CN105632869A - Vacuum ultraviolet light ionization source device based on glow discharge - Google Patents
Vacuum ultraviolet light ionization source device based on glow discharge Download PDFInfo
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- CN105632869A CN105632869A CN201410619985.6A CN201410619985A CN105632869A CN 105632869 A CN105632869 A CN 105632869A CN 201410619985 A CN201410619985 A CN 201410619985A CN 105632869 A CN105632869 A CN 105632869A
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- glow discharge
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Abstract
The invention relates to a vacuum ultraviolet light ionization source device based on glow discharge. The device includes a glow discharge cavity and an ionization chamber cavity. The glow discharge cavity is provided with an ultraviolet light outlet at a lower end, and is internally provided with a hollow cathode and an annular electrode, the two electrodes are oppositely arranged, and a direct voltage is applied. Rare gas inlet and outlet pipes are arranged on a cavity wall. One end of the rare gas inlet pipe is connected with a rare gas source, and the other end stretches into between the two electrodes. One end of the rare gas outlet pipe stretches into the glow discharge cavity, and the other end is emptied through a sealing valve. A through hole is arranged along an axis direction of the electrodes, the direct voltage is applied to the electrodes in sequence, and the electrodes are connected through precise resistors with the same resistance. A sample injection capillary tube, a vacuum pump extraction opening and a vacuum gauge connector are arranged on an ionization chamber cavity wall. The glow discharge cavity and the ionization chamber cavity are separated by MgF2 glass, and ultraviolet light generated by glow discharge enters the ionization chamber cavity through the MgF2 glass along the axis direction of the electrodes, thereby ionizing a sample.
Description
Technical field
The present invention relates to mass spectrometer, it is exactly a kind of vacuum ultraviolet light ionization source device based on glow discharge specifically, rare gas glow discharge is utilized to produce the ultraviolet light of different-energy, the ionization analysis of relative broad range analyte can be realized, and select suitable rare gas according to organic ionization energy, reduce Organic substance degree of fragmentation.
Background technology
Vacuum-ultraviolet light can make the ionization energy organic molecule generation Single-photon ionization lower than its photon energy, mainly produces molecular ion, almost without fragment ion, is suitable for quick qualitative and quantitative analysis. Vacuum ultraviolet light ionization source is combined by Hou Keyong [Chinese invention patent: 200610011793.2] and Zheng Peichao [Chinese invention patent: 200810022557.X] with mass spectrum, the organic substance spectrogram obtained only comprises organic molecular ion peak, spectrogram is simple, can carry out quick qualitative and quantitative analysis according to molecular weight and signal intensity. But, relative to traditional electron impact ionization source (EI), the ionization energy molecule lower than photon energy can only be ionized, can analyte ranges limited. And commercial vacuum ultraviolet light source is usually the vacuum UV lamp being filled with a kind of rare gas, therefore the vacuum-ultraviolet light photon energy of its transmitting is single and fixing. Such as, the main energy of photon that VUV Kr lamp is launched is 10.6eV, but can not ionize analysis for ionization energy higher than the Organic substance of 10.6eV, and for some legibility from molecule, too high photon energy easily strengthens dissociation degree. Market also has the radio-frequency discharge lamp of a kind of replaceable rare gas, it is possible to by better gaseous species, obtain the photon of different wave length. But this lamp body is long-pending relatively big, and cost is high, and power consumption is big, and structure is complicated, and the radio-frequency field penetrated into may result in ionization chamber organic ionization or dissociates. What is more important is without under window construction, and ion and the metastable neutral molecule of generation of not only discharging all can enter ionized region and react with sample generation molecular ion, and the sample gas of ionized region also can be returned gas and enter region of discharge and cause electric discharge spectral line impure.
It is an object of the invention to provide a kind of vacuum ultraviolet-ionization source apparatus based on glow discharge, it is possible to change rare gas and obtain the photon of different wave length, and by increasing the optical window between ionized region, it is to avoid molecular ion reaction and the interference to region of discharge. This device glow discharge produces the principle of vacuum-ultraviolet light. Advantage is to change rare gas kind as radio-frequency discharge lamp, utilizes a kind of electric discharge device to obtain the vacuum ultraviolet photon of multiple different-energy, can widen the kind of ionizable analyte. Simultaneously, it is possible to select suitable rare gas according to the ionization energy of analyte height, reduce the degree of fragmentation of analyte. This device, compact, power consumption is relatively low, simple in construction, it is simple to integrated.
Summary of the invention
It is an object of the invention to provide a kind of vacuum ultraviolet light ionization source device based on glow discharge.
For achieving the above object, technical scheme is as follows:
A kind of vacuum ultraviolet light ionization source device based on glow discharge, it is characterised in that: include glow discharge cavity, hollow cathode, annular electrode, MgF2Glass, ionization chamber cavity, several Ion Extraction electrodes and difference pore electrode, be provided with vacuum gauge interface and vacuum pump bleeding point in ionization chamber cavity wall;
Hollow cathode and annular electrode are placed in glow discharge cavity, and hollow cathode is the tubular structure that lower ending opening, upper end are airtight, and annular electrode is placed in below the opening of hollow cathode;
One rare gas air inlet pipe and a rare gas escape pipe are each passed through on the wall of glow discharge cavity and stretch in glow discharge cavity, one end of rare gas air inlet pipe extend between hollow cathode and annular electrode, the other end is connected with rare gas source of the gas, rare gas escape pipe one end is positioned at glow discharge cavity, the sealed valve emptying of the other end;
Ion Extraction electrode is cylindrical-shaped structure, is placed in ionization chamber inside cavity, Ion Extraction electrode axially have through hole; When Ion Extraction electrode is more than two, the Ion Extraction electrode of more than two from top to bottom successively parallel, interval, be coaxially disposed;
In ionization chamber cavity, Ion Extraction electrode be connected with tabular difference pore electrode, the hole of difference pore electrode is coaxial with the through hole of Ion Extraction electrode;
Glow discharge cavity is placed in the top of ionization chamber cavity, above the through hole of Ion Extraction electrode, the ionization chamber cavity wall at place offers ultraviolet light entrance, corresponding offers ultraviolet light outlet bottom glow discharge cavity, the ultraviolet light of glow discharge cavity exports, the ultraviolet light entrance of ionization chamber cavity is coaxial with the through hole of Ion Extraction electrode, and ultraviolet light outlet and ultraviolet light entrance are by a MgF2Glass separates, and the ultraviolet light produced in glow discharge cavity passes through MgF from ultraviolet light outlet2Glass enters to inject in ionization chamber cavity through ultraviolet light entrance;
Ionization chamber cavity wall is provided with sample introduction capillary tube, and the gas outlet of sample introduction capillary tube is between ion extraction electrode and difference pore electrode or between Ion Extraction electrode and Ion Extraction electrode; The gas outlet end of sample introduction capillary tube is perpendicular to and enters to inject the ultraviolet light beam in ionization chamber cavity through ultraviolet light entrance.
It is connected with the resistance of similar resistance between two adjacent Ion Extraction electrodes and between the tabular difference pore electrode Ion Extraction electrode adjacent with above it; Tabular difference pore electrode resistance grounded.
The ultraviolet source that glow discharge cavity produces is rare gas glow discharge source; Can pass through to change rare gas kind and obtain the ultraviolet light of different-energy, it is achieved the analysis of relative broad range analyte; Simultaneously, it is possible to select suitable rare gas according to the size of Organic substance ionization energy, reduce organic degree of fragmentation.
Direct current transmission voltage it is applied with respectively on Ion Extraction electrode, difference pore electrode, direct current transmission voltage adopts same DC source, DC voltage carries out dividing potential drop, Ion Extraction electrode and the voltage applied successively on difference pore electrode by resistance and reduces successively along light incident direction.
Separated by ring-type insulant between Ion Extraction electrode and difference pore electrode, coaxial and interval setting between electrode.
When for the Ion Extraction electrode of more than two, being separated by ring-type insulant between adjacent two panels Ion Extraction electrode, between Ion Extraction electrode, coaxial and interval is arranged.
Being connected with mass analyzer in difference pore electrode, the ion that ionization chamber produces enters mass analyzer by the aperture of difference pore electrode; Described mass analyzer is time of flight mass analyzer, level Four bar mass analyzer or ion strap mass analyzer.
Sample passes through sample introduction capillary sample inlet; Be provided with vacuum gauge interface and vacuum pump bleeding point in ionization chamber cavity wall, vacuum pump bleeding point is adjusted valve and is connected with vacuum pump; Ionization chamber vacuum, by vacuum pump and control valve are controlled, maintains between 0.1Pa to 500Pa; Ionization chamber vacuum values is obtained by vacuum gauge.
Ionization source involved in the present invention utilizes glow discharge to produce vacuum-ultraviolet light, and can pass through to change the ultraviolet light of the kind acquisition different-energy of electric discharge rare gas, widens the kind of ionizable analyte. Simultaneously, it is possible to select suitable rare gas according to the ionization energy of analyte height, reduce the degree of fragmentation of analyte. This device, compact, power consumption is relatively low, simple in construction, it is simple to integrated.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram of the vacuum ultraviolet light ionization source device based on glow discharge: 1-glow discharge cavity; 2-hollow cathode; 3-annular electrode; 4-MgF2Glass; 5-rare gas air inlet pipe; 6-rare gas escape pipe; 7-sealed valve; 8-ionization chamber cavity; 9-sample introduction capillary tube; 10-Ion Extraction electrode; 11-difference pore electrode; 12-vacuum gauge; 13-vacuum pump; 14-control valve.
Detailed description of the invention
First, Fig. 1 is a kind of vacuum ultraviolet light ionization source device based on glow discharge, it is characterised in that: include glow discharge cavity 1, hollow cathode 2, annular electrode 3, MgF2Glass 4, ionization chamber cavity 8, several Ion Extraction electrodes 10 and difference pore electrode 11, be provided with vacuum gauge 12 interface and vacuum pump 13 bleeding point in ionization chamber cavity 8 wall;
Hollow cathode 2 and annular electrode 3 are placed in glow discharge cavity 1, and hollow cathode 2 is the tubular structure that lower ending opening, upper end are airtight, and annular electrode 3 is placed in below the opening of hollow cathode 2;
One rare gas air inlet pipe 5 and a rare gas escape pipe 7 are each passed through on the wall of glow discharge cavity 1 and stretch in glow discharge cavity 1, one end of rare gas air inlet pipe 5 extend between hollow cathode 2 and annular electrode 3, the other end is connected with rare gas source of the gas, rare gas escape pipe 7 one end is positioned at glow discharge cavity 1, the sealed valve emptying of the other end;
Ion Extraction electrode 10 is cylindrical-shaped structure, is placed in ionization chamber cavity 8 internal, Ion Extraction electrode 10 axially have through hole; When Ion Extraction electrode 10 is more than two, the Ion Extraction electrode 10 of more than two from top to bottom successively parallel, interval, be coaxially disposed;
In ionization chamber cavity 8, Ion Extraction electrode 10 be connected with tabular difference pore electrode 11, the hole of difference pore electrode 11 is coaxial with the through hole of Ion Extraction electrode 10;
Glow discharge cavity 1 is placed in the top of ionization chamber cavity 8, above the through hole of Ion Extraction electrode 10, ionization chamber cavity 8 wall at place offers ultraviolet light entrance, corresponding offers ultraviolet light outlet bottom glow discharge cavity 1, the ultraviolet light of glow discharge cavity 1 exports, the ultraviolet light entrance of ionization chamber cavity 8 is coaxial with the through hole of Ion Extraction electrode 10, and ultraviolet light outlet and ultraviolet light entrance are by a MgF2Glass 4 separates, and the ultraviolet light produced in glow discharge cavity 1 passes through MgF from ultraviolet light outlet2Glass 4 enters to inject in ionization chamber cavity 8 through ultraviolet light entrance;
Ionization chamber cavity 8 sidewall is provided with sample introduction capillary tube 9, and the gas outlet of sample introduction capillary tube 9 is between ion extraction electrode 10 and difference pore electrode 11 or between Ion Extraction electrode 10 and Ion Extraction electrode 10; The gas outlet end of sample introduction capillary tube 9 is perpendicular to and enters to inject the ultraviolet light beam in ionization chamber cavity 8 through ultraviolet light entrance.
It is connected with the resistance of similar resistance between two adjacent Ion Extraction electrodes and between the tabular difference pore electrode 11 Ion Extraction electrode 10 adjacent with above it; Tabular difference pore electrode 11 resistance grounded.
The ultraviolet source that glow discharge cavity 1 produces is rare gas glow discharge source; Can pass through to change rare gas kind and obtain the ultraviolet light of different-energy, it is achieved the analysis of relative broad range analyte; Simultaneously, it is possible to select suitable rare gas according to the size of Organic substance ionization energy, reduce organic degree of fragmentation.
Direct current transmission voltage it is applied with respectively on Ion Extraction electrode 10, difference pore electrode 11, direct current transmission voltage adopts same DC source, DC voltage carries out dividing potential drop, Ion Extraction electrode 10 and the voltage applied successively on difference pore electrode 11 by resistance and reduces successively along light incident direction.
Separated by ring-type insulant between Ion Extraction electrode 10 and difference pore electrode 11, coaxial and interval setting between electrode.
When for the Ion Extraction electrode 10 of more than two, being separated by ring-type insulant between adjacent two panels Ion Extraction electrode 10, between Ion Extraction electrode 10, coaxial and interval is arranged.
Being connected with mass analyzer in difference pore electrode 11, the ion that ionization chamber produces enters mass analyzer by the aperture of difference pore electrode 11; Described mass analyzer is time of flight mass analyzer, level Four bar mass analyzer or ion strap mass analyzer.
Sample passes through sample introduction capillary tube 9 sample introduction; Be provided with vacuum gauge 12 interface and vacuum pump 13 bleeding point in ionization chamber cavity 8 sidewall, vacuum pump 13 bleeding point is adjusted valve 14 and is connected with vacuum pump 13; Ionization chamber vacuum, by vacuum pump 13 and control valve 14 are controlled, maintains between 0.1Pa to 500Pa; Ionization chamber vacuum values is obtained by vacuum gauge 12.
Claims (8)
1. the vacuum ultraviolet light ionization source device based on glow discharge, it is characterised in that: include glow discharge cavity (1), hollow cathode (2), annular electrode (3), MgF2Glass (4), ionization chamber cavity (8), several Ion Extraction electrodes (10) and difference pore electrode (11), be provided with vacuum gauge (12) interface and vacuum pump (13) bleeding point in ionization chamber cavity (8) wall;
Hollow cathode (2) and annular electrode (3) are placed in glow discharge cavity (1), the tubular structure that hollow cathode (2) is lower ending opening, upper end is airtight, annular electrode (3) is placed in below the opening of hollow cathode (2);
One rare gas air inlet pipe (5) and a rare gas escape pipe (7) are each passed through on the wall of glow discharge cavity (1) and stretch in glow discharge cavity (1), one end of rare gas air inlet pipe (5) extend between hollow cathode (2) and annular electrode (3), the other end is connected with rare gas source of the gas, rare gas escape pipe (7) one end is positioned at glow discharge cavity (1), the sealed valve emptying of the other end;
Ion Extraction electrode (10) is cylindrical-shaped structure, is placed in ionization chamber cavity (8) internal, Ion Extraction electrode (10) axially have through hole; When Ion Extraction electrode (10) is more than two, the Ion Extraction electrode (10) of more than two from top to bottom successively parallel, interval, be coaxially disposed;
In ionization chamber cavity (8), Ion Extraction electrode (10) be connected with tabular difference pore electrode (11), the hole of difference pore electrode (11) is coaxial with the through hole of Ion Extraction electrode (10);
Glow discharge cavity (1) is placed in the top of ionization chamber cavity (8), above the through hole of Ion Extraction electrode (10), ionization chamber cavity (8) wall at place offers ultraviolet light entrance, corresponding offers ultraviolet light outlet in glow discharge cavity (1) bottom, the ultraviolet light of glow discharge cavity (1) exports, the ultraviolet light entrance of ionization chamber cavity (8) is coaxial with the through hole of Ion Extraction electrode (10), and ultraviolet light outlet and ultraviolet light entrance are by a MgF2Glass (4) separates, and the ultraviolet light produced in glow discharge cavity (1) passes through MgF from ultraviolet light outlet2Glass (4) enters to inject in ionization chamber cavity (8) through ultraviolet light entrance;
Ionization chamber cavity (8) sidewall is provided with sample introduction capillary tube (9), and the gas outlet of sample introduction capillary tube (9) is positioned between ion extraction electrode (10) and difference pore electrode (11) or between Ion Extraction electrode (10) and Ion Extraction electrode (10); The gas outlet end of sample introduction capillary tube (9) is perpendicular to and enters to inject the ultraviolet light beam in ionization chamber cavity (8) through ultraviolet light entrance.
2. ionization source according to claim 1, it is characterised in that:
It is connected with the resistance of similar resistance between two adjacent Ion Extraction electrodes and between tabular difference pore electrode (11) the Ion Extraction electrode (10) adjacent with above it; Tabular difference pore electrode (11) resistance grounded.
3. ionization source according to claim 1, it is characterised in that:
The ultraviolet source that glow discharge cavity (1) produces is rare gas glow discharge source; Can pass through to change rare gas kind and obtain the ultraviolet light of different-energy, it is achieved the analysis of relative broad range analyte; Simultaneously, it is possible to select suitable rare gas according to the size of Organic substance ionization energy, reduce organic degree of fragmentation.
4. ionization source according to claim 1 or claim 2, it is characterised in that:
In Ion Extraction electrode (10), difference pore electrode, (11) are applied with direct current transmission voltage respectively, direct current transmission voltage adopts same DC source, DC voltage carries out dividing potential drop, Ion Extraction electrode (10) and the voltage applied successively on difference pore electrode (11) by resistance and reduces successively along light incident direction.
5. according to claim 1 ionization source, it is characterised in that:
Separated by ring-type insulant between Ion Extraction electrode (10) and difference pore electrode (11), coaxial and interval setting between electrode.
6. ionization source according to claim 1, it is characterised in that:
When for Ion Extraction electrode (10) of more than two, being separated by ring-type insulant between adjacent two panels Ion Extraction electrode (10), between Ion Extraction electrode (10), coaxial and interval is arranged.
7. ionization source according to claim 1 or 3, it is characterised in that:
Being connected with mass analyzer in difference pore electrode (11), the ion that ionization chamber produces enters mass analyzer by the aperture of difference pore electrode (11); Described mass analyzer is time of flight mass analyzer, level Four bar mass analyzer or ion strap mass analyzer.
8. ionization source according to claim 1, it is characterised in that:
Sample passes through sample introduction capillary tube (9) sample introduction; Be provided with vacuum gauge (12) interface and vacuum pump (13) bleeding point in ionization chamber cavity (8) sidewall, vacuum pump (13) bleeding point is adjusted valve (14) and is connected with vacuum pump (13); Ionization chamber vacuum, by vacuum pump (13) and control valve (14) are controlled, maintains between 0.1Pa to 500Pa; Ionization chamber vacuum values is obtained by vacuum gauge (12).
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| CN201410619985.6A CN105632869A (en) | 2014-11-06 | 2014-11-06 | Vacuum ultraviolet light ionization source device based on glow discharge |
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| CN201410619985.6A CN105632869A (en) | 2014-11-06 | 2014-11-06 | Vacuum ultraviolet light ionization source device based on glow discharge |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108663162A (en) * | 2018-06-27 | 2018-10-16 | 佛山市金净创环保技术有限公司 | Parallel-moving type closed container vacuum degree measurement system |
| CN109461642A (en) * | 2018-12-07 | 2019-03-12 | 中国烟草总公司郑州烟草研究院 | A kind of ion initiation electron impact ionization source |
| CN114334603A (en) * | 2021-12-14 | 2022-04-12 | 中国计量科学研究院 | Glow discharge electron bombardment ionization source mass spectrum system |
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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 |
| CN103972018A (en) * | 2013-02-01 | 2014-08-06 | 中国科学院大连化学物理研究所 | Radio-frequency electric field enhanced single photon and chemical ionization source |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100032559A1 (en) * | 2008-08-11 | 2010-02-11 | Agilent Technologies, Inc. | Variable energy photoionization device and method for mass spectrometry |
| CN102103971A (en) * | 2009-12-18 | 2011-06-22 | 中国科学院大连化学物理研究所 | Hollow cathode discharge vacuum ultraviolet light ionization source inside minitype mass spectrograph |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108663162A (en) * | 2018-06-27 | 2018-10-16 | 佛山市金净创环保技术有限公司 | Parallel-moving type closed container vacuum degree measurement system |
| CN109461642A (en) * | 2018-12-07 | 2019-03-12 | 中国烟草总公司郑州烟草研究院 | A kind of ion initiation electron impact ionization source |
| CN109461642B (en) * | 2018-12-07 | 2024-04-02 | 中国烟草总公司郑州烟草研究院 | Ion-initiated electron bombardment ionization source |
| CN114334603A (en) * | 2021-12-14 | 2022-04-12 | 中国计量科学研究院 | Glow discharge electron bombardment ionization source mass spectrum system |
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Application publication date: 20160601 |