CN102117728B - Mass spectrum VUV (Vacuum Ultraviolet) photoionization source device for in-source collision induced dissociation - Google Patents
Mass spectrum VUV (Vacuum Ultraviolet) photoionization source device for in-source collision induced dissociation Download PDFInfo
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- 238000001819 mass spectrum Methods 0.000 title claims abstract description 26
- 238000001360 collision-induced dissociation Methods 0.000 title claims abstract description 14
- 150000002500 ions Chemical class 0.000 claims description 111
- 239000007789 gas Substances 0.000 claims description 39
- 230000005684 electric field Effects 0.000 claims description 27
- 239000012159 carrier gas Substances 0.000 claims description 5
- 230000001846 repelling effect Effects 0.000 abstract 4
- 238000005086 pumping Methods 0.000 abstract 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 20
- 239000012634 fragment Substances 0.000 description 16
- 150000001793 charged compounds Chemical class 0.000 description 15
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 14
- 239000000126 substance Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000004451 qualitative analysis Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 150000005194 ethylbenzenes Chemical class 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
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- 231100000419 toxicity Toxicity 0.000 description 1
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Abstract
The invention relates to a mass spectrum analyzer, in particular to a mass spectrum VUV (Vacuum Ultraviolet) photoionization source device for in-source collision induced dissociation, which comprises a sample injecting capillary tube, an ion repelling electrode, an ion accelerating electrode, a vacuum ultraviolet lamp, a side pumping valve and an ionization source cavity, wherein the ion repelling electrode and the ion accelerating electrode are placed in the ionization source cavity at interval in parallel, the sample injecting capillary tube passes through the outer wall of the ionization source cavity, and one end of the sample injecting capillary tube is arranged in a central small hole of the ion repelling electrodes; a light emitting window of the vacuum ultraviolet lamp is placed opposite to a gap between the ion repelling electrode and the ion accelerating electrode; and an air outlet is arranged on the side wall of the ionization source cavity, and the side pumping valve is connected with the air outlet through a pipeline. The mass spectrum VUV photoionization source device can be used together with any types of quality analyzers, can simultaneously obtain the molecular weight and the structural information of a matter to be analyzed and also be used for rapidly distinguishing isomerides by utilizing in-source collision induced dissociation.
Description
Technical field
The present invention relates to mass spectrometer, the mass spectrum VUV light ionization source device of collision induced dissociation in the provenance specifically, that the ion that the VUV photo ionization produces is accelerated under suitable ionization source electric field, bump to induce with background gas under certain ionization source air pressure and dissociate, can obtain simultaneously the molecular weight of material to be analyzed and the device of structural information, and be applied to the quick resolution of isomer.
Background technology
The organic pollution of volatility, the half volatile usually content in environment is very low, but it has toxicity, excitant and carcinogenicity, human body is caused various acute and chronic infringements, therefore the monitoring of various organic pollutions in the environment has been subject to people's close attention, and has been studied widely.Mass spectrum is highly sensitive with it, detection speed is fast, universality good, and qualitative, quantitative characteristics accurately, environmental sample fast, more and more adopted as Site Detection instrument and analytical method in the on-line analysis.Ionization source commonly used in the on-line mass spectroscopy is the electron impact ionization source (EI) with 70eV energy, and this ionization source has its feature spectrogram, accurately qualitative analysis for every kind of organic substance.But EI has relatively high expectations to vacuum in the source, makes vacuum system complicated, produces more fragment peak during its ionization organic substance, and the identification of spectrogram difficulty has restricted its development when the Analysis of Complex mixture.
In order to reduce the spectrum unscrambling difficulty, accelerate analysis speed, Hou Keyong [Chinese invention patent: 200610011793.2] and Zheng Peichao [Chinese invention patent: 200810022557.X] use VUV light as the mass spectrum ionization source, have to organic molecular ion peak when measuring organic substance, spectrogram is simple, can carry out fast qualitative and quantitative analysis according to molecular weight.But the photon energy of this vacuum-ultraviolet light only has tens eV, can only obtain its molecular ion peak for most organic substances, can't obtain the abundant structural information of organic substance, and is then helpless to the resolution of isomer, qualitative accurate not.
Summary of the invention
The object of the present invention is to provide the mass spectrum VUV light ionization source device of collision induced dissociation in the provenance, can obtain simultaneously molecular weight and the structural information of sample, can be used for the quick resolution of isomer.
For achieving the above object, the technical solution used in the present invention is:
The mass spectrum VUV light ionization source device of collision induced dissociation comprises vacuum UV lamp and ionization source cavity in one provenance,
The ultraviolet light that vacuum UV lamp sends is positioned at the inside of ionization source cavity, the light path both sides of the ultraviolet light that sends at ionization source inside cavity, vacuum UV lamp are respectively arranged with ion repulsion electrode and ion accelerating electrode, ion repulsion electrode and ion accelerating electrode space, coaxial, be arranged in parallel;
Ion repulsion electrode is plank frame, and its centre is provided with aperture, and a sample introduction capillary passes the outer wall of ionization source cavity, and sample introduction gas outlet end capillaceous inserts in the aperture, and sample introduction gas access capillaceous links to each other with the carrier gas source of the gas with the sample source of the gas;
The plank frame that the ion accelerating electrode is 1 or 1 above space, be arranged in parallel; Aperture with respect to the centre of ion repulsion electrode is equipped with the sample ions through hole on the flat board of ion accelerating electrode;
Be provided with gas vent on the ionization source cavity wall, gas vent is taken out valve by vacuum line with a side and is linked to each other, and the other end of taking out valve in side is connected with oil-sealed rotary pump by vacuum line.
Place in the light emission windows of vacuum UV lamp zone under ion repulsion electrode centers aperture; Vacuum UV lamp institute emissioning light is by under the central small hole of ion repulsion electrode; The sample introduction capillary tube gas exports on the light path of the ultraviolet light that sends perpendicular to vacuum UV lamp.
Be provided with the differential interface pole plate in the ion accelerating electrode away from an end of ion repulsion electrode, differential interface pole plate and ion accelerating electrode space, parallel placement, with respect to the ion through hole on the ion accelerating electrode flat board, on the differential interface pole plate, be provided with the differential interface aperture, the differential interface aperture links to each other with mass spectrometric mass analyzer, and the ion that namely gaseous sample ionization obtains in the ionization source cavity is introduced directly in the mass spectrometer by the differential interface aperture on the differential interface pole plate.
Mass analyzer can be the mass analyzer of any type, such as (being such as but not limited to) time of flight mass analyzer, level Four bar mass analyzer, ion strap mass analyzer etc.; It is the adjustable vacuum valve of flow that side is taken out valve, such as (being such as but not limited to) vacuum flapper valve, vacuum butterfly valve, vacuum needle-valve etc.;
Ion through hole and the differential interface aperture at the central small hole of ion repulsion electrode, ion accelerating electrode center are on the same axis.
Ion repulsion electrode is 0.2~20cm to the distance between the differential interface pole plate; On ion repulsion electrode, ion accelerating electrode and differential interface pole plate according to voltage order from high to low, load successively different voltage, form evenly or inhomogeneous field at ion repulsion electrode, ion accelerating electrode and differential interface pole plate central axis place, electric field strength is adjustable at 0V/cm~100V/cm.
On the ionization source cavity wall, have through hole, be connected with vacuum gauge by vacuum line.
Can take out the adjusting of valve flow and sample size is controlled in the change of sample introduction capillary inner diameter and length according to side, regulate the vacuum degree in the ionization source cavity, the sample introduction capillary inner diameter is Φ 50~530 μ m, length is 5~200cm, the gas sample introduction amount is 0.1~100ml/min, and the vacuum degree in the ionization source cavity maintains 10
-3Torr~10Torr.
Vacuum UV lamp is arranged at the inside of ionization source cavity, and perhaps vacuum UV lamp is arranged at the outside of ionization source cavity, and the sidewall at the ionization source cavity arranges light incident aperture simultaneously, and the light emission windows of vacuum UV lamp is right against this light incident aperture.
Mass spectrum VUV light ionization source device provided by the invention, by with mass spectral:mass spectrographic mass analyzer coupling, can obtain simultaneously molecular weight and the structural information of test substance, and can realize the quick resolution to isomer.Apparatus of the present invention use capillary directly the sample gas in the atmospheric environment to be incorporated in the ionization source cavity, organic pollution in the sample gas is ionized under the irradiation of VUV light, produce the organic molecule ion, the mass analyzer that these molecular ions enter behind the ionization source obtains organic molecular weight information.Take out valve and sample introduction capillary control gas sample introduction amount by side, regulate the vacuum degree in the ionization source cavity, the organic molecule ion that the VUV photo ionization produces is under the acceleration of the ionization source electric field of certain field intensity, obtain enough energy, bumping with background gas in the ionization source, inducing dissociates produces the organic substance fragment ion, thereby obtains organic structural information.According to the difference that isomer dissociates energy, under suitable ionization source field intensity and air pressure conditions, the molecular ion peak of different isomers is different with the relative intensity of fragment peak, therefore, can realize the quick resolution to isomer.The package unit volume is small and exquisite, applying flexible, after the coupling of different quality analyzer, can realize fast, accurately qualitative analysis of environmental organic pollutant, quantitatively accurately, has broad application prospects in the on-line monitoring field of environmental pollution.
Description of drawings
Fig. 1 is mass spectrum VUV light ionization source apparatus structure schematic diagram of the present invention.
Fig. 2 is the mass spectrogram that the normal heptane sample obtains under identical ionization source air pressure, different ionization source electric field strength among the embodiment 1.
Fig. 3 is the mass spectrogram that the normal heptane sample obtains under identical ionization source electric field strength, different ionization source air pressure among the embodiment 1.
Fig. 4 is the mass spectrogram that dimethylbenzene sample and ethylbenzene sample obtain under identical ionization source air pressure, different ionization source electric field strength among the embodiment 2.
Fig. 5 be among the embodiment 2 dimethylbenzene sample and ethylbenzene sample under the same conditions the proportionate relationship of collision induced dissociation degree size with the change curve of ionized region electric field strength.
Embodiment
See also Fig. 1, be structural representation of the present invention, 12 is gaseous sample among the figure, and 13 is VUV light.Mass spectrum VUV light ionization source device of the present invention, by sample introduction capillary 1, ion repulsion electrode 2, ion accelerating electrode 3, differential interface pole plate 4, vacuum UV lamp 6, side take out valve 7, ionization source cavity 9 consists of.
Vacuum UV lamp 6 is positioned at the inside of ionization source cavity 9, and (perhaps vacuum UV lamp is arranged at the outside of ionization source cavity 9, sidewall at ionization source cavity 9 arranges light incident aperture simultaneously, the light emission windows of vacuum UV lamp 6 is right against this light incident aperture), the light path both sides of the ultraviolet light that sends at ionization source cavity 9 inside, vacuum UV lamp 6 are symmetrically arranged with respectively ion repulsion electrode 2 and ion accelerating electrode 3, ion repulsion electrode 2 and ion accelerating electrode 3 spaces, coaxial, be arranged in parallel;
The plank frame that ion accelerating electrode 3 is 3 above spaces, be arranged in parallel; Aperture with respect to the centre of ion repulsion electrode 2 is equipped with the sample ions through hole on the flat board of ion accelerating electrode 3;
Be provided with gas vent on ionization source cavity 9 sidewalls, gas vent is taken out valve 7 by vacuum line and a side and is linked to each other, and the other end of taking out valve 7 in side is connected with oil-sealed rotary pump 8 by vacuum line.
On the light path of the ultraviolet light that sample introduction capillary 1 gas vent sends perpendicular to vacuum UV lamp (6).
Be provided with differential interface pole plate 4 in ion accelerating electrode 3 away from an end of ion repulsion electrode 2, differential interface pole plate 4 and ion accelerating electrode 3 spaces, parallel placement, with respect to the ion through hole on ion accelerating electrode 3 flat boards, on differential interface pole plate 4, be provided with differential interface aperture 5, differential interface aperture 5 links to each other with mass spectrometric mass analyzer 10, i.e. the ion that ionization source cavity 9 interior gaseous sample ionization obtain is introduced directly in the mass spectrometer 10 by the differential interface aperture 5 on the differential interface pole plate 4.
Ion through hole and the differential interface aperture 5 at the central small hole of ion repulsion electrode 2, ion accelerating electrode 3 centers are on the same axis.
Be specially:
One sample introduction capillary is used for atmospheric environment gaseous sample direct injected, and it passes the outer wall of an ionization source cavity, and an end is visited in the central small hole of an ion repulsion electrode, and the sample introduction capillary inner diameter is Φ 50~530 μ m, and length is 5~200cm;
One side is taken out valve and is linked to each other by the gas vent that arranges on vacuum line and the ionization source cavity wall, and it is the adjustable vacuum valve of flow that side is taken out valve; Can take out the adjusting of valve flow and sample size is controlled in the change of sample introduction capillary inner diameter and length according to side, regulate the vacuum degree in the ionization source cavity, the gas sample introduction amount is 0.1~100ml/min, and the vacuum degree in the ionization source cavity maintains 10
-3Torr~10Torr.
One differential interface pole plate, an ion accelerating electrode and ion repulsion electrode are spaced a distance successively and are placed in parallel in the ionization source inside cavity, and ion repulsion electrode is 0.2~20cm to the distance between the differential interface pole plate; On ion repulsion electrode, ion accelerating electrode and differential interface pole plate according to voltage order from high to low, load successively different voltage, form evenly or inhomogeneous field at ion repulsion electrode, ion accelerating electrode and differential interface pole plate central axis place, electric field strength is adjustable at 0V/cm~100V/cm.
One vacuum UV lamp, the VUV light of emission is used for ionized sample γ-ray emission organic molecule ion, place in its light emission windows zone under ion repulsion electrode centers aperture, and the VUV light that vacuum UV lamp is launched is by under the central small hole of ion repulsion electrode.
During application, side in the mass spectrum VUV light ionization source device of the present invention is taken out valve 7 (the adjustable vacuum flapper valve of flow) rear end and is connected with oil-sealed rotary pump 8 by vacuum line, ionization source cavity 9 interior unnecessary gases are taken out valve 7 via side and are extracted out by oil-sealed rotary pump 8, thereby keep air pressure in the ionization source cavity 9 at suitable numerical value; Vacuum gauge 11 is connected to the through hole that arranges on the sidewall of ionization source cavity 9 by vacuum line, in order to measure the air pressure numerical value of ionization source cavity 9 inside; Ionization source cavity 9 links to each other with mass spectrometric mass analyzer 10 (time of flight mass analyzer) by the differential interface aperture 5 on the differential interface pole plate 4.
Wherein:
One end of sample introduction capillary 1 is arranged in the atmospheric environment of ionization source cavity 9 outsides, and the other end is visited in the central small hole of the ion repulsion electrode 2 of ionization source cavity 9 inside.During sample introduction, gaseous sample enters into ionized space by atmospheric environment under the driving of ionization source cavity 9 inside and outside differential pressures, the VUV photo ionization of being launched by vacuum UV lamp 6 by the sample gas of ion repulsion electrode 2 central small hole ejections, produce the molecular ion of sample, unnecessary gas molecule is taken out valve 7 via side and is extracted out by oil-sealed rotary pump 8, Pneumatic pipe cleaners in the ionization source cavity 9 are crossed regulating and controlling that offside takes out valve 7 flows to suitable numerical value, and vacuum values is measured by the vacuum gauge 11 with ionization source cavity 9 internal communication.
At first, on ion repulsion electrode 2, ion accelerating electrode 3 and differential interface pole plate 4 according to voltage order from high to low, load successively different low-voltages, so, form weak electric field even or heterogeneous at ion repulsion electrode 2, ion accelerating electrode 3 and differential interface pole plate 4 central axis places.The sample molecule ion that the VUV photo ionization produces enters into mass analyzer 10 via the differential interface aperture 5 on the differential interface pole plate 4 under the repulsion of ion repulsion electrode 2 lower end weak electric fields, obtain the molecular ion peak-to-peak signal of testing sample.
Then, the fixing air pressure of ionization source cavity 9 inside, increase ion repulsion electrode 2, institute's making alive on ion accelerating electrode 3 and the differential interface pole plate 4, form highfield 2 times at ion repulsion electrode, the sample molecule ion that the VUV photo ionization produces accelerates under the 2 lower end highfield effects of ion repulsion electrode, obtaining the sample molecule ion of enough kinetic energy and the background gas in the ionization source cavity 9 constantly collides, produce collision induced dissociation, form the fragment ion of sample, it is detected that these fragment ions enter into mass analyzer 10 by differential interface aperture 5, obtains the fragment peak signal of testing sample.
Equally, the fixing electric field strength of repulsion electrode 2 lower ends, reduce the air pressure of ionization source cavity 9 inside by the internal diameter of sample introduction capillary 1 and the change of length or the adjusting that side is taken out the flow of valve 7, then the mean free path of ion increases, ion can obtain equally enough kinetic energy and produce collision induced dissociation under the acceleration of electric field, obtain the fragment peak signal of testing sample.
Isomer is owing to its structure is different, the size of its dissociation energy is not quite similar, air pressure in the adjusting ionization source cavity 9 and field intensity are to suitable numerical value, the degree that collision induced dissociation occurs under identical condition so different isomers is different, the molecular ion peak that obtains is different with the relative intensity of fragment peak, thereby realizes the quick resolution of isomer.
Embodiment 1
Examination for collision induced dissociation effect in the source of mass spectrum VUV light ionization source device of the present invention, use normal heptane sample configuration 100ppm sample gas to detect, carrier gas is 99.999% high pure nitrogen, and mass analyzer adopts the time of flight mass analyzer.Regulate the interior air pressure of ionization source cavity to 0.15Torr, remain unchanged, increase gradually the electric field strength of ion repulsion electrode lower end, the normal heptane mass signal that records under different electric field strength as shown in Figure 2.As seen the electric field strength a little less than is (such as the 2V/cm among Fig. 2, but be not limited to 2V/cm, decide on ionization source cavity internal gas pressure size) under, ion in the ionization source mainly is the sample molecule ion that is produced by the VUV photo ionization, the spectrogram that obtains is simple, can carry out fast qualitative and quantitative analysis according to molecular weight.Along with the increase of electric field strength, the molecular ion of sample accelerates the kinetic energy that obtains under electric field increasing, with the collision of the background gas nitrogen of neutrality after, bump to induce and dissociate, the fragment peak of sample appears.When ionization source electric field strength increases to certain numerical value (such as the 14V/cm among Fig. 2, but be not limited to 14V/cm, decide on ionization source cavity internal gas pressure size) after, the molecular ion of most samples all is dissociated into fragment ion, can analyze accordingly, obtain the structural information of sample.
Equally, regulate ion repulsion electrode lower end electric field strength to 4V/cm, remain unchanged, the air pressure of ionization source inside cavity is regulated in the control of the flow of taking out valve by change or the side of sample introduction internal diameter capillaceous and length, also can obtain simultaneously molecular ion peak and the fragment peak information of sample, as shown in Figure 3.
The examination of differentiating fast the isomer performance for mass spectrum VUV light ionization source device of the present invention, the example that is distinguished as with dimethylbenzene and ethylbenzene isomer, 100ppm dimethylbenzene and the 100ppm ethylbenzene standard sample gas prepared respectively take 99.999% high pure nitrogen as carrier gas detect, and mass analyzer adopts the time of flight mass analyzer.In the measuring process, keep the air pressure in the ionization source cavity constant at 0.15Torr, under identical sampling condition, the dimethylbenzene that records and the ethylbenzene mass spectrogram when different ionization source electric field strength as shown in Figure 4.Can find out, increase along with ionization source electric field strength, the m/z106 molecular ion of dimethylbenzene and ethylbenzene all can produce the m/z91 fragment ion by collision induced dissociation in the source, but the dissociation degree of the two is different under identical ionization source electric field strength, in Fig. 4, when electric field strength is 22V/cm, the ratio of the m/z91 fragment peak of dimethylbenzene and the peak intensity of m/z106 molecular ion peak is 0.67, the ratio of the m/z91 fragment peak of ethylbenzene and the peak intensity of m/z106 molecular ion peak is 5.31, the two differs a nearly magnitude, can realize the resolution of dimethylbenzene and ethylbenzene isomer fully, by the optimal control of computer to ionization source electric field strength, whole analytic process can be finished within 1 minute.
Fig. 5 is that the proportionate relationship of intensity ratio of the molecular ion peak m/z106 of the intensity ratio of the molecular ion peak m/z106 of dimethylbenzene and fragment peak m/z91 and ethylbenzene and fragment peak m/z91 is with the variation tendency of ionization source electric field strength.As seen from the figure, under certain ionization source cavity air pressure conditions, choose suitable ionization source electric field strength and can well differentiate dimethylbenzene and ethylbenzene isomer.
Claims (10)
1. the mass spectrum VUV light ionization source device of collision induced dissociation in the provenance comprises vacuum UV lamp (6), ionization source cavity (9), it is characterized in that:
The ultraviolet light that vacuum UV lamp (6) sends is positioned at the inside of ionization source cavity (9), the light path both sides of the ultraviolet light inner at ionization source cavity (9), that vacuum UV lamp (6) sends are respectively arranged with ion repulsion electrode (2) and ion accelerating electrode (3), ion repulsion electrode (2) and ion accelerating electrode (3) space, coaxial, be arranged in parallel;
Ion repulsion electrode (2) is plank frame, its centre is provided with aperture, one sample introduction capillary (1) passes the outer wall of ionization source cavity (9), the gas outlet end of sample introduction capillary (1) inserts in the aperture, and the gas access of sample introduction capillary (1) links to each other with the carrier gas source of the gas with the sample source of the gas;
The plank frame that ion accelerating electrode (3) is 1 or 1 above space, be arranged in parallel; Aperture with respect to the centre of ion repulsion electrode (2) is equipped with the sample ions through hole on the flat board of ion accelerating electrode (3);
Be provided with gas vent on ionization source cavity (9) sidewall, gas vent is taken out valve (7) by vacuum line and a side and is linked to each other, and the other end of taking out valve (7) in side is connected with oil-sealed rotary pump (8) by vacuum line.
2. mass spectrum VUV light ionization source device according to claim 1 is characterized in that:
Place in the light emission windows of vacuum UV lamp (6) zone under ion repulsion electrode (2) central small hole; Vacuum UV lamp (6) institute emissioning light is by under the central small hole of ion repulsion electrode (3); On the light path of the ultraviolet light that sample introduction capillary (1) gas vent sends perpendicular to vacuum UV lamp (6).
3. mass spectrum VUV light ionization source device according to claim 1 is characterized in that:
Be provided with differential interface pole plate (4) in ion accelerating electrode (3) away from an end of ion repulsion electrode (2), differential interface pole plate (4) and ion accelerating electrode (3) space, parallel placement, with respect to the ion through hole on ion accelerating electrode (3) flat board, on differential interface pole plate (4), be provided with differential interface aperture (5), differential interface aperture (5) links to each other with mass spectrometric mass analyzer (10), i.e. the ion that the interior gaseous sample ionization of ionization source cavity (9) obtains is introduced directly in the mass spectrometer (10) by the differential interface aperture (5) on the differential interface pole plate (4).
4. mass spectrum VUV light ionization source device according to claim 1 is characterized in that:
Ion through hole and the differential interface aperture (5) at the central small hole of ion repulsion electrode (2), ion accelerating electrode (3) center are on the same axis.
5. mass spectrum VUV light ionization source device according to claim 1 is characterized in that:
Ion repulsion electrode (2) is 0.2~20cm to the distance between the differential interface pole plate (4).
6. mass spectrum VUV light ionization source device according to claim 3 is characterized in that:
Described mass analyzer (10) is time of flight mass analyzer, level Four bar mass analyzer or ion strap mass analyzer;
It is the adjustable vacuum valve of flow that side is taken out valve (7), is vacuum flapper valve, vacuum butterfly valve or vacuum needle-valve.
7. mass spectrum VUV light ionization source device according to claim 1 is characterized in that:
Upper according to voltage order from high to low in ion repulsion electrode (2), ion accelerating electrode (3) and differential interface pole plate (4), load successively different voltage, form evenly or inhomogeneous field at ion repulsion electrode (2), ion accelerating electrode (3) and differential interface pole plate (4) central axis place, electric field strength is adjustable at 0V/cm~100V/cm.
8. mass spectrum VUV light ionization source device according to claim 1 is characterized in that:
On ionization source cavity (9) sidewall, have through hole, be connected with vacuum gauge (11) by vacuum line.
9. mass spectrum VUV light ionization source device according to claim 1 is characterized in that:
Can take out the adjusting of valve (7) flow and sample size is controlled in the change of sample introduction capillary (1) internal diameter and length according to side, regulate the vacuum degree in the ionization source cavity (9), sample introduction capillary (1) internal diameter is Φ 50~530 μ m, length is 5~200cm, the gas sample introduction amount is 0.1~100ml/min, and the vacuum degree in the ionization source cavity (9) maintains 10
-3Torr~10Torr.
10. mass spectrum VUV light ionization source device according to claim 1 is characterized in that:
Vacuum UV lamp (6) is arranged at the inside of ionization source cavity (9), perhaps vacuum UV lamp is arranged at the outside of ionization source cavity (9), sidewall at ionization source cavity (9) arranges light incident aperture simultaneously, and the light emission windows of vacuum UV lamp (6) is right against this light incident aperture.
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CN114973899B (en) * | 2022-06-02 | 2023-08-29 | 中国科学院合肥物质科学研究院 | Simulation device for electronic excitation of atmospheric radiation |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN101149326A (en) * | 2006-09-21 | 2008-03-26 | 中国科学院生态环境研究中心 | Vacuum ultraviolet ionized aerosol mass spectrometer |
CN101339161A (en) * | 2008-08-15 | 2009-01-07 | 中国科学院安徽光学精密机械研究所 | Multi- wavelength vacuum ultraviolet light ionization source for mass spectrum and ion transfer spectrum device |
-
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Patent Citations (3)
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---|---|---|---|---|
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 |
CN101149326A (en) * | 2006-09-21 | 2008-03-26 | 中国科学院生态环境研究中心 | Vacuum ultraviolet ionized aerosol mass spectrometer |
CN101339161A (en) * | 2008-08-15 | 2009-01-07 | 中国科学院安徽光学精密机械研究所 | Multi- wavelength vacuum ultraviolet light ionization source for mass spectrum and ion transfer spectrum device |
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