CN112798677A - Multi-mode mass spectrometry system and method - Google Patents
Multi-mode mass spectrometry system and method Download PDFInfo
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- CN112798677A CN112798677A CN202011643590.1A CN202011643590A CN112798677A CN 112798677 A CN112798677 A CN 112798677A CN 202011643590 A CN202011643590 A CN 202011643590A CN 112798677 A CN112798677 A CN 112798677A
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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
- H01J49/107—Arrangements for using several ion sources
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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Abstract
The invention provides a multimode mass spectrometry system and a method, wherein the multimode mass spectrometry system comprises a first ion source, a second ion source and a multi-stage transmission rod, wherein the first ion source is an ion source under atmospheric pressure; the separator between the first vacuum chamber and the second vacuum chamber is provided with a first through hole suitable for passing ions; the interior of the container is separated into a first part and a second part by a first sliding part, the first part is communicated with the second vacuum chamber, the second part is communicated with the first vacuum chamber, and the first sliding part sliding in the container keeps sealed with the inner wall of the container; one end of the connecting piece is connected with the first sliding piece, and the other end of the connecting piece passes through the second part and is connected with the second sliding piece; the second sliding part is provided with a second through hole; when the second sliding part slides on the surface of the isolating part, the second sliding part closes the first through hole, or the second through hole is communicated with the first through hole; the elastic piece is connected with the second sliding piece and used for blocking the second sliding piece from moving towards the first part. The invention has the advantages of low cost and the like.
Description
Technical Field
The present invention relates to mass spectrometry, and more particularly to a system and method for multimodal mass spectrometry.
Background
GC-MS and LC-MS are two common mass spectrum technologies, the application of the two technologies is complementary, and the principle of the MS part is the same, so that the GC-LC-MS formed by combining the two technologies by using one set of MS can optimize the application range and cost, and has great market advantages.
The vacuum degree requirements of the ion sources used by the two are different, the GC (EI/CI source) needs the vacuum degree of more than 1e-5Torr, and the atmospheric pressure needs to be blocked directly; LC (ESI/APCI source) operates at atmospheric pressure and requires the transfer of ions between atmospheric pressure and vacuum by means of a multi-stage vacuum chamber transition.
Aiming at the same problem, the waters company uses the mode of ion source integral replacement to avoid the problem, needs manual disassembly and cannot realize the online switching of GC/LC two modes;
aiming at the problem of vacuum isolation, the ICP-MS product of Hangzhou spectral culture uses a pneumatic gate valve to isolate vacuum and atmosphere, but the conventional gate valve has large volume and is not suitable for being integrated on a lens device;
the isolation is also realized by driving a micro valve plate to act by using power of a built-in electromagnet and the like, but the electromagnet needs an additional lead wire, and the magnetic field brought by the magnet can influence ion transmission.
It can be seen that the existing solutions all have some problems that are not favorable for the dual mode combination.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a multimode mass spectrometry system.
The purpose of the invention is realized by the following technical scheme:
the multi-mode mass spectrometry system comprises a first ion source, a second ion source and multi-stage transmission rods, wherein the multi-stage transmission rods are respectively arranged in a plurality of vacuum chambers connected in series; the first ion source is an ion source under atmospheric pressure, emergent ions sequentially pass through the first vacuum chamber and the second vacuum chamber, and the second ion source is arranged in the vacuum chamber; a partition is arranged between the first vacuum chamber and the second vacuum chamber, and is provided with a first through hole suitable for ions to pass through; the multimode mass spectrometry system further comprises:
a container, the interior of which is separated into a first part and a second part by a first sliding piece, the first part is communicated with the second vacuum chamber, the second part is communicated with the first vacuum chamber, and the first sliding piece slides in the container and keeps sealed with the inner wall of the container;
one end of the connecting piece is connected with the first sliding piece, and the other end of the connecting piece penetrates through the second part and is connected with the second sliding piece;
a second slider having a second through hole; when the second sliding piece slides on the surface of the isolating piece, the second sliding piece closes the first through hole, or the second through hole is communicated with the first through hole;
and the elastic piece is connected with the second sliding piece and is used for blocking the second sliding piece from moving towards the first part.
The invention also aims to provide a multimode mass spectrometry method applying the multimode mass spectrometry system, and the aim of the invention is realized by the following technical scheme:
the multimode mass spectrometry method applying the multimode mass spectrometry system comprises the following steps:
in the first mode: vacuumizing a first vacuum chamber and a second vacuum chamber, wherein the pressure in the first vacuum chamber is higher than the pressure in the second vacuum chamber; the second through hole is communicated with the first through hole;
ions emitted by the first ion source enter the transmission rod in the first vacuum chamber, and then sequentially pass through the second through hole and the first through hole to enter the transmission rod in the second vacuum chamber;
in the second mode: the second vacuum chamber is vacuumized, and the first vacuum chamber is communicated with the outside atmosphere; the first sliding piece moves upwards, and the second sliding piece moving upwards along the surface of the isolating piece closes the first through hole;
the second ion source operates.
Compared with the prior art, the invention has the beneficial effects that:
1. the mode switching is convenient and fast;
the switching of the working modes is realized automatically, if the second ion source works to be switched into the first ion source, only the gas in the first vacuum chamber needs to be automatically pumped out, and the second through hole of the second sliding part is communicated with the first through hole of the isolating part; if the first ion source work is converted into the first ion source work, the gas in the first vacuum chamber does not need to be pumped out, the second sliding part automatically seals the first through hole, the isolation of the vacuum chamber (not the first vacuum chamber) from the outside atmosphere is realized, and the whole switching process is simple and quick;
the first part in the container is communicated with the second vacuum chamber, the second part is communicated with the first vacuum chamber, and the first sliding part is automatically driven by the pressure difference between the first vacuum chamber and the second vacuum chamber, so that the second sliding part is driven to move on the surface of the isolating part, the first through hole is further sealed or opened, the first vacuum chamber and the second vacuum chamber are automatically controlled to be communicated or not, and the switching of mass spectrum working modes is also realized;
the guide piece or the guide rail is used, so that the second sliding piece tightly adheres to the isolating piece to move up and down, and the plugging effect of the first through hole is improved; meanwhile, the second sliding part element has no left and right displacement, and has no left and right deviation when the second through hole is communicated with the first through hole, so that the communication effect is improved;
2. the structure is simple;
the container, the sliding part and the connecting part are all conventional parts, so that the volume is small, the cost is low, and the operation reliability is good;
3. the analysis result is reliable;
an electromagnet is not needed, and normal ion transmission and mass spectrometry cannot be influenced.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic block diagram of a multimode mass spectrometry system according to an embodiment of the invention;
FIG. 2 is a schematic diagram of a portion of a multimode mass spectrometry system according to an embodiment of the invention.
Detailed Description
Fig. 1-2 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 shows a schematic structural diagram of a multimode mass spectrometry system according to an embodiment of the invention, as shown in fig. 1, the multimode mass spectrometry system includes:
a first ion source 21, a second ion source 22 (such as an EI source or a CI source), and a multi-stage transfer rod respectively disposed in a plurality of vacuum chambers connected in series; the first ion source 21 is an atmospheric pressure ion source, such as an ESI source or an APCI source, and the emitted ions sequentially pass through the first vacuum chamber 12 and the second vacuum chamber 13, and the second ion source 22 is arranged in the vacuum chamber; a partition 61 is arranged between the first vacuum chamber 12 and the second vacuum chamber 13, and the partition 61 is provided with a first through hole 62 suitable for passing ions;
as shown in fig. 2, a container 91, the interior of the container 91 being partitioned into a first portion 92 and a second portion 93 by a first sliding member 94, the first portion 92 communicating with the second vacuum chamber 13, the second portion 93 communicating with the first vacuum chamber 12, the first sliding member 94 sliding within the container 91 and maintaining a seal with the inner wall of the container 91;
a connecting member 98, one end of the connecting member 98 is connected to the first sliding member 94, and the other end passes through the second portion 93 and is connected to the second sliding member 95;
a second slide 95, said second slide 95 having a second through hole 96; when the second sliding member 95 slides on the surface of the partition 61, the second sliding member 95 closes the first through hole 62, or the second through hole 96 communicates with the first through hole 62;
an elastic member 97, the elastic member 97 being connected to the second slider 95 for obstructing the second slider 95 from moving towards the first portion 92.
In order to make the second slider translate against the partition to better close the first through hole, further, the distance of said elastic element 97 from the surface of said partition 61 is progressively greater in the direction from the second portion 93 to the first portion 92.
In order to improve the ion transmission effect and the vacuum degree, the multimode mass spectrometry system further comprises:
a third vacuum chamber 14 and a fourth vacuum chamber 15, said second ion source 22 being disposed within said third vacuum chamber 14, and a mass analyzer 51 being disposed within said fourth vacuum chamber 15.
In order to share various suction pumps, further, the interiors of the second vacuum chamber 13, the third vacuum chamber 14 and the fourth vacuum chamber 15 are respectively communicated with a molecular pump 72 and a backing pump 71 in sequence;
the interior of the first vacuum chamber 12 communicates with the inlet of the valve 81 and the backing pump 71 in this order.
In order to define the moving path of the second slider so that the second through hole and the first through hole are coaxial and to enhance the effect of the second slider closing the first through hole, further, a guide is provided on the partition along which the second slider slides up and down.
The multimode mass spectrometry method of the embodiment of the present invention, that is, the operating method of the multimode mass spectrometry system of the embodiment of the present invention, includes:
in the first mode: the first vacuum chamber 12 and the second vacuum chamber 13 are vacuumized, the pressure in the first vacuum chamber 12 is higher than the pressure in the second vacuum chamber 13, the first sliding piece 94 is pushed upwards, the elastic piece 97 is elongated, the first sliding piece 94 (the second sliding piece 95) is made to be static, and the second through hole 96 is communicated with the first through hole 62;
the first ion source 21 works in an atmospheric pressure environment, and the emergent ions pass through the sampling cone 31 and enter the transmission rod 41 in the first vacuum chamber 12, and then sequentially pass through the second through hole 96 and the first through hole 62 and enter the transmission rod 42 in the second vacuum chamber 13;
the second ion source 22 is disposed in the other vacuum chamber, such as the third vacuum chamber 14 downstream of the second vacuum chamber 13, and in the first mode, the second ion source 22 is inactive;
in the second mode: the second vacuum chamber 13 is vacuumized, the first vacuum chamber 12 is not vacuumized any more, and is communicated with the outside atmosphere; the pressure difference in the first and second vacuum chambers 12 and 13 pushes the first slider 94 to move upward, and the second slider 95 moving upward along the surface of the partition 61 closes the first through hole 62;
the second ion source operates.
To exclude the influence of the external atmosphere on the second ion source, further, in the first mode, the ions sequentially pass through the transmission rods in the second vacuum chamber 13 and the third vacuum chamber 14, and then enter the mass analyzer 51 in the fourth vacuum chamber 15;
in the second mode, the ions emitted from the second ion source 22 are deflected and enter the transmission rod 43 in the third vacuum chamber 14, and then enter the mass analyzer 51 in the fourth vacuum chamber 15.
Example 2:
an application example of the multimode mass spectrometry system and method according to embodiment 1 of the present invention.
In this application example, as shown in fig. 1-2, the multimode mass spectrometry system comprises four vacuum chambers connected in series, three-stage transmission rods are provided in the first three vacuum chambers (first to third vacuum chambers), respectively, and a mass analyzer 51 is provided in the fourth vacuum chamber 15; a partition is arranged between the adjacent vacuum chambers and is provided with a through hole suitable for the passing of ions; wherein, a first through hole 62 is arranged on the first isolating piece 61 between the first vacuum chamber 12 and the second vacuum chamber 13; the first ion source 21 is an ESI source and is arranged in the ionization chamber 11 under atmospheric pressure; the second ion source 22, which is an EI source, is disposed inside the third vacuum chamber 14 at the side of the transfer rod 43; the ion deflection module is arranged in the third vacuum chamber 14, and the ions emitted from the second ion source 22 pass through the ion deflection module and then enter the transmission rod 43 for transmission;
the container 91 is a cylindrical structure, the first sliding member 94 slides along the central axis direction of the container 91, keeps a seal with the inside of the container 91 during sliding, and separates the inside of the container 91 into a first part 92 and a second part 93 at the upper part, the first part 92 is communicated with the second vacuum chamber 13, and the second part 93 is communicated with the first vacuum chamber 12; a rigid connecting member 98 having an upper end connected to the first slider 94 and a lower end passing through the second portion 93 and connected to the second slider 95; the second slider 95 has a second through hole 96; the elastic element 97 is a spring, one end of the elastic element is fixed at the bottom of the first vacuum chamber 12, the other end of the elastic element is connected with the bottom of the second sliding element 95, namely, the spring is arranged at the lower side of the second sliding element 95, the distance between the spring and the first isolating element 61 is gradually increased from bottom to top, the second sliding element 95 is tightly attached to the first isolating element 61 by the pulling force of the spring, and the blocking effect of the second sliding element 95 on the first through hole 62 is provided;
a valve 81 and a pump set, wherein the pump set comprises a molecular pump 72 and a backing pump 71, the interior of the first vacuum chamber 12 is communicated with the inlet of the backing pump 71, and the valve 81 controls whether the first vacuum chamber 12 is communicated with the backing pump 71 or not; the molecular pump 72 and the backing pump 71 are connected in this order inside the second-fourth vacuum chambers so that the gas pressure inside the first vacuum chamber 12 is higher than the gas pressure inside the second-fourth vacuum chambers.
The multimode mass spectrometry method of the embodiment of the present invention, that is, the operating method of the multimode mass spectrometry system of the embodiment of the present invention, includes:
in the first mode: evacuating the first-fourth vacuum chambers, wherein the gas pressure in the first vacuum chamber 12 is higher than the gas pressure in the second-fourth vacuum chambers; the pressure difference between the first vacuum chamber 12 and the second vacuum chamber 13 pushes the first sliding member 94 upward, and the elastic member 97 is elongated (generates downward elastic force to hinder the upward movement of the second sliding member 95) so that the first sliding member 94 (the second sliding member 95) is stationary, the second through hole 96 is communicated with the first through hole 62, and the central axes of the second through hole 96 and the first through hole 62 are coaxial;
the first ion source 21 works in the ionization chamber 11 under atmospheric pressure, and the emergent ions pass through the sampling cone 31 and enter the transmission rod 41 in the first vacuum chamber 12, then sequentially pass through the second through hole 96 and the first through hole 62 and enter the transmission rod 42 in the second vacuum chamber 13, then pass through the third vacuum chamber 14 and enter the mass analyzer 51 in the fourth vacuum chamber 15;
the second ion source 22 is disposed within the third vacuum chamber 14 and is inoperative;
in the second mode: the second vacuum chamber 13 is vacuumized, the valve 81 is closed, the first vacuum chamber 12 is not vacuumized any more, and the outside atmosphere is communicated; the pressure difference in the first and second vacuum chambers 12 and 13 pushes the first slider 94 to move upward, the second slider 95 moving upward along the surface of the partition 61 closes the first through hole 62, and the spring is further elongated;
the second ion source 22 works, and the emergent ions enter the transmission rod 43 after being deflected and then enter the fourth vacuum chamber 15;
when switching from the second mode to the first mode, the valve 81 is opened, the first vacuum chamber 12 is evacuated, at this time, the difference in internal pressure between the first vacuum chamber 12 and the second vacuum chamber 13 becomes small, and the second slider 95 (the first slider 94) is moved downward by spring pulling so that the second through hole 96 and the first through hole 62 communicate, and the center axes of the second through hole 96 and the first through hole 62 are coaxial.
Example 3:
the application example of the multimode mass spectrometry system and method according to embodiment 1 of the present invention is different from embodiment 1 in that:
the first isolating piece is provided with the guide piece or the guide rail, and the second sliding piece moves on the guide piece or the guide rail, so that the second sliding piece does not move left and right when moving up and down, and the correspondence and the communication between the second through hole and the first through hole are well ensured.
The spring is arranged on the upper side of the second sliding part, and when the second sliding part moves upwards, the spring is compressed to generate downward elastic force, namely the spring resists the second sliding part to move upwards.
Claims (8)
1. The multi-mode mass spectrometry system comprises a first ion source, a second ion source and multi-stage transmission rods, wherein the multi-stage transmission rods are respectively arranged in a plurality of vacuum chambers connected in series; the first ion source is an ion source under atmospheric pressure, emergent ions sequentially pass through the first vacuum chamber and the second vacuum chamber, and the second ion source is arranged in the vacuum chamber; a partition is arranged between the first vacuum chamber and the second vacuum chamber, and is provided with a first through hole suitable for ions to pass through; characterized in that the multimode mass spectrometry system further comprises:
a container, the interior of which is separated into a first part and a second part by a first sliding piece, the first part is communicated with the second vacuum chamber, the second part is communicated with the first vacuum chamber, and the first sliding piece slides in the container and keeps sealed with the inner wall of the container;
one end of the connecting piece is connected with the first sliding piece, and the other end of the connecting piece penetrates through the second part and is connected with the second sliding piece;
a second slider having a second through hole; when the second sliding piece slides on the surface of the isolating piece, the second sliding piece closes the first through hole, or the second through hole is communicated with the first through hole;
and the elastic piece is connected with the second sliding piece and is used for blocking the second sliding piece from moving towards the first part.
2. The system of claim 1, wherein the spring is progressively more distant from the spacer surface in a direction from the second portion to the first portion.
3. The multimode mass spectrometry system of claim 1, further comprising:
a third vacuum chamber and a fourth vacuum chamber, the second ion source being disposed within the third vacuum chamber and a mass analyzer being disposed within the fourth vacuum chamber.
4. The multimode mass spectrometry system of claim 3, wherein the second, third and fourth vacuum chambers are in sequential communication with a molecular pump and a backing pump, respectively;
the interior of the first vacuum chamber is sequentially communicated with a valve and an inlet of the backing pump.
5. The system of claim 1, wherein a guide is provided on the spacer, the second slide sliding up and down the guide.
6. A method of multimodal mass spectrometry using the multimodal mass spectrometry system of any of claims 1 to 5, the method of multimodal mass spectrometry comprising:
in the first mode: vacuumizing a first vacuum chamber and a second vacuum chamber, wherein the pressure in the first vacuum chamber is higher than the pressure in the second vacuum chamber; the second through hole is communicated with the first through hole;
ions emitted by the first ion source enter the transmission rod in the first vacuum chamber, and then sequentially pass through the second through hole and the first through hole to enter the transmission rod in the second vacuum chamber;
in the second mode: the second vacuum chamber is vacuumized, and the first vacuum chamber is communicated with the outside atmosphere; the first sliding piece moves upwards, and the second sliding piece moving upwards along the surface of the isolating piece closes the first through hole;
the second ion source operates.
7. The method of claim 6, wherein in the first mode, the ions pass sequentially through transport rods in the second and third vacuum chambers before entering the mass analyser in the fourth vacuum chamber;
in the second mode, ions emitted by the second ion source enter the transmission rod in the third vacuum chamber after being deflected, and then enter the mass analyzer in the fourth vacuum chamber.
8. The method of multimode mass spectrometry of claim 6, wherein in the second mode the first vacuum chamber is not evacuated.
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| CN202011643590.1A CN112798677A (en) | 2020-12-31 | 2020-12-31 | Multi-mode mass spectrometry system and method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011643590.1A CN112798677A (en) | 2020-12-31 | 2020-12-31 | Multi-mode mass spectrometry system and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022258966A1 (en) * | 2021-06-08 | 2022-12-15 | Micromass Uk Limited | Vacuum system for a mass spectrometer |
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| WO2009031179A1 (en) * | 2007-09-04 | 2009-03-12 | Shimadzu Corporation | Mass spectrometer |
| US20140217279A1 (en) * | 2011-06-03 | 2014-08-07 | Micromass Uk Limited | Aperture Gas Flow Restriction |
| CN104347343A (en) * | 2014-09-30 | 2015-02-11 | 聚光科技(杭州)股份有限公司 | Analysis device and method |
| WO2017046849A1 (en) * | 2015-09-14 | 2017-03-23 | 株式会社日立ハイテクノロジーズ | Mass spectrometer |
| CN112147264A (en) * | 2020-09-21 | 2020-12-29 | 聚光科技(杭州)股份有限公司 | Combined system of chromatography and mass spectrometry |
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2020
- 2020-12-31 CN CN202011643590.1A patent/CN112798677A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009031179A1 (en) * | 2007-09-04 | 2009-03-12 | Shimadzu Corporation | Mass spectrometer |
| US20140217279A1 (en) * | 2011-06-03 | 2014-08-07 | Micromass Uk Limited | Aperture Gas Flow Restriction |
| CN104347343A (en) * | 2014-09-30 | 2015-02-11 | 聚光科技(杭州)股份有限公司 | Analysis device and method |
| WO2017046849A1 (en) * | 2015-09-14 | 2017-03-23 | 株式会社日立ハイテクノロジーズ | Mass spectrometer |
| CN112147264A (en) * | 2020-09-21 | 2020-12-29 | 聚光科技(杭州)股份有限公司 | Combined system of chromatography and mass spectrometry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022258966A1 (en) * | 2021-06-08 | 2022-12-15 | Micromass Uk Limited | Vacuum system for a mass spectrometer |
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