CN102103972A - Vacuum ultraviolet lamp ionization device - Google Patents
Vacuum ultraviolet lamp ionization device Download PDFInfo
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- CN102103972A CN102103972A CN2009102654470A CN200910265447A CN102103972A CN 102103972 A CN102103972 A CN 102103972A CN 2009102654470 A CN2009102654470 A CN 2009102654470A CN 200910265447 A CN200910265447 A CN 200910265447A CN 102103972 A CN102103972 A CN 102103972A
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Abstract
The invention discloses a vacuum ultraviolet lamp ionization device, which comprises an ionization chamber, an ultraviolet lamp, a repulsion plate, a permanent-magnet focusing ring, a small-hole plate, a capillary sample injector and a lens system. An ionization source in the vacuum ultraviolet lamp ionization device has two working modes: an ultraviolet ionization mode and an ultraviolet and electron collision ionization mode, which can be converted by voltage regulation. An electron moves helically under the action of the permanent-magnet focusing ring on the electron, thereby increasing a probability of electron collision and improving the detection sensitivity of the electron collision ionization mode. The vacuum ultraviolet lamp ionization device is characterized by wide range of a sample to be detected, high sensitivity, low energy consumption, long service life, wide range of a working pressure and the like, and has a wide application prospect in process monitoring and environmental on-line analysis.
Description
Technical field
The present invention relates to the mass spectrum ionization source, design permanent-magnetic focusing ring is to improve ion transmission efficiency in ionization process; This technology has not only improved the ionization efficiency of transmission, and has realized the switching from pattern of ultraviolet light and electron impact ionization pattern and ultraviolet light photo.
Background technology
The vacuum UV lamp ionization source has advantages such as volume is little, low in energy consumption, highly sensitive, and the life-span is long, and spectrogram is simple, is suitable for the on-line monitoring of complex sample analysis and sample, fields such as process monitoring.But compare with the electron impact ionization source, the ionization energy that the vacuum UV lamp ionization source requires to be ionized sample is lower than its energy of photoelectron, and the fragment information of compound is less, is difficult to obtain the structural information of sample compound.
The electron impact ionization source has simple in structure, can obtain compound fragment information, contrasts the advantage that can realize the evaluation of compound with the standard spectrogram.But its power consumption height, the life-span is short because the spectrogram more complicated, and molecular ion peak often a little less than, be difficult to complex sample is differentiated.
It is important research project that two kinds of ionization sources are combined always.Present solution mainly is that the electron impact ionization device is integrated in the ultraviolet light ionization device.This scheme all has harsh requirement in power consumption and useful life to air pressure, and technical sophistication in the integrating process, causes cost to increase greatly.
Summary of the invention
The object of the present invention is to provide a kind of mass spectral ionization device of vacuum UV lamp that is used for, it is low, highly sensitive to have a detection line, advantage such as the sample range of choice is wide, and the life-span is long, and is low in energy consumption.
For achieving the above object, the technical solution used in the present invention is:
A kind of ionization device of vacuum UV lamp comprises an ionization chamber, and the vacuum UV lamp as ionization source is installed above ionization chamber, is provided with a repeller plate at distance vacuum UV lamp beneath window 1-4mm place,
The 10-30mm place is provided with a permanent-magnetic focusing ring under the distance repeller plate, and the permanent-magnetic focusing ring is the plectane of middle perforate, and the aperture is 2mm-20mm, and coaxial with repeller plate;
The 0.1-100mm place is provided with an aperture plate under the permanent-magnetic focusing ring, and aperture plate is the plectane of middle perforate, and the aperture is 0.1mm-20mm, and coaxial with repeller plate;
The 1-4mm place is provided with three coaxial lens under aperture plate, and is coaxial with repeller plate;
Being respectively equipped with the thick insulated enclosure pad of 1-3mm between permanent-magnetic focusing ring, aperture plate and lens intercepts;
One sample introduction capillary carries out ionization with the beneath window that gaseous sample is introduced the vacuum UV lamp front end from a side of ionization chamber, and the optical axis of vacuum UV lamp is perpendicular with the sample introduction direction of gaseous sample;
Repeller plate, permanent-magnetic focusing ring, aperture plate and lens all be provided with ionization chamber inside and with the light shaft coaxle of vacuum UV lamp; On the ionization chamber wall under the lens, have the hole, under the hole, be provided with a mass analyzer.
The sidewall of ionization chamber is provided with pump interface; On repeller plate, apply the voltage of 1-100V; The voltage that applies on the permanent-magnetic focusing ring is the 60-95% of repeller plate voltage;
The permanent-magnetic focusing ring is the permanent magnet with 100～2000 Gausses, and has electric conductivity.
Under vacuum ultraviolet ionized pattern, the voltage that applies on aperture plate is 0～-20V.
Under vacuum-ultraviolet light and electron impact ionization pattern, the voltage that applies on aperture plate is-10～-150V.
The vacuum-ultraviolet light that is sent by uviol lamp impinges upon and produces photoelectron on the aperture plate, is accelerated in the electric field of photoelectron between aperture plate and repeller plate, with the sample molecule generation electron impact ionization in the ionization chamber.The vacuum-ultraviolet light that vacuum UV lamp sends can also form sample ions with the ionization of sample molecule direct sunshine.The sample ions that produces is focused on the back by the permanent-magnetic focusing ring and introduces aperture plate, enters mass analyzer after the adjustment of scioptics system.
Because use the structural design of permanent-magnetic focusing ring and aperture plate, the present invention has following advantage:
1. the convex electric field can converge to the cation in a big way in the hole of aperture plate, has improved ion transmission efficiency greatly.
2. the voltage pressure reduction between permanent-magnetic focusing ring and the repeller plate is less, and the ion beam of Xing Chenging energy dispersion on direction of principal axis is smaller like this, helps the shaping of lens combination.
3. by regulating aperture plate voltage, can realize that ultraviolet light photo is from pattern and ultraviolet light and electron impact ionization mode switch.
4. the magnetic field that on the permanent-magnetic focusing ring surrounding space is applied can make electronics move with helical trajectory, has strengthened the collision probability of electronics and sample molecule, improves the sensitivity of ionization source under ultraviolet light and the electron impact ionization pattern.
Under ultraviolet light and electron impact ionization pattern, ionization source have ultraviolet light photo from the advantage of two kinds of ionization sources of electron impact ionization.This ionization source can strengthen the signal peak of its molecular ion on the basis of the fragment that electron impact ionization produces, and its life-span and power consumption all is better than because the electron impact ionization source.The comparative result of ultraviolet light and electron impact ionization source and electron impact ionization source and ultraviolet light ionization source is as shown in table 1, from the table more as can be seen, the advantage of electron impact ionization source and ultraviolet light ionization source has been concentrated in ultraviolet light and electron impact ionization source.
Because the photon ratio less (10 that produces in the unit interval of vacuum UV lamp
10Photons/s), thus its sensitivity not high be the key factor that restriction vacuum UV lamp photo ionization is used always.In the present invention, use the permanent-magnetic focusing ring, can make the interior in a big way ion focusing that produces to aperture plate, thereby scioptics obtain stronger ion signal to the ion shaping then.In the present invention, be the convex electric field by permanent-magnetic focusing ring and the formed electric field of aperture plate, cation is converged effect.Electronics is subjected to the constraint in magnetic field, advances in the screw mode.The Simion analog result as shown in Figure 4.As can be seen from the figure the convex electric field to the effect of converging of ion and magnetic field to the prolongation effect of electron path.Do not compare with adding the permanent-magnetic focusing ring among the present invention, signal strength signal intensity can improve about 2 orders of magnitude under the uviol lamp ionization pattern, and signal improves about 5-10 times under the electron ionization pattern.The present invention is not having under the situation of enrichment with after the time of flight mass analyzer is connected, and adds up for 300,000 times in the 24s, and the benzene detection line can reach 0.1ppm in the mass spectrogram that obtains, and is better than the similar ionization source of bibliographical information greatly.
In sum, it is wide that the present invention has the testing sample scope, highly sensitive, low in energy consumption, and the life-span is long, and characteristics such as operating air pressure wide ranges are having broad application prospects aspect process monitoring and the analysis of organic pollution real-time online.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is for adding behind the magnetic field contrast of air signal strength signal intensity when not adding magnetic field among the present invention
Fig. 3 is the Simion analog result that the permanent-magnetic focusing ring is strengthened the EI ionization mechanism
Embodiment
As shown in Figure 1, a kind of ionization device of vacuum UV lamp comprises an ionization chamber 2, and the vacuum UV lamp 1 as ionization source is installed above ionization chamber 2, and 1 beneath window 1-4mm place is provided with a repeller plate 3 at the distance vacuum UV lamp,
The 30mm place is provided with a permanent-magnetic focusing ring 5 under distance repeller plate 3, and permanent-magnetic focusing ring 5 is the plectane of middle perforate, and the aperture is 6mm, and coaxial with repeller plate 3;
The 1mm place is provided with an aperture plate 7 under permanent-magnetic focusing ring 5, and aperture plate 7 is the plectane of middle perforate, and the aperture is 1mm, and coaxial with repeller plate 3;
The 1mm place is provided with three coaxial lens 8 under aperture plate 7, and is coaxial with repeller plate 3;
Being respectively equipped with the thick insulated enclosure pad of 1mm between permanent-magnetic focusing ring 5, aperture plate 7 and lens 8 intercepts;
One sample introduction capillary 4 carries out ionization with the beneath window that gaseous sample is introduced vacuum UV lamp 1 front end from a side of ionization chamber, and the optical axis of vacuum UV lamp 1 is perpendicular with the sample introduction direction of gaseous sample;
Utilize the air pressure in capillary pipe length and the caliber adjustment assurance ionized region among the present invention, sample is introduced into ionized region from atmosphere, vertical with the uviol lamp light beam.Repeller plate adds 10V voltage with uviol lamp is coaxial at a distance of 1mm, and the permanent-magnetic focusing ring is the 20mm place below repeller plate, and institute's making alive is 90% of a repeller plate voltage.Aperture plate is the 1mm place below the permanent-magnetic focusing ring, according to use pattern difference, and institute's making alive difference.Under vacuum ultraviolet ionized pattern, aperture plate ground connection, for-4V.Under vacuum-ultraviolet light and electron impact ionization pattern, aperture plate institute making alive is-60V.Lens combination is the 1mm place below aperture plate, and by the insulation spacer hermetic barrier, institute's making alive is relevant with aperture plate voltage with repeller plate voltage.
Under pattern, aperture plate is-4V at ultraviolet light photo.The photon that uviol lamp is launched with interact by the sample of the vertical introducing of capillary, make sample generation ionization, the cation that produces after the ionization enters lens combination after converging the aperture that converges to aperture plate under the effect of electric field.By voltage-regulation, lens carry out shaping to ion beam.
Under ultraviolet light and electron impact ionization pattern, aperture plate connects negative voltage, when connect-during the 60V left and right sides, the effect of the electron impact ionization of acquisition is better, the signal that is produced by electron impact ionization is compared when not adding magnetic field and is risen to original 5-10 doubly.The electron helical motion that causes by magnetic field by a sample gas part of introducing by capillary shown in Figure 3 by ultraviolet light photo from, the product multiform becomes molecular ion.The electron collision that another part has been accelerated, product is fragment ion and molecular ion.The ion signal that is produced by two kinds of ionization all is focused the shaping of back introducing lens combination, enters in the mass analyzer at last and analyzes.
Have or not under the magnetic field condition mass signal as shown in Figure 2.What test was used is benzene, toluene, and the gaseous mixture of each 100ppm of dimethylbenzene, nitrogen are balance gas.(black) has not improved 7 times under the magnetic field condition than not adding to add nitrogen signal under the magnetic field condition and argon gas signal (redness), and benzene, toluene, the signal of dimethylbenzene is influenced hardly.This figure has proved the humidification of magnetic field to the photoelectron ionization by collision simultaneously.
With the running orbit of electronics and ion under the Simion analog magnetic field condition, the result as shown in Figure 3.The spiral movement locus of electronics clearly (green) as we can see from the figure, and ion does not have tangible spiral movement locus, and the influence that is subjected to magnetic field less (redness) is described.
Table 1 is the pluses and minuses comparative result of the present invention and electron impact ionization.
| The ionization source type | Structural information | Molecular ion peak | Operating air pressure | The detection of complex sample | Power consumption | Life-span | Oxidizing gas | The material that can be ionized | The ionization source type |
| The electron impact ionization source | Have | A little less than | 10 -4～10 -5Pa | Not | About 100W | 10 -4The about 2000h of Pa | Not | All | EI |
| The uviol lamp ionization source | Seldom | By force | Do not limit | Be | ＜0.3W | Under the 1mA operating current＞5000h | Be | Ionization energy is less than photon energy (10.6e V) | VUV |
| Electron collision and uviol lamp ionization source | Have | By force | Less than 1Pa | Not | ＜0.3W | Under the 1mA operating current＞5000h | Be | All | VUV+EI |
Ionization source among the present invention has two kinds of mode of operations, a kind of be ultraviolet light photo from pattern, another kind is ultraviolet light and electron impact ionization pattern, two kinds of patterns can be changed by voltage-regulation.Utilize of the effect of permanent magnetism permanent-magnetic focusing ring, make electronics, strengthened the electron collision probability, improved the detection sensitivity of electron impact ionization pattern along spiral motion to electronics.It is wide that the present invention has the testing sample scope, highly sensitive, low in energy consumption, and the life-span is long, and characteristics such as operating air pressure wide ranges are having broad application prospects aspect process monitoring and the analysis of organic pollution real-time online.
Claims (8)
1. ionization device of vacuum UV lamp is characterized in that: comprise an ionization chamber (2),
Vacuum UV lamp (1) as ionization source is installed above ionization chamber (2), is provided with a repeller plate (3) in distance vacuum UV lamp (1) beneath window,
Be provided with a permanent-magnetic focusing ring (5) under distance repeller plate (3), permanent-magnetic focusing ring (5) is the plectane of middle perforate, and coaxial with repeller plate (3);
Be provided with an aperture plate (7) under permanent-magnetic focusing ring (5), aperture plate (7) is the plectane of middle perforate, and coaxial with repeller plate (3);
The 1-4mm place is provided with coaxial three lens (8) under aperture plate (7), and is coaxial with repeller plate (3);
Being respectively equipped with the insulated enclosure pad between permanent-magnetic focusing ring (5), aperture plate (7) and lens (8) intercepts;
The sidewall of ionization chamber (2) is provided with and stretches into the inner sample introduction capillary (4) of ionization chamber (2);
Repeller plate (3), permanent-magnetic focusing ring (5), aperture plate (7) and lens (8) all be arranged on ionization chamber (2) inner and with the light shaft coaxle of vacuum UV lamp (1);
On ionization chamber (2) wall under the lens (8), have the hole, under the hole, be provided with a mass analyzer (9).
2. according to the described device of claim 1, it is characterized in that:
The inside of ionization chamber (2), between repeller plate (3) and permanent-magnetic focusing ring (5), form ionization chamber, sample introduction capillary (4) carries out ionization with the beneath window that gaseous sample is introduced vacuum UV lamp (1) front end from a side of ionization chamber, and the optical axis of vacuum UV lamp (1) is perpendicular with the sample introduction direction of gaseous sample.
3. according to the described device of claim 1, it is characterized in that: the sidewall of ionization chamber (2) is provided with pump interface (6).
4. according to the described device of claim 1, it is characterized in that: the voltage that on repeller plate (3), applies 1-100V; The voltage that applies on permanent-magnetic focusing ring (5) is 10～500% of repeller plate voltage.
5. according to the described device of claim 1, it is characterized in that: permanent-magnetic focusing ring (5) has 100-2000 Gauss's permanent magnet for the interstitial hole diameter is 2-20mm, and has electric conductivity;
Aperture plate (7) is 0.1mm-20mm for the aperture of middle perforate;
Being respectively equipped with the thick insulated enclosure pad of 0.1-10mm between permanent-magnetic focusing ring (5), aperture plate (7) and lens (8) intercepts.
6. according to the described device of claim 1, it is characterized in that: under vacuum ultraviolet ionized pattern, the voltage that applies on aperture plate (7) is 0～-20V.
7. according to the described device of claim 1, it is characterized in that: under vacuum-ultraviolet light and electron impact ionization pattern, the voltage that applies on aperture plate (7) is-10～-150V.
8. according to the described device of claim 1, it is characterized in that:
At distance vacuum UV lamp (1) beneath window 1-4mm place, ionization chamber (2) inside is provided with a repeller plate (3),
The 10-30mm place is provided with a permanent-magnetic focusing ring (5) under distance repeller plate (3), and permanent-magnetic focusing ring (5) is the plectane of middle perforate, and coaxial with repeller plate (3);
The 0.1-100mm place is provided with an aperture plate (7) under permanent-magnetic focusing ring (5), and aperture plate (7) is the plectane of middle perforate, and coaxial with repeller plate (3).
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009102654470A CN102103972B (en) | 2009-12-18 | 2009-12-29 | Vacuum ultraviolet lamp ionization device |
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| CN200910248566 | 2009-12-18 | ||
| CN200910248566.5 | 2009-12-18 | ||
| CN2009102654470A CN102103972B (en) | 2009-12-18 | 2009-12-29 | Vacuum ultraviolet lamp ionization device |
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| CN102103972B CN102103972B (en) | 2012-07-04 |
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| CN103854952A (en) * | 2012-11-30 | 2014-06-11 | 中国科学院大连化学物理研究所 | Mass spectrum vacuum ultraviolet ionization source based on optical-window-free gas discharge lamp |
| CN103871828A (en) * | 2012-12-17 | 2014-06-18 | 中国科学院大连化学物理研究所 | Array type photoelectric transmission ionizing source and application thereof |
| CN103887142A (en) * | 2012-12-21 | 2014-06-25 | 中国科学院大连化学物理研究所 | Discharge photoionization source in linear acceleration type flight time mass spectrum |
| CN103959427A (en) * | 2011-11-30 | 2014-07-30 | 安捷伦科技有限公司 | Ionization device |
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| CN104701129A (en) * | 2015-03-12 | 2015-06-10 | 广西电网有限责任公司电力科学研究院 | Device and method of inhibiting anions generated by low-energy photoelectron resonance ionization |
| CN105070630A (en) * | 2015-07-30 | 2015-11-18 | 安徽中杰信息科技有限公司 | Ionization device of self-cleaning two-dimensional flow type structure used for gas detection |
| CN106876243A (en) * | 2015-12-11 | 2017-06-20 | 中国科学院大连化学物理研究所 | One kind aids in low pressure vacuum ultraviolet light ionization source for mass spectrographic reagent molecule |
| CN111653470A (en) * | 2020-05-25 | 2020-09-11 | 清华大学深圳国际研究生院 | Ultraviolet lamp ionization source |
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| JP2006244717A (en) * | 2005-02-28 | 2006-09-14 | Mitsubishi Heavy Ind Ltd | Multi-element and multi-component simultaneous measuring device and method |
| CN100483130C (en) * | 2006-04-26 | 2009-04-29 | 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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| CN103959427A (en) * | 2011-11-30 | 2014-07-30 | 安捷伦科技有限公司 | Ionization device |
| CN103854952A (en) * | 2012-11-30 | 2014-06-11 | 中国科学院大连化学物理研究所 | Mass spectrum vacuum ultraviolet ionization source based on optical-window-free gas discharge lamp |
| CN103871828B (en) * | 2012-12-17 | 2016-05-18 | 中国科学院大连化学物理研究所 | A kind of array photoelectricity transmitting ionization source and application thereof |
| CN103871828A (en) * | 2012-12-17 | 2014-06-18 | 中国科学院大连化学物理研究所 | Array type photoelectric transmission ionizing source and application thereof |
| CN103887142A (en) * | 2012-12-21 | 2014-06-25 | 中国科学院大连化学物理研究所 | Discharge photoionization source in linear acceleration type flight time mass spectrum |
| CN103887142B (en) * | 2012-12-21 | 2016-03-16 | 中国科学院大连化学物理研究所 | Discharging light ionization source in a kind of linear accelerating type flight time mass spectrum |
| CN104144553A (en) * | 2014-08-11 | 2014-11-12 | 厦门大学 | Photoionization plasma generator |
| CN104701129A (en) * | 2015-03-12 | 2015-06-10 | 广西电网有限责任公司电力科学研究院 | Device and method of inhibiting anions generated by low-energy photoelectron resonance ionization |
| CN105070630A (en) * | 2015-07-30 | 2015-11-18 | 安徽中杰信息科技有限公司 | Ionization device of self-cleaning two-dimensional flow type structure used for gas detection |
| CN106876243A (en) * | 2015-12-11 | 2017-06-20 | 中国科学院大连化学物理研究所 | One kind aids in low pressure vacuum ultraviolet light ionization source for mass spectrographic reagent molecule |
| CN111653470A (en) * | 2020-05-25 | 2020-09-11 | 清华大学深圳国际研究生院 | Ultraviolet lamp ionization source |
| CN114361006A (en) * | 2022-01-11 | 2022-04-15 | 深圳市步锐生物科技有限公司 | Vacuum sealed ion source and mass spectrometer |
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