CN110085504B - Ion source system based on small-hole in-situ sampling interface and miniaturized mass spectrometer - Google Patents
Ion source system based on small-hole in-situ sampling interface and miniaturized mass spectrometer Download PDFInfo
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- CN110085504B CN110085504B CN201910383449.3A CN201910383449A CN110085504B CN 110085504 B CN110085504 B CN 110085504B CN 201910383449 A CN201910383449 A CN 201910383449A CN 110085504 B CN110085504 B CN 110085504B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
Abstract
The invention discloses an ion source system based on a small-hole in-situ sampling interface and a miniaturized mass spectrometer. Only a vacuum ion source is adopted, wherein the vacuum ion source is connected with a sample to be detected through a small hole, and the method can be suitable for detecting gaseous samples. The mass spectrometer provided by the invention utilizes the small hole as the in-situ sampling interface, the conductance of the mass spectrometer is kept constant during working, the mass discrimination effect in the sampling process can be quantitatively calibrated, the sampling transmission path is short, the mass spectrometer can quickly respond, the number of ions in the detection device can be increased by adopting internal ionization, the stability of vacuum degree can be ensured by continuous sampling, and the scanning speed of the mass spectrometer can be improved.
Description
Technical Field
The invention relates to the field of mass spectrometry, in particular to an ion source system based on an in-situ sampling interface of a small hole and a miniaturized mass spectrometer.
Background
A mass spectrometer is an instrument that can measure the partial pressure of a gas mixture. The method has wide application in the aspects of homeland safety, environmental detection, space exploration, medical health and the like. The mass spectrometer mainly comprises an ionization device, a detector and an ion binding structure. Mainly divided into quadrupole mass spectrometers, ion trap mass spectrometers, time-of-flight mass spectrometers and the like according to structure and principle.
In recent years, due to the increasing demand for on-line rapid detection and on-site real-time analysis, a miniaturized mass spectrometer is convenient to carry and can meet the demand for on-site analysis, so that the miniaturized mass spectrometer becomes one of the research hotspots in the international mass spectrometry field. Too high interface gas pressure for in situ analysis is one of the major limitations of small mass spectrometers. Because of the limited pumping capacity of small mass spectrometers, the gas flow into the vacuum system must be reduced to a very low level, and the in-situ sampling interface has two major effects, flow limitation and gas transport in the mass spectrometer. So far, the in-situ sampling interface of the miniature mass spectrometer only has two modes of a discontinuous atmospheric pressure interface and a continuous atmospheric pressure interface developed by universities. The discontinuous atmospheric pressure interface needs to sample in a discontinuous mode in order to guarantee the vacuum degree requirement, the sampling time is short, the scanning speed and the system stability are reduced, the continuous atmospheric pressure interface adopts a capillary as an interface element, continuous sampling can be carried out, but a transmission path is increased, so that the sample loss is high, and the response time is long. So far, there are two ionization methods for miniaturized mass spectrometers: first, external ionization, and second, internal ionization. Internal ionization can only be used for gaseous samples, while external ionization is rarely used in miniaturized mass spectrometers due to the requirements of ion transport efficiency and vacuum.
Disclosure of Invention
In order to overcome a series of technical defects of low scanning speed, poor system stability or long transmission path and slow response time of an in-situ sampling interface of the existing miniature mass spectrometer, the invention provides an in-situ sampling interface system with wider applicability, and aims to provide an ion source system based on a small-hole in-situ sampling interface; it is another object of the present invention to provide a miniaturized mass spectrometer.
The ion source system of the in-situ sampling interface provided by the invention comprises a vacuum ion source, wherein a sample to be detected is connected to the upstream of the vacuum ion source.
In the ion source system, the vacuum ion source is connected with the sample to be detected through the graphene small hole.
Preferably, the small holes are graphene small holes, the small holes are always in a molecular flow state in the sampling process, and the conductance value of the small holes is kept constant.
The conductance value of the small hole is designed according to the pressure of the sampled gas, so that the conductance value is constant in the sampling process, and the requirement of the working vacuum degree of a mass spectrometer is met.
The conductance and the required total area of the orifice are determined in the following manner:
the effective pumping speed of the vacuum pump is Se, the pressure inside the vacuum cavity is Pv, the pressure atmosphere of the sample to be detected is Po, and the conductance of the small hole is C. When the system is stable, the amount of gas entering the vacuum cavity through the small hole is equal to the amount of gas pumped out through the vacuum pump:
C(Po-Pv)＝SePv (1)
by measuring the values of the other three parameters, the desired orifice conductance value can be obtained.
When the flow state is molecular flow, the conductance C of the small hole is as follows:
where R is the ideal gas constant, T is the temperature, M is the relative molecular mass of the gas molecules, and the desired total area A of the pores can be obtained by introducing conductance values and other known parametersO。
The miniaturized mass spectrometer provided by the invention comprises a vacuum ion source, a vacuum cavity and an air extraction system, wherein the vacuum ion source adopts the vacuum ion source system in any one of the technical schemes.
In the mass spectrometer, the vacuum ion source is arranged in a vacuum cavity of the mass spectrometer.
The in-situ sampling interface ion source system and the corresponding miniaturized mass spectrometer provided by the invention use the graphene small hole with the aperture of 2nm as the in-situ sampling interface for the first time, the conductance of the in-situ sampling interface ion source system is kept constant during working, the mass discrimination effect in the sampling process can be quantitatively calibrated, the sampling transmission path is short, the in-situ sampling interface ion source system can quickly respond, and the ion quantity in the detection device can be increased by adopting internal ionization.
In the mass spectrometer, because the conductance of the small hole can be very small, the vacuum pump with small pumping speed can meet the requirement of vacuum, and can realize continuous sample introduction to ensure the stability of vacuum degree and improve the scanning speed of the mass spectrometer.
The miniaturized mass spectrometer can be obtained by only a small amount of adjustment on the basis of the prior art, is easy to process and manufacture, and has wide application prospect.
Drawings
FIG. 1 is a schematic structural diagram of a miniaturized mass spectrometer according to a second embodiment of the present invention;
wherein the reference numbers in the figures are as follows: the system comprises a graphene in-situ sampling interface 1, a vacuum cavity 2, a detector 3, a vacuum pump 4, a mass analyzer 5 and a vacuum ion source 6.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, technical solutions of embodiments of the present invention will be described below with reference to the accompanying drawings. Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The described embodiments are only some embodiments of the invention, not all embodiments. The described embodiments are to be considered in all respects only as illustrative and not restrictive. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without any inventive step are within the scope of the present invention.
In a first embodiment of the present invention, an ion source system of an in-situ sampling interface is provided, which is a vacuum ion source disposed inside a vacuum chamber downstream of the in-situ sampling interface.
When the ion source system is used, a sample to be tested is directly sampled in situ, enters the vacuum cavity from the in-situ sampling interface, then enters the vacuum ion source, and is ionized in the vacuum ion source, so that an ionized sample can be obtained. Then the components of the sample are analyzed and detected.
As an optimal technical scheme, the vacuum ion source is connected with a sample to be detected through other small holes with fixed conductance, such as a graphene small hole.
The conductance and the required total area of the orifice are determined in the following manner:
the effective pumping speed of the vacuum pump is Se, the pressure inside the vacuum cavity is Pv, the pressure atmosphere of the sample to be detected is Po, and the conductance of the small hole is C. When the system is stable, the amount of gas entering the vacuum cavity through the small hole is equal to the amount of gas pumped out through the vacuum pump:
C(Po-Pv)＝SePv (1)
by measuring the values of the other three parameters, the desired orifice conductance value can be obtained.
When the flow state is molecular flow, the conductance C of the small hole is as follows:
where R is the ideal gas constant, T is the temperature, M is the relative molecular mass of the gas molecules, and the desired total area A of the pores can be obtained by introducing conductance values and other known parametersO. As a preferable technical scheme, the graphene small-hole element can be selected from graphene with a uniform pore diameter of 2nm, the thickness of the graphene is in the angstrom magnitude, and the graphene can work in a molecular flow region from vacuum to atmospheric pressure.
As a preferred technical solution, the vacuum ion source may be any one of the existing vacuum ion sources, and the vacuum ion source system includes, but is not limited to, an electron bombardment ion source, a plasma discharge ionization source, a glow discharge electron bombardment ion source or an ultraviolet lamp discharge ionization source.
A second embodiment of the present invention provides a miniaturized mass spectrometer, as shown in fig. 1, the miniaturized mass spectrometer of the vacuum ion source system based on the small-hole in-situ sampling interface includes a vacuum cavity 2, a detector 3 and a mass analyzer 5 are disposed inside the vacuum cavity 2, a vacuum ion source 6 and other conventional analyzing devices and detecting devices are disposed inside the mass analyzer 5, a vacuum pump 4 with a small pumping speed is used to provide a required vacuum degree inside the vacuum cavity, and the vacuum ion source 6 is connected with a sample to be measured through an AAO in-situ sampling interface 1.
As a preferable technical scheme, the graphene small-hole element can be selected to have a uniform pore diameter of 2nm, the thickness of graphene is in the angstrom level, and the graphene small-hole element can work in a molecular flow region from vacuum to atmospheric pressure.
As a preferred technical solution, the vacuum ion source may be any one of the existing vacuum ion sources, and the vacuum ion source system includes, but is not limited to, an electron bombardment ion source, a plasma discharge ionization source, a glow discharge electron bombardment ion source or an ultraviolet lamp discharge ionization source.
When the miniaturized mass spectrometer is used for detecting a sample, the sample to be detected enters the vacuum cavity 2 through the graphene pore in-situ sampling interface 1, then enters the vacuum ion source 6 to ionize the sample to be detected, ions obtained through ionization firstly enter the mass analyzer 5, and then enter the detector 3 to analyze and detect.
Claims (2)
1. An ion source system based on an in-situ sampling interface of a small hole comprises a vacuum ion source and is characterized in that the vacuum ion source is connected with a sample to be detected through the in-situ sampling interface, a graphene small hole element with the aperture of 2nm is selected as the small hole, the thickness magnitude of graphene is in the angstrom magnitude, the graphene is always in a molecular flow state from vacuum to atmosphere sampling, a conductance value is kept constant, and a quality discrimination effect in the sampling process can be calibrated.
2. A miniaturized mass spectrometer comprises an ion source and a vacuum cavity, wherein the ion source adopts the ion source system of claim 1, and is characterized in that a graphene pore element with the pore diameter of 2nm is selected as a pore, the thickness of graphene is in the angstrom level, the graphene is in a molecular flow state all the time from vacuum to atmosphere sampling, the conductance value is kept constant, and the mass discrimination effect in the sampling process can be calibrated.
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| CN102800554A (en) * | 2012-09-02 | 2012-11-28 | 王利兵 | Multimode ionization method |
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| CN104576287A (en) * | 2013-10-16 | 2015-04-29 | 北京理工大学 | Ion source system and mass spectrometer for atmospheric pressure interface |
| CN104637774A (en) * | 2013-11-08 | 2015-05-20 | 中国科学院大连化学物理研究所 | Electrospray ion leading-in device |
| CN105702553A (en) * | 2016-04-19 | 2016-06-22 | 东华理工大学 | Ion mobility spectrometer and carrier gas flow control method thereof |
| CN106340437A (en) * | 2015-07-09 | 2017-01-18 | 株式会社岛津制作所 | Mass spectrometer and method used to reduce ion loss and post-stage vacuum load |
| CN108439377A (en) * | 2018-05-18 | 2018-08-24 | 浙江大学 | It is a kind of to cooperate with processing organic liquid waste using non-thermal plasma trap and prepare the device and method of graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10204774B2 (en) * | 2014-05-22 | 2019-02-12 | W. Henry Benner | Instruments for measuring ion size distribution and concentration |
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Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0962958A1 (en) * | 1998-06-01 | 1999-12-08 | The Institute Of Physical & Chemical Research | Ion scattering spectrometer |
| EP2378539A2 (en) * | 2010-04-19 | 2011-10-19 | Hitachi High-Technologies Corporation | Mass spectrometer |
| CN102800554A (en) * | 2012-09-02 | 2012-11-28 | 王利兵 | Multimode ionization method |
| CN104465296A (en) * | 2013-09-13 | 2015-03-25 | 岛津分析技术研发（上海）有限公司 | Ion transmission apparatus and ion transmission method |
| CN104576287A (en) * | 2013-10-16 | 2015-04-29 | 北京理工大学 | Ion source system and mass spectrometer for atmospheric pressure interface |
| CN104637774A (en) * | 2013-11-08 | 2015-05-20 | 中国科学院大连化学物理研究所 | Electrospray ion leading-in device |
| CN106340437A (en) * | 2015-07-09 | 2017-01-18 | 株式会社岛津制作所 | Mass spectrometer and method used to reduce ion loss and post-stage vacuum load |
| CN105702553A (en) * | 2016-04-19 | 2016-06-22 | 东华理工大学 | Ion mobility spectrometer and carrier gas flow control method thereof |
| CN108439377A (en) * | 2018-05-18 | 2018-08-24 | 浙江大学 | It is a kind of to cooperate with processing organic liquid waste using non-thermal plasma trap and prepare the device and method of graphene |
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