CN203242599U - Vacuum ultraviolet light ionization source - Google Patents

Vacuum ultraviolet light ionization source Download PDF

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Publication number
CN203242599U
CN203242599U CN 201320292993 CN201320292993U CN203242599U CN 203242599 U CN203242599 U CN 203242599U CN 201320292993 CN201320292993 CN 201320292993 CN 201320292993 U CN201320292993 U CN 201320292993U CN 203242599 U CN203242599 U CN 203242599U
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China
Prior art keywords
ultraviolet light
ionization source
vacuum ultraviolet
ionization
mass
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Expired - Fee Related
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CN 201320292993
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Chinese (zh)
Inventor
郭寅龙
潘洋
张芳
王昊阳
张立
张菁
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Shanghai Institute of Organic Chemistry of CAS
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Shanghai Institute of Organic Chemistry of CAS
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Abstract

The utility model discloses a vacuum ultraviolet light ionization source comprising a vacuum ultraviolet light source and an ionization source chamber which are arranged inside a mass spectrometer and are in a vacuum state. The side wall of the ionization source chamber is provided with a gas inlet which is communicated with a gas phase capillary chromatographic column inside a gas phase chromatographic instrument through a direct introduction device; repulsion electrodes, temperature sensors, ionization chambers, extraction electrodes and focusing electrodes are sequentially arranged in a separated, coaxial and parallel way in a direction perpendicular to a gas sample introduction direction inside the ionization source chamber; the outer sides of the repulsion electrodes, the temperature sensors and the ionization chambers are provided with heating devices; and the vacuum ultraviolet light source is located at one side of the ionization source chamber. The vacuum ultraviolet light ionization source can be matched with a combined gas phase chromatography-mass spectrometry analyzer in use for multi-component sample detection analysis.

Description

A kind of vacuum ultraviolet light ionization source
Technical field
The utility model relates to a kind of vacuum ultraviolet light ionization source, relates in particular to a kind of vacuum ultraviolet light ionization source for the gas chromatography-mass spectrography analysis, belongs to the mass spectrometer technical field.
Background technology
In multicomponent gas chromatography-mass spectrography is analyzed, universal ionization mode is the electronics bombardment, but for the unsettled compound of molecular ion, the electronics bombardment can cause it that excessive fragmentation often occurs in ionization process, can't produce molecular ion, or the molecular ion signal a little less than.Meanwhile, electron impact ionization cracking meeting produces a large amount of fragment ions, makes mass spectrogram complicated, is unfavorable for the parsing of mixture.Equally, can be used for the chemical ionization source that gas chromatography-mass spectrography is analyzed, it can provide stronger molecular ion signal or quasi-molecular ion signal based on ion-molecule reaction, but be confined to specific compound structure and exclusive reaction reagent, therefore can't be general.For the analysis of this compounds, relatively more good is the ionization mode of utilizing the vacuum ultraviolet (VUV) light modulation.
Vacuum-ultraviolet light refers to that wavelength is less than the deep UV (ultraviolet light) of 200nm.It can make ionization energy be lower than the compound molecule generation single photon ionization of its photon energy, produces a large amount of molecular ions, and does not almost have fragment ion.As mass spectral:mass spectrographic ion source, the spectrogram that obtains is simple with vacuum-ultraviolet light, can carry out fast qualitative and quantitative analysis according to the molecular weight information of compound, obtains using more and more widely in fields such as process analysis procedure analysis and organic substance detections.Hou Keyong [Chinese utility model patent: 200610011793.2] disclose a kind of with vacuum UV lamp as mass spectral:mass spectrographic ion source analysis time, can the fast detecting air in the Components of Organic Pollutants of trace; Li Haiyang etc. [Chinese utility model patent: 200920176812.0] utility model be used for the vacuum ultraviolet light ionization source that the high flux gaseous sample is analyzed.But in the sample analysis that contains Multiple components, very mixed and disorderly by the mass spectrogram that the mass spectrum direct-detection generally obtains, and low abundance components or the mass signal that is difficult for the gasification component also may be covered by other strong mass signal, causes relevant information distortion in the analysis result.
The utility model content
The problems referred to above for the prior art existence, the purpose of this utility model provides a kind of vacuum ultraviolet light ionization source that gas chromatography-mass spectrography is analyzed that can be used for, realize that sample is behind the gas chromatograph gasification separation, each cut enters into the ionization source inside cavity successively, through vacuum ultraviolet ionized generation molecular ion peak or quasi-molecular ion peak, to reduce the excessive fragmentation of compound in ionization process, simplify mass spectrogram.
For realizing above-mentioned utility model purpose, the technical solution adopted in the utility model is as follows:
A kind of vacuum ultraviolet light ionization source comprises vacuum ultraviolet light source and ionization source cavity, and both all are located at mass spectrometer inside, are in vacuum state; It is characterized in that: the sidewall at the ionization source cavity is provided with the gas access, and described gas access is connected by the Capillary Column for Gas Chromatography of direct gatherer with gas chromatograph inside; In the ionization source inside cavity, be disposed with space, coaxial, parallel repulsion electrode, temperature sensor, ionization chamber, extraction electrode and focusing electrode perpendicular to the gas sample incoming direction, be provided with heater in the outside of described repulsion electrode, temperature sensor and ionization chamber; Described vacuum ultraviolet light source is positioned at ionization source cavity one side, and its vacuum-ultraviolet light that sends is perpendicular to the repulsion electrode and pass that the zone of space enters into ionization chamber between pole plate.
As a kind of preferred version, the Capillary Column for Gas Chromatography of gas chromatograph inside is connected by the ionization chamber of direct gatherer with the ionization source inside cavity.
As a kind of preferred version, the direction of an electric field between the pole plate of described gas sample incoming direction and repulsion electrode, extraction electrode is perpendicular.
As a kind of preferred version, on repulsion electrode, ionization chamber, extraction electrode and focusing electrode, apply respectively different voltage.
As a kind of preferred version, above-mentioned vacuum ultraviolet light ionization source is connected with mass spectrometric mass analyzer through ends of the earth bar, ion lens.
As further preferred version, described mass analyzer be in flying time mass spectrum analysis device, quadrupole rod mass spectrometer, the ion trap mass spectrometry device any one or by wherein several series connection mass analyzers that form.
As a kind of preferred version, the vacuum-ultraviolet light that described vacuum ultraviolet light source sends passes the duct that arranges in repulsion electrode and the temperature sensor along the axis direction of ionization source cavity, enters ionization chamber inside.
Compared with prior art, the utlity model has following conspicuousness effect:
Experimental result shows, the vacuum ultraviolet light ionization source that the utility model provides can be complementary with the gas chromatography-mass spectrography analyzer, can be used for the detection analysis to the multicomponent sample, not only can make the unsettled compound of molecular ion produce abundant molecular ion peak or quasi-molecular ion peak, and can reduce the excessive fragmentation of this compounds in ionization process, simplify mass spectrogram, have a wide range of applications at the multicomponent analysis field.
Description of drawings
The structural representation of a kind of vacuum ultraviolet light ionization source that Fig. 1 provides for the utility model is among the figure: 1, vacuum ultraviolet light source; 2, ionization source cavity; 3, repulsion electrode; 4, temperature sensor; 5, ionization chamber; 6, heater; 7, extraction electrode; 8, focusing electrode; 9, ends of the earth bar; 10, ion lens; 11, mass analyzer; 12, mass spectrometer; 13, direct gatherer; 14, gas chromatograph;
Fig. 2 is the Mutiple Choice ion flow graph that the multicomponent sample described in the embodiment is analyzed in conjunction with gas chromatography-mass spectrography through described vacuum ultraviolet light ionization source;
Fig. 3 is the mass spectrogram that each composition is analyzed in conjunction with gas chromatography-mass spectrography through vacuum ultraviolet light ionization source in the multicomponent sample described in the embodiment, and wherein: a is oxolane; B is toluene; C2 is dimethylbenzene.
Embodiment
Below in conjunction with embodiment and accompanying drawing to the utility model do further in detail, intactly explanation.
As shown in Figure 1, a kind of vacuum ultraviolet light ionization source that the utility model provides comprises vacuum ultraviolet light source 1 and ionization source cavity 2, and both all are located at mass spectrometer 12 inside, are in vacuum state; It is characterized in that: the sidewall at ionization source cavity 2 is provided with the gas access, and described gas access is connected by the Capillary Column for Gas Chromatography of direct gatherer 13 with gas chromatograph 14 inside; In the inside of ionization source cavity 2, be disposed with space, coaxial, parallel repulsion electrode 3, temperature sensor 4, ionization chamber 5, extraction electrode 7 and focusing electrode 8 perpendicular to the gas sample incoming direction, be provided with heater 6 in the outside of described repulsion electrode 3, temperature sensor 4 and ionization chamber 5; Described vacuum ultraviolet light source 1 is positioned at a side of ionization source cavity 2, and its vacuum-ultraviolet light that sends is perpendicular to repulsion electrode 3 and pass that the zone of space enters into ionization chamber 5 between pole plate.
As a kind of preferred version, the Capillary Column for Gas Chromatography of gas chromatograph 14 inside is connected by the ionization chamber 5 of direct gatherer 13 with ionization source cavity 2 inside, make gasifiable sample after gas-chromatography is separated, under the drive of carrier gas, directly enter ionization chamber 5 inside, make neutral molecule absorb the photon that vacuum ultraviolet light source sends and be ionized; Direction of an electric field between the pole plate of described gas sample incoming direction and repulsion electrode 3, extraction electrode 7 is perpendicular, is beneficial to avoid a large amount of carrier gas, unionized neutral molecule to enter mass spectrum inside by ion source, reduces and pollutes; On repulsion electrode 3, ionization chamber 5, extraction electrode 7 and focusing electrode 8, apply respectively different voltage, the ion that photo ionization produces is under the acting in conjunction of these electric fields, after being pushed and focusing on, enter the ends of the earth bar 9 behind the ionization source cavity, by 9 transmission of ends of the earth bar, be incorporated in the mass analyzer 11 after focusing on through ion lens 10 again.Described mass analyzer 11 can in flying time mass spectrum analysis device, quadrupole rod mass spectrometer, the ion trap mass spectrometry device any one or by wherein several series connection mass analyzers that form (as: triple quadrupole bar mass spectrometer, quadrupole rod-flight time Tandem Mass Spectrometry Analysis device); The vacuum-ultraviolet light that described vacuum ultraviolet light source 1 sends passes the duct that arranges in repulsion electrode 3 and the temperature sensor 4 along the axis direction of ionization source cavity 2, enters ionization chamber 5 inside.
Embodiment
Carry out the gas chromatography-mass spectrography analysis with the sample that contains oxolane (a), toluene (b) and five compositions of three dimethylbenzene isomers (c1, c2, c3), the vacuum ultraviolet light ionization source that mass spectrometric ion source provides for the utility model (as shown in Figure 1), mass analyzer are quadrupole rod-flight time Tandem Mass Spectrometry Analysis device.
Fig. 2 is the Mutiple Choice ion flow graph that the multicomponent sample described in the present embodiment is analyzed in conjunction with gas chromatography-mass spectrography through described vacuum ultraviolet light ionization source, as seen from Figure 2: take the molecular ion of above-mentioned five compounds as selecting ion (oxolane m/z72, toluene m/z92, dimethylbenzene m/z106) that total ion current is extracted, obtain Mutiple Choice ion flow graph respectively; Five signal peaks represent five compounds successively, and retention time is respectively: oxolane 1.73min, toluene 2.03min, three dimethylbenzene 2.46,2.52 and 2.68min.
Fig. 3 is the mass spectrogram that each composition is analyzed in conjunction with gas chromatography-mass spectrography through vacuum ultraviolet light ionization source in the multicomponent sample described in the present embodiment, and wherein: a is oxolane; B is toluene; C2 is dimethylbenzene (because the isomer of three dimethylbenzene has identical mass spectrogram, this sentences c2 is representative), compares with traditional E I mass spectrogram, all presents abundant molecular ion peak.Above result shows that vacuum ultraviolet light ionization source of the present utility model can be complementary with the gas chromatography-mass spectrography analytical instrument, realizes the detection analysis to the multicomponent sample.Sample is after good separation on the gas-chromatography, and each component in succession enters vacuum ultraviolet light ionization source and ionizes, and produces abundant molecular ion, and is detected by the time of flight mass analyzer.
In sum as seen: the vacuum ultraviolet light ionization source that the utility model provides can be complementary with the gas chromatography-mass spectrography analyzer, can be used for the detection analysis to the multicomponent sample, not only can make the unsettled compound of molecular ion produce abundant molecular ion peak or quasi-molecular ion peak, and can reduce the excessive fragmentation of this compounds in ionization process, simplify mass spectrogram, have a wide range of applications at the multicomponent analysis field.
Be necessary at last in this explanation to be: above embodiment only is used for the technical solution of the utility model is described in more detail; can not be interpreted as the restriction to the utility model protection range, some nonessential improvement and adjustment that those skilled in the art makes according to foregoing of the present utility model all belong to protection range of the present utility model.

Claims (5)

1. a vacuum ultraviolet light ionization source comprises vacuum ultraviolet light source and ionization source cavity, and both all are located at mass spectrometer inside; It is characterized in that: the sidewall at the ionization source cavity is provided with the gas access, and described gas access is connected by the Capillary Column for Gas Chromatography of direct gatherer with gas chromatograph inside; In the ionization source inside cavity, be disposed with space, coaxial, parallel repulsion electrode, temperature sensor, ionization chamber, extraction electrode and focusing electrode perpendicular to the gas sample incoming direction, be provided with heater in the outside of described repulsion electrode, temperature sensor and ionization chamber; Described vacuum ultraviolet light source is positioned at ionization source cavity one side.
2. vacuum ultraviolet light ionization source as claimed in claim 1, it is characterized in that: the Capillary Column for Gas Chromatography of gas chromatograph inside is connected by the ionization chamber of direct gatherer with the ionization source inside cavity.
3. vacuum ultraviolet light ionization source as claimed in claim 1, it is characterized in that: the direction of an electric field between the pole plate of described gas sample incoming direction and repulsion electrode, extraction electrode is perpendicular.
4. vacuum ultraviolet light ionization source as claimed in claim 1, it is characterized in that: described vacuum ultraviolet light ionization source is connected with mass spectrometric mass analyzer through ends of the earth bar, ion lens.
5. vacuum ultraviolet light ionization source as claimed in claim 4 is characterized in that: described mass analyzer be in flying time mass spectrum analysis device, quadrupole rod mass spectrometer, the ion trap mass spectrometry device any one or by wherein several series connection mass analyzers that form.
CN 201320292993 2013-05-24 2013-05-24 Vacuum ultraviolet light ionization source Expired - Fee Related CN203242599U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108091540A (en) * 2016-11-21 2018-05-29 中国科学院大连化学物理研究所 A kind of radio frequency focusing enhances vacuum-ultraviolet light mass spectrum ionization source
US20210096111A1 (en) * 2017-05-15 2021-04-01 The Regents Of The University Of Michigan Progressive Cellular Architecture For Microfabricated Gas Chromatograph

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108091540A (en) * 2016-11-21 2018-05-29 中国科学院大连化学物理研究所 A kind of radio frequency focusing enhances vacuum-ultraviolet light mass spectrum ionization source
CN108091540B (en) * 2016-11-21 2019-10-25 中国科学院大连化学物理研究所 A kind of radio frequency focusing enhancing vacuum-ultraviolet light mass spectrum ionization source
US20210096111A1 (en) * 2017-05-15 2021-04-01 The Regents Of The University Of Michigan Progressive Cellular Architecture For Microfabricated Gas Chromatograph
US11927574B2 (en) * 2017-05-15 2024-03-12 The Regents Of The University Of Michigan Progressive cellular architecture for microfabricated gas chromatograph

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20131016

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CF01 Termination of patent right due to non-payment of annual fee