CN113488371A - Ion interface device and plasma-mass spectrometry system - Google Patents
Ion interface device and plasma-mass spectrometry system Download PDFInfo
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- CN113488371A CN113488371A CN202110549674.7A CN202110549674A CN113488371A CN 113488371 A CN113488371 A CN 113488371A CN 202110549674 A CN202110549674 A CN 202110549674A CN 113488371 A CN113488371 A CN 113488371A
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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
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/062—Ion guides
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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
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/067—Ion lenses, apertures, skimmers
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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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Abstract
本发明提供了离子接口装置及等离子体‑质谱分析系统，所述离子接口装置包括：沿着第一部分的中心轴线方向，所述第一部分的内径和外径之间逐渐变大，所述第一部分的尖端具有通孔；第二部分呈筒形，设置在所述第一部分的远离所述尖端的一侧；所述第二部分和第一部分连接或具有缝隙，所述第二部分的内径大于所述通孔的直径。本发明具有抑制离子发散等优点。
The present invention provides an ion interface device and a plasma-mass spectrometry system. The ion interface device includes: along the direction of the central axis of the first part, the inner diameter and the outer diameter of the first part gradually become larger, the first part The tip has a through hole; the second part is cylindrical and is arranged on the side of the first part away from the tip; the second part and the first part are connected or have a gap, and the inner diameter of the second part is larger than that of the first part. the diameter of the through hole. The present invention has the advantages of suppressing ion dispersion and the like.
Description
Technical Field
The present invention relates to mass spectrometry, and more particularly to an ion interface device and a plasma-mass spectrometry system.
Background
Inductively coupled plasma mass spectrometry (ICP-MS) has high sensitivity, wide linear range, simultaneous detection of multiple elements and small sample consumption, is suitable for measuring a large number of samples, and is widely applied to the fields of life science, earth science, environmental analysis, food science, petroleum industry, metallurgical analysis and the like.
In an ICP-MS instrument, an interface is a key technology and directly determines the performance of the ICP-MS in various aspects. The plasma is operated above 6000 degrees celsius and the ion focusing device is operated at temperatures near room temperature as if the earth were to be placed half a mile away from the sun. In addition to the large temperature difference, the pressure required for plasma operation is much higher than the vacuum environment required for the ion lens and mass spectrometer sections. The interface portion allows the plasma and the ion lens system to coexist, and ions generated by the plasma action can pass through the interface to reach the ion lens region. This interface consists of 2-3 inverted funnel type devices, called cones.
Until recently, almost all ICP-MS systems on the market used a funnel-shaped cone design, as shown in fig. 1, which requires that the ion beam exiting the interface region must be focused, since the plasma (at the ICP edge of the sampling cone) is operated at atmospheric pressure while the lens and mass analyzer (at the MS edge of the skimmer cone) that filter non-ionized species and photons are operated at very low pressure, which causes the ion beam to exhibit a funnel-shaped expansion divergence. Such focusing can be achieved using a single or a series of charged devices, referred to as "ion extraction lenses".
Yet another approach to ion beam focusing is to use three cones. When using a biconic design, only a two-step pressure reduction can be performed between the plasma and the ion lens, which results in a significant divergence of the ion beam as it leaves the second cone. The triple cone design of the interface provides a good reduction in divergence of the ion beam passing through the interface region. The third cone, called the super-skimmer cone, as shown in fig. 2, allows for a three-step pressure reduction between the plasma and the quadrupole rods for filtering, thereby substantially reducing the divergence of the generated ion beam. By adopting the three-cone design, an ion extraction lens can be omitted, better ion transmission is obtained, the long-distance stability is improved, and the instrument maintenance is reduced. In a three-cone design, no one cone would require a voltage to be applied as would an extraction lens. Since these cones are uncharged (are charge neutral), their surface can be made of any material without significantly affecting their function. Furthermore, experience has shown that a triple cone design does not require more maintenance than a double cone design.
Whether the design of a bicone and an ion extraction lens or a tricone design, the existing cone is funnel-shaped, and the problem of serious ion beam divergence exists.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides an ion interface device.
The purpose of the invention is realized by the following technical scheme:
an ionic interface device, comprising:
the first part is gradually enlarged between the inner diameter and the outer diameter along the central axis direction of the first part, and the tip of the first part is provided with a through hole;
a second portion, the second portion being cylindrical and disposed on a side of the first portion remote from the tip; the second part and the first part are connected or provided with a gap, and the inner diameter of the second part is larger than that of the through hole.
The invention also aims to provide a method for measuring trace elements by using the ion interface device, and the aim is realized by the following technical scheme:
the plasma-mass spectrometry system comprises a rectangular tube and a sampling cone; the sampling cone adopts the ion interface device.
Compared with the prior art, the invention has the beneficial effects that:
1. the ion divergence is inhibited;
when the ion beam enters the interior of the first part through the through hole of the first part and continues to be transmitted, the divergence of the ion beam is restrained by the mechanical constraint of the second part, and the ion divergence is restrained without applying a voltage to the first part and the second part;
2. the working modes are various;
focusing the internally transported ion beam with an electric potential when the second portion is positively charged;
when the second portion is charged with a negative voltage, the ions can be accelerated, allowing more ions to pass through the cone aperture, thereby increasing sensitivity.
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 diagram of a sampling cone according to the prior art;
FIG. 2 is another schematic diagram of a sampling cone according to the prior art;
fig. 3 is a schematic structural view of an ion interface device according to embodiment 1 of the present invention;
fig. 4 is a schematic structural diagram of an ion interface device according to embodiment 2 of the present invention.
Detailed Description
Fig. 3-4 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 explaining the technical solution of 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 an ion interface device according to an embodiment of the present invention, and as shown in fig. 1, the ion interface device includes:
the first part is gradually enlarged between the inner diameter and the outer diameter along the central axis direction of the first part, and the tip of the first part is provided with a through hole;
a second portion, the second portion being cylindrical and disposed on a side of the first portion remote from the tip; the second part and the first part are connected or provided with a gap, and the inner diameter of the second part is larger than that of the through hole.
To reduce ion divergence, further, the central axes of the first and second portions are collinear.
In order to provide the interface device with more functions, the ion interface device further comprises:
a power supply that focuses ions when a positive voltage is applied to the second portion, or accelerates ions when a negative voltage is applied.
Example 2:
an application example of the ion interface device according to embodiment 1 of the present invention to a plasma-mass spectrometry system.
In the application example, the plasma-mass spectrometry system comprises a vacuum chamber, the horizontally arranged vacuum chamber is divided into a plurality of vacuum chambers connected in series and communicated with each other, and the ion deflection lens group, the transmission lens and the mass analyzer are sequentially arranged in each vacuum chamber;
the cavity is arranged at the lower side of the vacuum chamber with the ion deflection lens group, the cavity is of a cylindrical structure and is provided with a first side wall and a second side wall which are opposite and parallel, and a side door is arranged on the front side wall of the cavity; the first side wall and the second side wall are provided with horizontal guide rails which extend forwards and backwards and have the same height, specifically, slide ways are adopted, the end parts of the guide rails are provided with limiting parts, such as steps, so that the sliding parts are prevented from further sliding inwards, and the sampling cone is ensured to be positioned on the upper side of the torch tube which is vertically arranged; the first side wall and the second side wall are respectively provided with a gas outlet, the central axes of the two gas outlets are collinear, and both the gas outlets penetrate through the coil of the torch tube and have the same height with the coil;
the heat dissipation module is a disc-shaped water cooling module, the center of the heat dissipation module is of a cylindrical structure with internal threads, and the heat dissipation module is provided with an annular step; the sampling cone is arranged on the annular step; a compression ring with an external thread matched with the internal thread compresses the sampling cone; the heat dissipation module is fixed on the bearing piece, the end part of the bearing piece is fixed on the sliding piece through a rotating shaft, and the rotating shaft is perpendicular to the extending direction of the sliding piece and parallel to the extending direction of the guide rail, so that the bearing piece rotates around the rotating shaft, and the downward heat dissipation module can be turned upwards; the sliding parts are arranged on the guide rails of the first side wall and the second side wall and slide along the guide rails, and the distance between the end parts of the two sliding parts is equal to the distance between the first side wall and the second side wall; the end parts of the bearing parts, which are adjacent to the first side wall and the second side wall, are arranged on the guide rail, so that the central axis of the sampling cone is vertical;
the sampling cone comprises a first part and a second part, the distance between the inner diameter and the outer diameter of the first part becomes larger gradually along the direction of the central axis of the first part, the tip of the first part is provided with a through hole, and the diameter of the through hole is 0.2-2 mm; the second part is cylindrical and is arranged on one side of the first part far away from the tip; the second part is connected with the first part, the inner diameter of the second part is larger than the diameter of the through hole, and ions pass through the through hole and enter the first part, then pass through the second part and finally enter the vacuum cavity; the inner diameter of the second part is 1-100mm, the thickness is 0.1-10mm, and the length is 1-100 mm; in this embodiment, as shown in fig. 3, the sampling cone is made of high-purity nickel, the diameter of the through hole of the first portion 11 is 0.5mm, the vertex angle of the cone of the first portion 11 is 60 degrees, the inner diameter of the second portion 12 is 10mm, and the length is 10 mm;
the bottom walls of the guide rails on the first side wall and the second side wall are respectively provided with two grooves which are positioned at the lower sides of the end parts of the bearing parts arranged on the guide rails, which are adjacent to the first side wall and the second side wall, the two supporting parts are positioned in the grooves and penetrate through the two limiting grooves of the side walls, the two supporting parts are connected together outside the chamber, and the bottom ends of the supporting parts outside the chamber are fixed with bearings; the top walls of the two grooves are consistent in height, and the bottom walls of the two grooves are consistent in height, so that when the two supporting pieces are positioned in the guide rail grooves, the parts of the supporting pieces penetrating through the limiting grooves are positioned at the bottom walls, the central axes of the sampling cones are vertical, and the sliding of the sliding pieces on the guide rails cannot be hindered; when the part of the supporting piece penetrating through the limiting groove is positioned on the top wall, the heights of the tops of the two supporting pieces positioned on the inner side of the side wall of the chamber are consistent, so that the heat dissipation module is kept horizontal, namely the central axis of the sampling cone is kept vertical; the width of the part of the supporting piece penetrating through the limiting groove is consistent with that of the limiting groove, so that the supporting piece is prevented from horizontally translating;
rotating shafts are arranged on the outer walls of the first side wall and the second side wall, one end of a rotating arm rotates around the rotating shafts in the positive direction and the positive direction, and the bearing is arranged in a groove in the middle of the rotating arm; the power unit adopts the cylinder, sets up the downside of the other end of rotor arm, drive the rotor arm is around axis of rotation forward and direction rotation: when rotating in the forward direction, the bearing converts the rotation of the rotating arm into a vertical translation of the support without a horizontal translation; the support piece in the groove of the bottom wall of the guide rail moves upwards, and the end parts of the support bearing piece respectively adjacent to the first side wall and the second side wall vertically move upwards, so that the upper end of the bearing piece and a vacuum chamber with the ion deflection lens group are sealed, and the central axis of the sampling cone is always vertical.
An inelastic voltage contact mounted on the upper side of the carrier,
a vacuum elastic voltage contact installed at the lower side of the vacuum chamber
The main control board is arranged on the upper side of the vacuum cavity, conducts voltage through the vacuum electrode, and loads the voltage onto the vacuum elastic voltage contact in a wiring mode inside the vacuum cavity; the interface and the extraction lens are conducted by applying voltage, and are not interfered by the radiation of the ion source.
The working method of the inductive coupling plasma mass spectrometer based on the vertical torch tube comprises the steps of installing and maintaining a sampling cone and analyzing a sample;
the sampling cone is installed as follows:
the bearing piece is turned over for a circle around the rotating shaft in the positive direction, the heat dissipation module faces upwards, and the sampling cone is installed;
the bearing piece is reversely turned for a circle around the rotating shaft, the heat dissipation module and the sampling cone face upwards, the bearing piece is pushed inwards, the sliding piece and the end part of the bearing piece slide inwards on the guide rail and are finally blocked by the step, and at the moment, the end part of the bearing piece sliding on the guide rail is positioned on the upper side of the supporting piece of the bottom wall of the guide rail;
closing the side door;
outside the cavity, the air cylinder pushes against the other end of the rotating arm to move upwards, the supporting pieces connected together outside the cavity are pushed to vertically move upwards in the guide groove, the supporting pieces inside the cavity support the end part of the bearing piece to move upwards until the supporting pieces move to the top wall of the guide groove, at the moment, the upper end of the bearing piece and the vacuum cavity are sealed, and the central axis of the sampling cone is vertical; the bearing piece is tightly connected with the vacuum cavity, and the inelastic voltage contact is conducted with the vacuum elastic voltage contact; applying a voltage to the interface and the extraction lens;
the maintenance of the sampling cone is as follows:
the cylinder drives the other end of the rotating arm to move downwards, the supporting piece moves downwards vertically, the bearing piece is separated from the vacuum cavity, and the inelastic voltage contact is not conducted with the vacuum elastic voltage contact;
the supporting piece in the cavity moves downwards into the guide rail comparison groove, and the end part of the bearing piece falls back onto the guide rail;
opening a side door, and pulling out the bearing piece outwards;
the bearing piece is positioned outside the cavity and rotates for a circle around the rotating shaft, so that the heat dissipation module and the sampling cone face upwards, and the sampling cone is maintained;
in sample analysis;
the sample is ionized by the flame of the torch tube, then passes through the through hole of the sampling cone and just enters the first part, and then enters the second part; the second part is arranged to inhibit ion divergence;
when the second part is applied with a positive voltage, ions are focused; when a negative voltage is applied, the ions are accelerated.
Example 3:
an example of application of the ion interface device according to embodiment 1 of the present invention to a plasma-mass spectrometry system is different from embodiment 2 in that:
as shown in FIG. 4, the sampling cone is made of high-purity nickel, the diameter of the through hole of the first part 11 is 0.5mm, the vertex angle of the cone is 60 degrees, the inner diameter of the second part 12 is 10mm, and the length of the second part is 10 mm.
Claims (10)
1. An ionic interface device, comprising:
the first part is gradually enlarged between the inner diameter and the outer diameter along the central axis direction of the first part, and the tip of the first part is provided with a through hole;
a second portion, the second portion being cylindrical and disposed on a side of the first portion remote from the tip; the second part and the first part are connected or provided with a gap, and the inner diameter of the second part is larger than that of the through hole.
2. The ionic interface device of claim 1 wherein the central axes of the first and second portions are collinear.
3. The ionic interface device of claim 1, wherein the second portion is in the shape of a hollow cylinder or a hollow truncated cone.
4. The ionic interface device of claim 1 further comprising:
a power supply that applies a positive or negative voltage to the second portion.
5. The ionic interface device of claim 1 wherein the through-hole has a diameter of 0.2-2mm, the second portion has an inner diameter of 1-100mm, a thickness of 0.1-10mm, and a length of 1-100 mm.
6. The plasma-mass spectrometry system comprises a rectangular tube and a sampling cone; the ion interface device of any one of claims 1 to 5 is used as the sampling cone.
7. The plasma-mass spectrometry system of claim 6, comprising:
a vacuum chamber in which an ion deflection lens group is disposed;
a chamber disposed at a lower side of the vacuum chamber; the cavity is provided with a side door, a first side wall and a second side wall which are opposite in position, the first side wall and the second side wall are respectively provided with a guide rail, and the guide rails are provided with limiting parts; a torch tube disposed vertically within the chamber;
the heat dissipation module is fixedly provided with a sampling cone, and the torch tube is positioned at the lower side of the sampling cone;
the two opposite sides of the bearing piece are positioned on the guide rails, and the heat dissipation module is arranged on the bearing piece; the upper side of the bearing piece is connected and sealed with the vacuum cavity; the extending direction of the guide rail is vertical to the central axis of the sampling cone;
the two ends of the sliding part are positioned on the guide rails, the bearing part is rotatably fixed on the sliding part, and the rotating shaft is perpendicular to the sliding part.
8. The plasma-mass spectrometry system of claim 7, wherein the mass spectrometer further comprises:
the supporting pieces are respectively arranged in the two grooves in the bottom wall of each guide rail and extend out of the cavity; the supporting piece in the groove is not higher than the bottom wall of the guide rail;
the first side wall and the second side wall are respectively provided with a guide mechanism, and the supporting piece moves up and down in the guide mechanisms;
and the driving structure is used for driving the supporting piece outside the cavity to move up and down in the guide mechanism, so that the supporting piece inside the cavity supports the bearing piece to move up and down.
9. The plasma-mass spectrometry system of claim 8, wherein the guide mechanism employs vertical guide grooves, the first side wall and the second side wall respectively have two guide grooves extending in a vertical direction, and top walls of the two vertical guide grooves have the same height; the support member passes through the guide groove.
10. The plasma-mass spectrometry system of claim 8, wherein the drive mechanism comprises:
the rotating arm rotates around a rotating shaft, and the rotating shaft is fixed on the first side wall and the second side wall respectively; a bearing is arranged at the bottom end of the supporting piece which penetrates through the guide groove and extends out of the cavity, and the middle part of the rotating arm supports the bearing;
a power unit driving the rotary arm to rotate in forward and reverse directions around a rotation axis.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011616670 | 2020-12-31 | ||
| CN2020116166708 | 2020-12-31 |
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| CN113488371A true CN113488371A (en) | 2021-10-08 |
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Citations (6)
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| CN85202304U (en) * | 1985-06-13 | 1986-04-02 | 南京工学院 | Auti-interference ion seperating device |
| CN101281165A (en) * | 2008-05-15 | 2008-10-08 | 复旦大学 | Ionization method and device for mass spectrometry sample |
| CN103681204A (en) * | 2012-09-08 | 2014-03-26 | 复旦大学 | Ion transmission system for inductively coupled plasma mass spectrometry |
| JP2014107012A (en) * | 2012-11-22 | 2014-06-09 | Shimadzu Corp | Icp mass spectrometer |
| CN106960777A (en) * | 2016-12-31 | 2017-07-18 | 宁波华仪宁创智能科技有限公司 | Mass spectrometry system and its method of work |
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-
2021
- 2021-05-20 CN CN202110549674.7A patent/CN113488371A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| CN85202304U (en) * | 1985-06-13 | 1986-04-02 | 南京工学院 | Auti-interference ion seperating device |
| CN101281165A (en) * | 2008-05-15 | 2008-10-08 | 复旦大学 | Ionization method and device for mass spectrometry sample |
| CN103681204A (en) * | 2012-09-08 | 2014-03-26 | 复旦大学 | Ion transmission system for inductively coupled plasma mass spectrometry |
| JP2014107012A (en) * | 2012-11-22 | 2014-06-09 | Shimadzu Corp | Icp mass spectrometer |
| CN106960777A (en) * | 2016-12-31 | 2017-07-18 | 宁波华仪宁创智能科技有限公司 | Mass spectrometry system and its method of work |
| CN108152358A (en) * | 2017-12-30 | 2018-06-12 | 杭州谱育科技发展有限公司 | Plasma-mass spectrometry system and its method of work |
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