CN101063673A - Vacuumeultraviolet lamp ionization device in time-of-flight mass spectrometer - Google Patents
Vacuumeultraviolet lamp ionization device in time-of-flight mass spectrometer Download PDFInfo
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- CN101063673A CN101063673A CN 200610011793 CN200610011793A CN101063673A CN 101063673 A CN101063673 A CN 101063673A CN 200610011793 CN200610011793 CN 200610011793 CN 200610011793 A CN200610011793 A CN 200610011793A CN 101063673 A CN101063673 A CN 101063673A
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- 230000005684 electric field Effects 0.000 claims description 6
- 230000003287 optical effect Effects 0.000 claims description 4
- 238000001819 mass spectrum Methods 0.000 abstract description 4
- 238000002955 isolation Methods 0.000 abstract 2
- 230000001133 acceleration Effects 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Triiodomethane Natural products IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 description 7
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 150000001793 charged compounds Chemical class 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- -1 nitrogen and oxygen Chemical class 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000012113 quantitative test Methods 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 238000013523 data management Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005040 ion trap Methods 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 239000008031 plastic plasticizer Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 230000005477 standard model Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
This invention relates to one fly time mass spectrum vacuum ultraviolet isolation device, which comprises the following parts: one ionization chamber fixed with vacuum ultraviolet lamp as ion source; one ion repel electrode in one to four mm to the lamp window and earth electrode at ten to fifteen mm to the dispel electrode; ion repel electrode and earth connection electrode weak field acceleration ion electron for isolation; light exit hole with diameter as two to 8mm down the electrodes; one capillary to lead vacuum ultraviolet lamp front end with light axis vertical to gas sample in direction.
Description
Technical field
The invention belongs to mass spectrometer, volatile organic pollutant analysis time of-flight mass spectrometer in particularly a kind of miniature air utilizes this ionization technique further to improve the ionization scope of VUV photoionization.
Background technology
Waving property sends out organism and half volatile organic contaminant content in atmospheric environment is very low, but has pathogenic, carcinogenesis mostly, so organic pollutant monitoring is subjected to people always and pays close attention to widely.Traditional off-line analysis method since consuming time many, cost is high, can't satisfy present needs to air, water and other pollution source continuous monitoring.Some shortcomings and the limitation of off-line monitoring analytical technology have promoted the development of quick in the environmental monitoring, online and high-resolution field instrumentation detection and corresponding analysis method.Mass spectral universality is good, highly sensitive, and therefore quick, Sensitive Detection organic contaminant instrument much adopts mass spectrometer.The normal ionization method that adopts of online mass spectrum is the 70eV beam bombardment ionization (EI) that electron gun produces, portable gas chromatography/mass spectrometer (GC/MS) that American I nficon company releases, the portable mass spectrum of film sample introduction of the Kore Technology company of Britain, the miniature TOF-MS of Comstock company development all adopts the ionization mode of 70eV electron bombard.
EI electric vacuum degree requires high, thereby make the vacuum system complexity, it is a lot of to the most important thing is that the 70eV energy exceeds the ionization energy of compound itself, tend to produce a lot of fragmentions, influence the identification of parent ion, and a large amount of fragmentions can cover tested quasi-molecular ions, reduced the sensitivity of analyzing, for the difference of the ionizing efficiency of different compounds and the complicacy that the competition between the electric charge has also aggravated spectrogram.For the accuracy that guarantees to measure needs to combine with pre-separation means such as chromatogram, monitoring in real time remains in a lot of difficulties present in a word mass-spectrometric technique for the micro constitutent in the complex sample.The laser of 118nm (10.5eV), VUV laser intensity height, pulse are short, are well suited for doing the ionization source of TOF-MS, but instrument costs an arm and a leg, and bulky, therefore technical sophistication only adapts to and is used for laboratory study.Vacuum UV lamp low price with identity function, stable performance, vacuum tightness requires low, long working life (can reach 5000 hours), and be particularly suitable for moving mass spectral light ionization source.
A puzzlement VUV key factor of widespread use more is the photon numbers fewer (10 that generates in the vacuum UV lamp unit interval
10Photon/s), therefore use vacuum UV lamp ionization realize high-sensitivity detection must with separate or the beneficiation technologies coupling, such as chromatogram pre-separation, membrane sample enrichment, ion trap ion enrichment etc., employing electron resonances such as this Mulhlberger are excited multi-photon, strengthened the density of photon, photon numbers can reach 2.6 * 10
18Photon/s, detectability has reached 10ppm under the situation of enrichment not having, but the complicated cost height of this kind way technical scheme.
Summary of the invention
The object of the present invention is to provide vacuum ultraviolet in a kind of time of-flight mass spectrometer (VUV) lamp ionization device, device maneuverability of the present invention is good, can measure organic contaminant in the air fast.
For achieving the above object, ionization device of vacuum UV lamp in the time of-flight mass spectrometer provided by the invention, has an ionization chamber, vacuum UV lamp is installed as ionization source above ionization chamber, be provided with an ion repulsion electrode at distance vacuum UV lamp window 1～4mm place, the sub-repulsion electrode 10～15mm of distance place is provided with ground-electrode abreast;
Below ion repulsion electrode, ground-electrode and ionization chamber, be equipped with the light hole of diameter 2～8mm, these three apertures and the same optical axis of vacuum UV lamp;
One kapillary is introduced vacuum ultraviolet light modulation front end with gaseous sample from a side of ionization chamber and is carried out ionization, and the sample introduction direction of the optical axis of vacuum UV lamp and gaseous sample is vertical;
Utilize the weak electric field between ion repulsion electrode and the ground connection electroplax to quicken the electronics that photoionization produces in said apparatus, electronics and sample molecule with energy carry out electron impact ionization, improve the utilization ratio of photon.
Described ionization device of vacuum UV lamp, wherein vacuum ultraviolet light ionization source be positioned at ionization chamber directly over.
Described ionization device of vacuum UV lamp, outlet wherein capillaceous is 5～10mm apart from the vacuum UV lamp center line.
Described ionization device of vacuum UV lamp, internal diameter wherein capillaceous is 0.2～0.5mm.
Described ionization device of vacuum UV lamp, its intermediate ion repulsion electrode making alive 40～75V.
Described ionization device of vacuum UV lamp, wherein the opposite side of ionization chamber is provided with mechanical pump.
Thus, the present invention utilizes the photoelectric effect of metal, makes VUV light direct irradiation on metallic surface, utilizes weak electric field to quicken the electronics that photoelectric effect produces, the electron bombard sample molecule carries out ionization, and the utilization ratio that has effectively improved photon makes sensitivity further improve.Simple VUV lamp soft ionization is had to the molion of analytic sample, structure of the present invention, the electronics that is accelerated can the original VUV lamp of ionization can not ionization compound, such as nitrogen and oxygen, the energy of ionization is quickened in control also can realize soft ionization, thereby make in the resulting spectrogram all are molecular ion peaks, spectrogram simply can carry out fast qualitative or quantitative test according to molecular weight.
Description of drawings
Fig. 1 is an ionization device of vacuum UV lamp synoptic diagram of the present invention.
Synoptic diagram when Fig. 2 is device of the present invention and portable mass spectrometer coupling.
Fig. 3 is the benzene spectrogram comparison diagram of electron collision (EI) and vacuum ultraviolet ionized (VUV), and wherein (a) is the benzene spectrogram of electron collision, (b) is vacuum ultraviolet ionized benzene spectrogram
Fig. 4 is the biased sample spectrogram of acetone, benzene,toluene,xylene and iodomethane.
Fig. 5 has shown that the actual detected limit of iodomethane, benzene is respectively 10,20ppm, and wherein (a) is iodomethane, (b) be benzene.
Embodiment
The present invention has adopted kapillary constraint sample diffusion in ionization chamber, sample is introduced directly into the vacuum UV lamp front end, carry out vertical ionization with vacuum UV lamp, vacuum ultraviolet light modulation front end making alive 40～75V, with ground-electrode distance 10～15mm, weak electric field between the two-plate can quicken the electronics that photoionization produces, and the sub-direct irradiation of VUV light metal surface also is accelerated by the electronics that photoelectric effect produces simultaneously, and electronics and sample molecule with certain energy carry out electron impact ionization.VUV lamp soft ionization is had to the molion of analytic sample, utilize structure of the present invention, the electronics that is accelerated can the original VUV lamp of ionization can not ionization compound, such as nitrogen and oxygen, the energy of ionization is quickened in control also can realize soft ionization, improve the utilization ratio of photon from the side, further improved sensitivity.All are molecular ion peaks in the resulting spectrogram, spectrogram simply can carry out fast qualitative or quantitative test according to molecular weight.Thereby can be by the low-down organic contaminant composition of content in the mass spectrometer fast detecting air.
See also Fig. 1, at ionization chamber in order effectively to prevent the sample gas diffusion in the vacuum cavity again, adopted internal diameter 0.2～0.5mm kapillary 1 directly the front end that sample is incorporated into VUV lamp 2 to be carried out ionization, the kapillary front end is controlled at about 2～10mm apart from the central shaft of VUV lamp.
Adopt the ionization of VUV lamp to mainly contain following two characteristics in the experiment:
A) to adopt the magnesium chloride window to be merely able to see through energy be the photon of 10.6eV to the VUV lamp, powerless less than the sample molecule of 10.6eV for ionization energy, can effectively suppress the component (N of content more than 99.99% in the air
2, O
2, H
2O, CO
2Deng) signal that produces disturbs, and can realize that for the organism of tested trace selectivity detects.
B) can be with narrowly, the fragment ion of generation is few, because the energy of photon has just surpassed the critical ionization energy of sample molecule, there is not unnecessary energy to generate fragmention, spectrogram is simple, is the comparison of electron impact ionization (EI) Yu the VUV ionization spectrogram of benzene as Fig. 3, and the latter's spectrogram is simple far beyond the former.Can carry out qualitative and quantitative analysis fast according to molecular weight.
The photon energy of VUV lamp emission is 10.6eV, powerless for ionization energy greater than the compound of 10.6eV, the structure of VUV lamp ionization chamber of the present invention is transformed, vacuum ultraviolet light modulation front end electrode making alive 40～75V, with ground-electrode distance 10～15mm, weak electric field between the two-plate can quicken the electronics that photoionization produces, the sub-direct irradiation of VUV light metal surface also is accelerated by the electronics that photoelectric effect produces simultaneously, electronics and sample molecule with certain energy carry out electron impact ionization, VUV lamp soft ionization is had to the molion of analytic sample, and the electronics that the present invention is accelerated can the original VUV lamp of ionization can not ionization compound, such as nitrogen and oxygen, the energy of ionization is quickened in control also can realize soft ionization, and realized that ionization energy is higher than the ionization of 10.6eV, improve the utilization ratio of photon from the side, further improved sensitivity.All are molecular ion peaks in the resulting spectrogram, spectrogram simply can carry out fast qualitative or quantitative test according to molecular weight.Thereby can be by micro quantity organic pollutant composition in the mass spectrometer fast detecting air.
Please in conjunction with Fig. 2, the synoptic diagram of device of the present invention and minitype flight time mass spectrum coupling.This time of flight mass analyzer adopts ion vertically to introduce method, adopts two electric fields once to focus in the vertical drawing-in system, and the field-free flight district adopts negative high voltage, three MCP receiving poles.The vacuum system of this time of-flight mass spectrometer adopts molecular pump and the forepump of 110L/s to keep.Ionization chamber vacuum tightness is 10^-5Torr, compares VUV with the electron gun electron ionization and is adapted at more moving under the low vacuum, has effectively reduced the burden of vacuum in the system, thereby lays a good foundation for the miniaturization of instrument.The forepump of molecular pump is the mechanical pump of 4L/s.
The ion that generates is quickened to earthy electrode 4 by the low electrostatic field that electrode 3 generates, sample ions is quickened to advance by one-level slit 5, then through vertically entering the pulse accelerating region of time of flight mass analyzer behind the 2mm aperture, arrive detector at last through accelerating field, from detector simulating signal is received on the high-speed data acquisition card, obtained the kind and the content of pollutant through Data Management Analysis.
Fig. 4 is a kind of acetone, benzene,toluene,xylene and iodomethane mixing organic sample, has occurred 28,32,119,149 and 223,279 Interference Peaks in the spectrogram, wherein 28,32 and 149 is respectively nitrogen, oxygen and plastic plasticizer.The peak that the ionization of VUV lamp obtains nitrogen and oxygen is that photoionization produces in the ionization chamber structure photoelectron quickens to obtain certain energy and (is 40～75V) to the maximum and bombards nitrogen, oxygen molecule gained in the weakness field, 149 peaks are because system heating causes that plastifier enters due to the system in the O circle, and 119,223 and 279 may be the returning due to the oil vapour of VUV lamp ionization mechanical pump.
There is not to adopt relevant enrichment measure in this instrument, but adopted direct atmosphere sample introduction, calibrating gas has adopted the calibrating gas of the acetone 20ppm of Dalian Da Te gas company limited production, benzene and iodomethane calibrating gas are respectively 100ppm, 50ppm, the dilution that utilizes the quality control flowmeter to carry out five times for the standard model of benzene and iodomethane obtains 20ppm, 10ppm, analyzes signal such as Fig. 5 of obtaining.Present as can be seen from Figure 5 signal to noise ratio (S/N ratio) is 6: 1, carry out Theoretical Calculation at 3: 1 according to signal to noise ratio (S/N ratio), lowest detectable limit is 5ppm for iodomethane so, benzene is 10ppm, it is similar substantially to utilize employing electron resonances such as sensitivity that this kind ionization mode obtains and Mulhlberger to strengthen the result that light obtains, and has proved absolutely the superiority of this method.
Claims (6)
1. ionization device of vacuum UV lamp in the time of-flight mass spectrometer, has an ionization chamber, vacuum UV lamp is installed as ionization source above ionization chamber, be provided with an ion repulsion electrode at distance vacuum UV lamp window 1～4mm place, the sub-repulsion electrode 10～15mm of distance place is provided with ground-electrode abreast;
Below ion repulsion electrode, ground-electrode and ionization chamber, be equipped with the light hole of diameter 2～8mm, these three apertures and the same optical axis of vacuum UV lamp;
One kapillary is introduced vacuum ultraviolet light modulation front end with gaseous sample from a side of ionization chamber and is carried out ionization, and the sample introduction direction of the optical axis of vacuum UV lamp and gaseous sample is vertical;
Utilize the weak electric field between ion repulsion electrode and the ground connection electroplax to quicken the electronics that photoionization produces in said apparatus, electronics and sample molecule with energy carry out electron impact ionization, improve the utilization ratio of photon.
2. ionization device of vacuum UV lamp according to claim 1, wherein vacuum ultraviolet light ionization source be positioned at ionization chamber directly over.
3. ionization device of vacuum UV lamp according to claim 1, outlet wherein capillaceous is 5～10mm apart from the vacuum UV lamp center line.
4. ionization device of vacuum UV lamp according to claim 1, internal diameter wherein capillaceous is 0.2～0.5mm.
5. ionization device of vacuum UV lamp according to claim 1, its intermediate ion repulsion electrode making alive 40～75V.
6. ionization device of vacuum UV lamp according to claim 1, wherein the opposite side of ionization chamber is provided with mechanical pump.
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