CN104347343A - Analysis device and method - Google Patents
Analysis device and method Download PDFInfo
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- CN104347343A CN104347343A CN201410521304.2A CN201410521304A CN104347343A CN 104347343 A CN104347343 A CN 104347343A CN 201410521304 A CN201410521304 A CN 201410521304A CN 104347343 A CN104347343 A CN 104347343A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/12—Ion sources; Ion guns using an arc discharge, e.g. of the duoplasmatron type
- H01J49/123—Duoplasmatrons
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Abstract
The invention relates to an analysis device. The analysis device comprises a vacuum cavity, an electrode group, an ion transmission unit, a quality analysis unit and a control unit. The analysis device is characterized in that at least two ionization sources are arranged in the vacuum cavity; the analysis device also comprises a partitioning unit; the partitioning unit and each ionization source are correspondingly arranged between the corresponding ionization source and the electrode group to realize connection and disconnection of ions generated by corresponding ionization sources and vacuum; and the control unit controls the application of voltage on the electrode group and a partitioning mode of the partitioning unit so as to realize the effect that the ions generated by the corresponding ionization sources under different working modes of the ionization sources pass through the partitioning unit, then pass through the electrode group and the ion transmission unit in sequence and further enter the quality analysis unit to carry out detection. The invention also provides an analysis method. The analysis device and method have the advantages of wide detection range and convenience in switching among different working modes and the like.
Description
Technical field
The present invention relates to a kind of analytical equipment and method, especially chromatograph-mass spectrometer coupling analytical equipment and method.
Background technology
Liquid phase-chromatograph-mass spectrometer device (LC-MS) general configuration atmospheric pressure ionization source, comprise atmospheric pressure ionization source as electron spray ionisation source (ESI), atmosphere pressure chemical ion source (APCI), some instrument is also configured with desorption electron spray ionisation source (DESI), directly real-time analysis ionization source (DART) etc.ESI is used for difficult volatile organic matter and macromolecule Analysis of Organic Substances, APCI source is used for polar micromolecules Analysis of Organic Substances, desorption electron spray ionisation source (DESI), directly real-time analysis ionization source (DART) can simplify sample pre-treatments, directly sample is analyzed, this several ionization source all works in atmospheric pressure, mainly obtains molecular ion peak.Gas phase-chromatograph-mass spectrometer device (GC-MS) general configuration electron ionization sources, some instrument configuration ultraviolet ionization source, electron ionization sources (EI) and ultraviolet ionization source are vacuum ionization source, work in vacuum condition, it can obtain fragment ion peak, by library searching, qualitative analysis can be carried out to unknown material, be generally used for GC-MS instrument.
If mass spectrometer can use vacuum ionization source and atmospheric pressure ionization source simultaneously, mass spectrometer and GC instrument, the coupling simultaneously of LC instrument will be made to become possibility, to analysis ability and the application of mass spectrometer be promoted, will the utilance of mass spectrometer be promoted, reduce user's mass spectroscopy device acquisition cost.Foreign vendor has carried out research at EI and ESI mixing ionization source, Varian company (being purchased by Agilent now) releases 300 serial LC-MS instruments, this instrument quality analyzer partial common, EI source and ESI source are modularized design, there is oneself independently sextupole bar in EI source and ESI source, can replace together with sextupole bar entirety.Although the EI source of this instrument energy support moduleization design and ESI source, cannot install EI source and ESI source module, user can only select to install one of them simultaneously.When changing module, need first to lay down vacuum, installation module during installation, and then vacuumize and analyze, operation is comparatively complicated.
Summary of the invention
In order to solve above-mentioned deficiency of the prior art, the invention provides that a kind of detection range is wide, switching analytical equipment and method easily between different working modes.
For achieving the above object, the present invention adopts following technical scheme:
A kind of analytical equipment, comprises vacuum chamber, electrode group, ion transfer unit, mass analysis cell and control unit, is characterized in:
In described vacuum chamber, at least two ionization sources are installed; Described ionization source, for generation of analyte ions, focuses on and shaping ion beam, and controls ion break-make;
Described analytical equipment also comprises isolation block, and described isolation block is arranged between corresponding ionization source and electrode group to each ionization source is corresponding, realizes the break-make between the ion of corresponding ionization source generation and vacuum;
Described control unit controls partition mode electrode group being applied to voltage and isolation block, with realize corresponding ionization source produces under different ionization source mode of operations ion by isolation block after successively by electrode group, ion transfer unit and then enter mass analysis cell and detect;
Electrode group is for realizing the deflection to different azimuth incident ion; Ion transfer unit for receiving the deflect ions of deflection lens, and by ion transfer to mass analysis cell; Mass analysis cell for separating of with detection ion.
As preferably, described isolation block includes but not limited to gate valve, ball valve.
As preferably, described at least two ionization sources are vacuum ionization source or atmospheric pressure ionization source.
As preferably, described electrode group is electrostatic deflection set of lenses or radio frequency deflection lens group.
As preferably, every cube electrode of described electrode group is inner surface is bi-curved electrode slice or planar sheet electrode slice.
As preferably, the ion optics axle of described at least two ionization sources overlaps or vertical.
As preferably, described ion transfer unit is six grades of bars or ion funnel.
As preferably, described atmospheric pressure ionization source includes but not limited to electron spray ionisation source, atmosphere pressure chemical ion source, desorption electron spray ionisation source, directly real-time analysis ionization source.
As preferably, described vacuum ionization source includes but not limited to electron ionization sources, vacuum ultraviolet-ionization source.
Present invention also offers a kind of analytical method, comprise the following steps:
In A, vacuum chamber, at least two ionization sources are installed;
Selection work ionization source, work ionization source and its ion outlet are all in opening; Inoperative ionization source and its ion outlet are all in closed condition;
The ion that B, work ionization source produce enters vacuum chamber by its ion outlet, successively by electrode group, ion transfer unit and then enter mass analysis cell and detect.
Further, above-mentioned arbitrary described analytical equipment is adopted to analyze, wherein, described isolation block is arranged between corresponding ionization source and electrode group to each ionization source is corresponding, realize the open and close of the ion outlet of corresponding ionization source, and then realize the break-make between the ion of corresponding ionization source generation and vacuum.
The present invention compared with prior art has following beneficial effect:
1, different ionization sources can be installed on an instrument simultaneously, has expanded the range of application of same mass spectrometer;
2, do not need to unload vacuum between different ionization sources can realize switching by means of only control isolation block, change speed fast;
3, different ionization sources is in different working regions, separate, there is not mutual interference;
4, ion transfer path is from axle design, reduces the interference of neutral particle;
5, by installing vacuum ionization source and atmospheric pressure ionization source in vacuum chamber, selecting different mode of operations, controlling the break-make of vacuum ionization source and atmospheric pressure ionization source, achieve the functions such as Ion-ion reaction and molecular ion reaction.
Accompanying drawing explanation
Fig. 1 is analytical equipment structural representation in embodiment 2;
Fig. 2 is analytical equipment structural representation in embodiment 3;
Fig. 3 is analytical equipment structural representation in embodiment 4.
Embodiment
Embodiment 1
A kind of analytical equipment, comprises vacuum chamber, isolation block, electrode group, ion transfer unit, mass analysis cell and controllers unit;
In described vacuum chamber, at least two ionization sources are installed; Described ionization source, for generation of analyte ions, focuses on and shaping ion beam, and by control circui ion break-make;
As preferably, described at least two ionization sources are vacuum ionization source or atmospheric pressure ionization source.
Liquid phase-chromatograph-mass spectrometer device (LC-MS) general configuration atmospheric pressure ionization source, described atmospheric pressure ionization source is as electron spray ionisation source (ESI), atmosphere pressure chemical ion source (APCI), and some instrument is also configured with desorption electron spray ionisation source (DESI), directly real-time analysis ionization source (DART) etc.ESI is used for difficult volatile organic matter and macromolecule Analysis of Organic Substances, APCI source is used for polar micromolecules Analysis of Organic Substances, desorption electron spray ionisation source (DESI), directly real-time analysis ionization source (DART) can simplify sample pre-treatments, directly sample is analyzed, this several ionization source all works in atmospheric pressure, mainly obtains molecular ion peak.
Gas phase-chromatograph-mass spectrometer device (GC-MS) general configuration electron ionization sources, some instrument configuration ultraviolet ionization source, electron ionization sources (EI) and ultraviolet ionization source are vacuum ionization source, work in vacuum condition, it can obtain fragment ion peak, by library searching, qualitative analysis can be carried out to unknown material, be generally used for GC-MS instrument.
Described isolation block is arranged between corresponding ionization source and electrode group to each ionization source is corresponding, realizes the break-make between the ion of corresponding ionization source generation and vacuum;
Described control unit controls partition mode electrode group being applied to voltage and isolation block, with realize corresponding ionization source produces under different ionization source mode of operations ion by isolation block after successively by electrode group, ion transfer unit and then enter mass analysis cell and detect;
Electrode group is for realizing the deflection to different azimuth incident ion; Ion transfer unit for receiving the deflect ions of deflection lens, and by ion transfer to mass analysis cell; Mass analysis cell for separating of with detection ion.
As preferably, described isolation block includes but not limited to gate valve, ball valve.
As preferably, described electrode group is electrostatic deflection set of lenses or radio frequency deflection lens group.
As preferably, every cube electrode of described electrode group is inner surface is bi-curved electrode slice or planar sheet electrode slice.
Restriction is not added to the ion optics axle of described at least two ionization sources, carries out analyzing as long as can ion transfer unit be entered and then enters mass analysis cell from the ion of corresponding ionization source outgoing by the deflection of electrode group.
As preferably, the ion optics axle of described at least two ionization sources overlaps or vertical.
As preferably, described ion transfer unit is six grades of bars or ion funnel.
Present invention also offers a kind of analytical method, comprise the following steps:
In A, vacuum chamber, at least two ionization sources are installed;
Selection work ionization source, work ionization source and its ion outlet are all in opening; Inoperative ionization source and its ion outlet are all in closed condition; Ion outlet is set as ion from ionization source to the connector of vacuum chamber, and ion outlet of the present invention can be understood as isolation block and is arranged on partition module between corresponding ionization source and electrode group;
The ion that B, work ionization source produce enters vacuum chamber by its ion outlet, successively by electrode group, ion transfer unit and then enter mass analysis cell and detect.
Further, above-mentioned arbitrary described analytical equipment is adopted to analyze, wherein, described isolation block is arranged between corresponding ionization source and electrode group to each ionization source is corresponding, realize the open and close of the ion outlet of corresponding ionization source, and then realize the break-make between the ion of corresponding ionization source generation and vacuum.
Different ionization sources can be installed on an instrument simultaneously, has expanded the range of application of same mass spectrometer;
Do not need to unload vacuum between different ionization sources can realize switching by means of only control isolation block, change speed fast;
Different ionization sources is in different working regions, separate, there is not mutual interference;
Ion transfer path is from axle design, reduces the interference of neutral particle;
By installing vacuum ionization source and atmospheric pressure ionization source in vacuum chamber, selecting different mode of operations, controlling the break-make of vacuum ionization source and atmospheric pressure ionization source, achieve the functions such as Ion-ion reaction and molecular ion reaction.
Embodiment 2
The present embodiment is the application examples of embodiment 1.
Should provide a kind of analytical equipment by use-case, refer to Fig. 1, described analytical equipment comprises atmospheric pressure ionization source 1, vacuum ionization source 2, electrode group 3, isolation block, ion transfer unit 5, mass analysis cell 6.
Wherein, described atmospheric pressure ionization source 1 is ESI source, and described vacuum ionization source 2 is EI source, and ESI source module 1 and EI source module 2 are installed vertically on vacuum cavity both sides and are oppositely arranged, and becomes 90 degree with the main ion optic axis of the mass analyzer 61 of mass analysis cell 6; The ion optics axle of ESI source module 1 and EI source module 2 overlaps.
ESI source comprises spray capillary 11, atomization gas 12, atomization tracheae 13, sample cone 14, extracts cone 15 and ESI pressure vessel body etc.EI source comprises filament 21, extraction lens 22, condenser lens 23, exit lens 24, repeller electrode 25 and ionization source capsule 20, EI source module entirety and is in vacuum, and vacuum degree is less than 10-4Torr, and vacuum is realized by supporting vacuum system.The corresponding construction in ESI source, EI source is the state of the art, does not repeat them here.
Electrode group 3 is that bi-curved electrode forms by D31, D32, D33, D34 tetra-groups of inner surfaces, and electrode loads direct voltage.
Isolation block is for cutting off module 41 and cutting off module 42, and described partition module 41 and partition module 42 are separately positioned between ESI source and electrode group 3, between EI source and electrode group 3.Described partition module 41 and partition module 42 are gate valve.
Ion transfer unit 5 comprises sextupole transmission pole 51 and lens 52, six grades of transmission poles 51 for transmission and focused ion, and by selecting suitable driving voltage, six grades of transmission poles 51 can high efficiency of transmission and focus on the ion that ESI source produces.Lens 52 are for focused ion and alleviate the fringing field effect of mass detector, improve the efficiency of transmission of ion.
Mass analysis cell 6 comprises mass analyzer 61 and detector 62, and wherein mass analyzer 61 is level Four bar mass analyzer.
The course of work is as follows:
A, need selection work ionization source, work ionization source and its ion outlet are all in opening; Inoperative ionization source and its ion outlet are all in closed condition;
Under different ionization source mode of operations, isolation block realizes the open and close of the ion outlet of corresponding ionization source, and then realizes the break-make between the ion of corresponding ionization source generation and vacuum;
The ion that B, work ionization source produce enters vacuum chamber by its ion outlet, successively by electrode group, ion transfer unit and then enter mass analysis cell and detect;
That is:
Control unit selects ESI source to be work ionization source, and the work of control ESI source, under the mode of operation of ESI source, spray capillary 11 loads 3000V high pressure (V11), after fluid sample flows out from spray capillary 11, the solution under atmospheric pressure, under the effect of spraying gas 12, forms charged droplet, along with the evaporation of solvent, charged droplet is transformed into charged particle.Sample cone 14 and extraction cone 15 form atmospheric pressure-vacuum Sampling Interface with supporting vacuum system, sample cone 14 and extraction cone 15 vacuum degree are a few Torr, and charged particle is after two cone samplings, and part ion is through cutting off module 41, through extracting lens 17, arrive electrode group 3.Extract lens 17 for compressing ion and controlling the break-make of ion.Now, controllers unit controls is cut off module 42 and is closed, and exit lens 24 is closed, and EI source is in closed condition.The course of work in ESI source is the state of the art, does not repeat them here.
By selecting suitable electrode group D31, D32, D33, D34 electrode voltage to combine, partially being turn 90 degrees by electrode group 3 from the ion of ESI source outgoing, arriving six grades of transmission poles 51.From the ion of sextupole transmission pole 51 outgoing, reach mass analyzer 61 through lens 52 and analyze.Mass analyzer 61 loads RF drive, and for being separated successively according to quality order by object ion, the ion after separation arrives detector 62 and is detected.
Control unit selects EI source to be work ionization source, and the work of control EI source, under the mode of operation of EI source, to filament 21 load driver electric current, a large amount of electronics of filament emission, in ionization source capsule, electronics forms charged ion by after sample ionization; Repeller electrode 25 on-load voltage V21, extract lens 22 on-load voltage V23, repeller electrode 25 is shifted onto for the ion produced by ionization source capsule and is extracted lens 22 place, extract lens 22 for being extracted from the ionization source capsule 20 producing ion by ion, under the acting in conjunction of extracting lens 22 and repeller electrode 25, the ion that ionization source capsule produces reaches condenser lens 23, condenser lens 23 on-load voltage V24, is used for ion to carry out compressing and focusing in radial direction; Ion after focusing through after partition module 42, then through exit lens 24, arrives electrode group 3.Now, controllers unit controls is cut off module 41 and is closed, and extract lens 17 and close, ESI source is in closed condition.The course of work in EI source is the state of the art, does not repeat them here.
By selecting suitable electrode group D31, D32, D33, D34 electrode voltage to combine, partially being turn 90 degrees by electrode group 3 from the ion of EI source outgoing, arriving sextupole transmission pole 51.From the ion of sextupole transmission pole 51 outgoing, reach mass analyzer 61 through lens 52 and analyze.Mass analyzer 61 loads RF drive, and for being separated successively according to quality order by object ion, the ion after separation arrives detector 62 and is detected.
The present embodiment, atmospheric pressure ionization source and vacuum ionization source are arranged on vacuum cavity simultaneously, select to adopt EI source or ESI source by gate valve.EI source and ESI source work alone, and there is not interference each other.The direct voltage that electrode group 3 loads is optimized according to analyzed sample, guarantees the highest efficiency of transmission.
Embodiment 3
The present embodiment is the application examples of embodiment 1.
The present embodiment is as different from Example 2: refer to Fig. 2, the atmospheric pressure ionization source 101 of the present embodiment is APCI ionization source, and electrode group 30 adopts D301, D302, D303, D304 planar sheet electrode; Ion transfer unit 50 comprises ion funnel 501, and ion funnel 501 is for transmission and focused ion, and by selecting suitable driving voltage, ion funnel 5 can high efficiency of transmission and the ion focusing on the generation of APCI source.Mass analysis cell 60 comprises time of flight mass analyzer 601, and time of flight mass analyzer 601 comprises the ion extraction and accelerating module 602, ion flight district 603 and ion repeller 604 etc.Ion is after the ion extraction and accelerating module 602 are selected and accelerated, enter into ion flight district 603, in movement area 603, ion is separated successively according to the size of mass number and reaches detector, the effect of ion repeller 604 increases ion flight distance, promotes mass resolution.
APCI source comprises spray capillary 11, spray point 102, sample cone 14, extracts cone 15 and APCI pressure vessel body etc.
Controllers Unit selection APCI source is work ionization source, and the work of control APCI source, under the mode of operation of APCI source, spray point 102 loads 1000V high pressure (V11), after gaseous sample flows out from spray capillary 11, gas molecule sample under atmospheric pressure, ionizes, is transformed into charged particle under the effect of spray point.Sample cone 14 and extraction cone 15 form atmospheric pressure-vacuum Sampling Interface with supporting vacuum system, and charged particle is after two cone samplings, and part ion, through partition module 41, through extracting lens 17, arrives electrode group 3.Under the mode of operation of APCI source, controllers unit controls is cut off module 42 and is closed, and exit lens 24 is closed, and EI source is in closed condition.The course of work in APCI source is the state of the art, does not repeat them here.
By selecting suitable deflecting electrode group D301, D302, D303, D304 electrode voltage to combine, partially being turn 90 degrees by electrode group from the ion of APCI source outgoing, arriving ion funnel 501.From the ion of ion funnel 501 outgoing, reach time of flight mass analyzer 601 through lens 52 and be separated and detected analysis by detector.
Control unit selects EI source to be work ionization source, and the work of control EI source, under the mode of operation of EI source, the ion that EI source produces through after partition module 42, then through exit lens 24, arrives electrode group 30.Now, control unit controls to cut off module 41 and closes, and extract lens 17 and close, APCI source is in closed condition.
By selecting suitable electrode group D301, D302, D303, D304 electrode voltage to combine, partially being turn 90 degrees by electrode group 3 from the ion of EI source outgoing, arriving ion funnel 501.From the ion of ion funnel 501 outgoing, reach time of flight mass analyzer 601 through lens 52 and be separated and detected analysis by detector.
Embodiment 4
The present embodiment is the application examples of embodiment 1.
The present embodiment and the analytical equipment described in embodiment 2 unlike: refer to Fig. 3, the vacuum ionization source 20 of the present embodiment is ultraviolet ionization source, ESI source and ultraviolet ionization source are installed vertically on vacuum cavity 10 both sides, become 90 degree with the main ion optic axis of the mass analyzer 61 of mass analysis cell 6; Ultraviolet ionization source comprises uviol lamp 201, extraction lens 202, condenser lens 203, exit lens 204, repeller electrode 205 and ionization source capsule 200, and ultraviolet ionization source entirety is in vacuum, and vacuum degree is less than 10
-4torr, vacuum is realized by supporting vacuum system.
The present embodiment also comprises APCI source 9, and described APCI source 9 is installed vertically on vacuum chamber 10, overlaps with the main ion optic axis of mass analyzer 61; The ion optics axle of ESI source and ultraviolet ionization source overlaps.
Isolation block also comprises and cuts off module 43, realizes the open and close of the ion outlet in APCI source, and then realizes the break-make between the ion of APCI ionization source generation and vacuum, and described partition module 43 is also gate valve.
APCI source 9 comprises spray capillary 91, spray point 92, sample cone 93, extracts cone 94 and exit lens 95 etc.
When ultraviolet ionization source, ESI source and APCI source are installed simultaneously, any one source can be selected to work, other two provenances are closed; In some particular application, such as need the application scenario of carrying out ion-molecule reaction or Ion-ion reaction, deflection lens running parameter can be optimized, open two sources or three sources simultaneously.
Above-mentioned execution mode should not be construed as limiting the scope of the invention.Key of the present invention is: be arranged on by multiple ionization source in same set of analytical instrument, and the ion being realized different ionization source outgoing by isolation block enters mass analysis cell analysis.Without departing from the spirit of the invention, all should fall within protection scope of the present invention any type of change that the present invention makes.
Claims (8)
1. an analytical equipment, comprises vacuum chamber, electrode group, ion transfer unit, mass analysis cell and control unit, it is characterized in that:
In described vacuum chamber, at least two ionization sources are installed;
Described analytical equipment also comprises isolation block, and described isolation block is arranged between corresponding ionization source and electrode group to each ionization source is corresponding, realizes the break-make between the ion of corresponding ionization source generation and vacuum;
Described controllers unit controls applies the partition mode of voltage and isolation block to electrode group, with realize corresponding ionization source produces under different ionization source mode of operations ion by isolation block after successively by electrode group, ion transfer unit and then enter mass analysis cell and detect.
2. analytical equipment according to claim 1, is characterized in that: described isolation block includes but not limited to gate valve, ball valve.
3. analytical equipment according to claim 1, is characterized in that: described at least two ionization sources are vacuum ionization source or atmospheric pressure ionization source.
4. analytical equipment according to claim 1, is characterized in that: described electrode group includes but not limited to electrostatic deflection set of lenses or radio frequency deflection lens group.
5. analytical equipment according to claim 1, is characterized in that: described electrode group includes but not limited to that every cube electrode be inner surface is bi-curved electrode slice or planar sheet electrode slice.
6. analytical equipment according to claim 1, is characterized in that: described ion transfer unit includes but not limited to six grades of bars or ion funnel.
7. an analytical method, comprises the following steps:
In A, vacuum chamber, at least two ionization sources are set;
Selection work ionization source, work ionization source and its ion outlet are all in opening; Inoperative ionization source and its ion outlet are all in closed condition;
The ion that B, work ionization source produce enters vacuum chamber by its ion outlet, successively by electrode group, ion transfer unit and then enter mass analysis cell and detect.
8. analytical method according to claim 7, it is characterized in that: adopt the arbitrary described analytical equipment of claim 1 ~ 6 to analyze, wherein, described isolation block is arranged between corresponding ionization source and electrode group to each ionization source is corresponding, realize the open and close of the ion outlet of corresponding ionization source, and then realize the break-make between the ion of corresponding ionization source generation and vacuum.
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| CN104792856A (en) * | 2015-04-21 | 2015-07-22 | 苏州大学 | Ion sample introduction method and multi-channel array ion trap mass spectrum system |
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| CN107359104A (en) * | 2017-06-14 | 2017-11-17 | 中国科学院地质与地球物理研究所 | A kind of magnetic substance spectralyzer couples conversion equipment with dual ion sources |
| CN107359100A (en) * | 2017-06-28 | 2017-11-17 | 武汉华星光电技术有限公司 | A kind of ion implantation apparatus and its application method |
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