life.
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram that the present invention strengthens photoionization efficiency;
Fig. 2 is resonator cavity direction in apparatus of the present invention, sample approach axis and Ion Extraction direction schematic diagram;
Fig. 3 is another structural representation of device that the present invention strengthens photoionization efficiency.
Main element symbol description
Light source 11 semi-transparent reflection mirrors 12
Completely reflecting mirror 13 capillary sample inlet mouths 14
Resonator cavity direction 21, y sample approach axis 22, x
Ion Extraction direction 23, z the second semi-transparent reflection mirror 32
Kr light source 31 second completely reflecting mirrors 33
Capillary sample inlet mouth 34 repulsion electrodes 35
Ground electrode 36 focusing electrodes 37
Immerse the utmost point 38 ion transfer 39
Embodiment
Below in conjunction with accompanying drawing, further illustrate specific embodiment of the invention step.
Strengthen a device for photoionization efficiency, this device comprises
Light source 31 (or 11), for generation of photon;
Optical resonator, adjacent with light source, photon enters rear generation resonance, and optical resonator is arranged and forms in opposite directions by semi-transparent reflection mirror 32 (or 12) and completely reflecting mirror 33 (or 13);
Electric field, puts on optical resonator, for drawing ion, comprises repulsion electrode 35 and the ground electrode 36 that arranges in opposite directions and be provided with through hole with repulsion electrode 35; This through hole is positioned at the middle part of ground electrode.
Described semi-transparent reflection mirror 32, completely reflecting mirror 33, repulsion electrode 35 and ground electrode 36 surround a host cavity;
Injection port 34 (or 14), is communicated with optical resonator for entering the sample molecule after vaporization; Focus place and described sample molecule approach axis that injection port 34 (or 14) is positioned at optical resonator are vertical with photon resonance directions and Ion Extraction.
Described sample molecule approach axis 22 (or x direction); Photon resonance directions 21 in resonator cavity (or y direction); And Ion Extraction direction 23 (or z direction) is vertical.
The position adjacent at the ground electrode 36 with being provided with through hole is provided with focusing electrode 37, and described focusing electrode 37 is provided with the second through hole communicating with the through hole of ground electrode 36.
Described focusing electrode 37 remotely a side of electrode be provided with and invade the utmost point 38, the described intrusion utmost point 38 is provided with the third through-hole communicating with the second through hole of focusing electrode 37.
During use, the photon that light source 31 produces is entered in optical resonator and is repeatedly shaken by catoptron 32 (completely reflecting mirror also can); Sample molecule after vaporization enters in optical resonator by capillary sample inlet mouth 34; Two common electric fields that form of electrode are drawn positive ion or negative ion from the through hole of ground electrode 36, and wherein photon concussion direction, sample molecule approach axis and Ion Extraction direction are orthogonal.This orthohormbic structure can reduce pollution, increases the service life.Resonator cavity direction, sample beam direction and ion beam direction, as shown in Figure 2, can reduce in orthohormbic structure at three dimensions:
1, the pollution of sample to catoptron;
2, sample is to mass spectrometric pollution
3, photon is to mass spectrometric interference
Thereby improve the reliability under unmanned situation, extend the mean free error time (MTBF).
Similar with CI source, the vacuum tightness in resonator cavity can 10
-5between～10Pa, higher air pressure can reduce the generation of fragmention.
The second through hole being provided with through focusing electrode 37 successively from the positive ion of drawing the through hole of ground electrode 36 or negative ion, enter in ion transfer path 39 after invading the third through-hole that the utmost point 38 is provided with.
By the shape of two catoptrons of composition resonator cavity and their relative position, optical resonator can be divided into: plane-parallel resonator, flat-concave cavity, symmetrical concave surface chamber, convex cavities etc.If the focus of concave mirror just in time drops on level crossing in flat-concave cavity, be called hemicon-focal resonator; If the centre of sphere of concave mirror drops on level crossing, just form hemi-concentric resonator.In symmetrical concave surface chamber, the radius-of-curvature of two reflecting spherical mirrors is identical.If reflector focal point is all positioned at the mid point in chamber, just be called Confocal Resonator.If the centre of sphere Qiang center of two spherical mirrors, is called concentric resonator.Gaseous sample molecule enters resonator cavity at focus place can obtain good photoionization effect, as shown in Figure 1.
Another specific embodiment as shown in Figure 3, light source 31 adopts Kr gas vacuum UV lamps; Enter the BeF that lens 32 adopt double-sided coating
2lens, the thickness of plated film can allow ultraviolet light enter resonator cavity but can not escape from; What mirror lens 33 adopted is the coated lens to ultraviolet light total reflection, it and 32 common composition optical resonators; Stainless steel injection port 34, perpendicular to paper, imports resonator cavity by gas; 35,36 electrodes form electric field jointly, when 35 apply positive voltage, will draw positive ion, otherwise draw negative ion, and the aperture of ion from 36 drawn; 37,38 electrodes are needs of focused ion, can increase and decrease according to actual needs; Final ion beam enters ion transfer 39, and imports mass spectrographic mass analyzer into by it.
The present invention will introduce optical resonator after sample vaporization, due to photon concussion repeatedly in resonator cavity, can increase substantially the effect chance of photon and sample molecule, thereby improve the efficiency of photoionization.
Above-described embodiment is the unrestricted technical scheme of the present invention in order to explanation only.Any technical scheme that does not depart from spirit and scope of the invention all should be encompassed in the middle of patent claim of the present invention.
Claims (7)
1. a device that strengthens photoionization efficiency, is characterized in that: this device comprises
Kr gas vacuum ultraviolet lamp source, for generation of photon;
The optical resonator adjacent with light source, photon enters rear generation resonance, by semi-transparent reflection mirror is relative with completely reflecting mirror, forms;
Electric field, for drawing ion, comprises repulsion electrode and arranges in opposite directions and be provided with the ground electrode of through hole with repulsion electrode;
Described semi-transparent reflection mirror, completely reflecting mirror, repulsion electrode and ground electrode surround a receiving space;
Injection port, is communicated with optical resonator for entering the sample molecule after vaporization;
Described sample molecule approach axis is vertical with photon resonance directions and Ion Extraction direction.
2. a kind of device that strengthens photoionization efficiency as claimed in claim 1, is characterized in that: the position adjacent at the ground electrode with being provided with through hole is provided with focusing electrode, and described focusing electrode is provided with the second through hole communicating with the through hole of ground electrode.
3. a kind of device that strengthens photoionization efficiency as claimed in claim 2, is characterized in that: described focusing electrode remotely a side of electrode be provided with the intrusion utmost point, the described intrusion utmost point is provided with the third through-hole communicating with the second through hole of focusing electrode.
4. a kind of device that strengthens photoionization efficiency as claimed in claim 1, is characterized in that: described injection port is positioned at the focus place of optical resonator.
5. a kind of device that strengthens photoionization efficiency as claimed in claim 1, is characterized in that: described injection port is capillary sample inlet mouth.
6. a kind of device that strengthens photoionization efficiency as claimed in claim 1, is characterized in that: described semi-transparent reflection mirror adopts the BeF of double-sided coating
2lens.
7. a kind of device that strengthens photoionization efficiency as claimed in claim 1, is characterized in that: described optical resonator is hemicon-focal resonator, hemi-concentric resonator, Confocal Resonator or concentric resonator.
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| CN200910054219.9A CN101592628B (en) | 2009-06-30 | 2009-06-30 | Device and method for increasing photoionization efficiency |
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|---|---|---|---|
| CN200910054219.9A CN101592628B (en) | 2009-06-30 | 2009-06-30 | Device and method for increasing photoionization efficiency |
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| CN101592628A CN101592628A (en) | 2009-12-02 |
| CN101592628B true CN101592628B (en) | 2014-10-15 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104377108A (en) * | 2013-08-13 | 2015-02-25 | 中国科学院大连化学物理研究所 | In-situ pyrolytic ion source for detecting free radicals and reaction intermediates |
| EP3567625A1 (en) * | 2018-05-09 | 2019-11-13 | Helmholtz Zentrum München - Deutsches Forschungszentrum für Gesundheit und Umwelt (GmbH) | Device and method for mass spectroscopic analysis of particles |
| CN110662336A (en) * | 2019-09-27 | 2020-01-07 | 北京石油化工学院 | Ionization device and method for laser resonant cavity |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002181788A (en) * | 2000-12-18 | 2002-06-26 | Mitsubishi Heavy Ind Ltd | Photoionization mass spectrometer |
| CN1818632A (en) * | 2006-03-17 | 2006-08-16 | 中国科学院安徽光学精密机械研究所 | Safety door inspector based on photoionization detecting technology |
| CN101063673A (en) * | 2006-04-26 | 2007-10-31 | 中国科学院大连化学物理研究所 | Vacuumeultraviolet lamp ionization device in time-of-flight mass spectrometer |
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| US20030075679A1 (en) * | 2001-10-16 | 2003-04-24 | Syage Jack A. | Photoionization mass spectrometer |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002181788A (en) * | 2000-12-18 | 2002-06-26 | Mitsubishi Heavy Ind Ltd | Photoionization mass spectrometer |
| CN1818632A (en) * | 2006-03-17 | 2006-08-16 | 中国科学院安徽光学精密机械研究所 | Safety door inspector based on photoionization detecting technology |
| CN101063673A (en) * | 2006-04-26 | 2007-10-31 | 中国科学院大连化学物理研究所 | Vacuumeultraviolet lamp ionization device in time-of-flight mass spectrometer |
Non-Patent Citations (2)
| Title |
|---|
| 一氧化氮的衰荡质谱;盛新志等;《北方交通大学学报》;20011231;第25卷(第6期);第26页最后一段到第27页第4段和图2 * |
| 盛新志等.一氧化氮的衰荡质谱.《北方交通大学学报》.2001,第25卷(第6期), |
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