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CN110233094B - Ion source, working method and application thereof - Google Patents

Ion source, working method and application thereof Download PDF

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Publication number
CN110233094B
CN110233094B CN201910626284.8A CN201910626284A CN110233094B CN 110233094 B CN110233094 B CN 110233094B CN 201910626284 A CN201910626284 A CN 201910626284A CN 110233094 B CN110233094 B CN 110233094B
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China
Prior art keywords
groove
ion source
pair
electrode
protrusions
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CN110233094A (en
Inventor
闻路红
洪欢欢
余晓梅
邵科敏
李文
范国正
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China Innovation Instrument Co ltd
Ningbo University
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China Innovation Instrument Co ltd
Ningbo University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • H01J49/16Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
    • H01J49/165Electrospray ionisation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • H01J49/16Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
    • H01J49/165Electrospray ionisation
    • H01J49/167Capillaries and nozzles specially adapted therefor

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention provides an ion source, a working method and application thereof, wherein the ion source comprises a capillary tube and a discharge electrode; the base body is provided with a body and an extension part; one end of the capillary tube is fixed in the extension part, and the other end extends out of the extension part; one end of the discharge electrode is exposed in the first groove of the body, and the other end of the discharge electrode is positioned in the capillary tube; the guide piece comprises an upper part and a lower part which are arranged up and down; the lower side of the upper part is provided with a second groove, and the connecting electrode extends into the second groove; the lower part is provided with a third groove which is arranged opposite to the second groove; the third groove comprises a first part, a slope and a second part which are sequentially arranged, and the second part is higher than the first part; the distance between the upper wall of the second portion and the bottom wall of the third recess is not less than the thickness. The invention has the advantages of good reliability, low cost, simple operation, good detection parallelism and the like.

Description

Ion source, working method and application thereof
Technical Field
The invention relates to an ion source, in particular to an ion source, a working method and application thereof.
Background
Electrospray ion sources (Electron Spray Ionization) are widely applied to mass spectrometry in recent years, are suitable for analyzing compounds with slightly smaller polarity, can also be used for analyzing macromolecules such as polypeptides, proteins and the like, and have the advantages of high ionization efficiency and stable spraying, but also have the problems of slightly complex pretreatment and sample adsorption and dead volume. In addition to nano-esi, conventional esi requires a large amount of sample and is economically disadvantageous.
In this context, pulsed DC ion sources (PDESI) have been developed to ionize the liquid under test by pulsed electrospray by applying a DC high voltage to the electrodes to generate an electrostatic field.
By adjusting the applied voltage intensity, the control of the pulse electrospray frequency is realized, the ion source can effectively solve the problems of dead volume and sample adsorption existing in the traditional electrospray ion source, the economy of a sample is greatly improved, the spray flow rate of electrospray is greatly reduced, the spray duration of electrospray is prolonged, and the analysis requirement of tandem mass spectrometry is fully ensured. However, there are disadvantages to this ion source, such as:
the difficulty in changing the capillary needle, the unprotected tip of the capillary, improper handling, and uncertainty in the fixed position of each mount PDESI to the mobile station result in poor test parallelism and long time.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the ion source which has good reliability, low cost, good suitability with other mass spectra and simple operation.
The invention aims at realizing the following technical scheme:
An ion source comprising a capillary and a discharge electrode; the ion source further comprises:
A base body having a body and an extension portion, the discharge electrode being insulated from the base body; one end of the capillary tube is fixed in the extension part, and the other end extends out of the extension part; the body is provided with a first groove, one end of the discharge electrode is exposed in the first groove, and the other end of the discharge electrode is positioned in the capillary tube;
A guide member including upper and lower portions disposed up and down; the lower side of the upper part is provided with a second groove, and the connecting electrode is arranged on the upper part and extends into the second groove; the lower part is provided with a third groove which is arranged opposite to the second groove; the third groove comprises a first part, a slope and a second part which are sequentially arranged, and the second part is higher than the first part; the distance between the upper wall of the second part and the bottom wall of the third groove is not smaller than the thickness of the body.
The invention also aims to provide application of the ion source in a pulse direct current ion source.
The invention also aims to provide a working method of the ion source, and the aim of the invention is realized by the following technical scheme:
The working method of the ion source comprises the following steps:
(A1) A first portion for positioning the substrate within the third recess;
(A2) Pushing the substrate, sliding the substrate up the ramp and into the second portion;
the connecting electrode and the matrix relatively move;
(A3) The connecting electrode enters the first groove and is contacted with the discharge electrode in the first groove; the base is captured between the second portion and the second recess.
Compared with the prior art, the invention has the following beneficial effects:
1. The reliability is good;
By arranging the third groove as the first part and the second part with different heights and by slope transition, the substrate is firmly clamped between the second part and the second groove (can not shake in the up-down direction) and blocked (in the left-right direction), the reliability of the substrate, namely the capillary tube, being fixed is improved, and the accuracy of subsequent mass spectrometry is correspondingly improved;
2. the structure is simple;
the matrix, the capillary tube and the discharge electrode can be formed at one time, for example, the capillary tube and the discharge electrode are fixed, and insulating materials are poured, so that the cost is low, and the manufacturing is convenient and quick;
The guide piece adopts an upper and lower detachable structure, so that the processing, the manufacturing and the assembly are convenient;
3. the adaptability is good;
The ion source can be combined with most of the existing mass spectrums, the original ESI source of the mass spectrums can be replaced in a lossless manner, a mass spectrum interface with a three-dimensional moving platform is used for fixing, and the operation can be performed by means of high ESI pressure of the mass spectrums or high pressure of a self-contained control box;
4. The operation is simple and convenient, the guide piece is put into a groove of the guide piece and pushed to a designated position to replace the insertion action, the fool-proof design is provided, and the mass spectrum and PDESI ion source needle points are prevented from being damaged by misoperation;
5. The capillary tube, the substrate and the discharge electrode form disposable consumable materials without independently replacing the capillary tube, the substrate and the discharge electrode, the single consumable material with low cost is less than 3 yuan, and the disposable consumable material is convenient and quick to use;
6. the detection parallelism is good, and the rigid stable connection among the devices ensures the detection parallelism, and the average RSD value is within 3% -10%.
Drawings
The present disclosure will become more readily understood with reference to the accompanying drawings. As will be readily appreciated by those skilled in the art: the drawings are only for illustrating the technical scheme 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 an ion source according to an embodiment of the present invention;
FIG. 2 is a simplified cross-sectional view of an ion source according to an embodiment of the present invention;
Fig. 3 is another schematic cross-sectional view of an ion source according to an embodiment of the invention.
Detailed Description
Figures 1-3 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. In order to teach the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will appreciate variations or alternatives derived from these embodiments that fall 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 invention is not limited to the following alternative embodiments, but only by the claims and their equivalents.
Example 1
Fig. 1 to 3 schematically show a schematic structure of an ion source according to embodiment 1 of the present invention, as shown in fig. 1 to 3, the ion source comprising:
A capillary tube 32 and a discharge electrode 31, wherein the outer diameter of the capillary tube 32 is 1mm-2mm, the inner diameter is 0.5mm-1.5mm, and the diameter of the discharge electrode 31 is 0.2mm-1mm;
A base body made of an insulating material and having a body 11 and an extension 12; one end of the capillary tube 32 is fixed in the extension 12, and the other end extends out of the extension 12; the body is provided with a first groove 21 and a fourth groove 22, one end of the discharge electrode 31 is exposed in the first groove 21, the other end of the discharge electrode 31 passes through and protrudes out of the extension part 12, and the discharge electrode 31 is positioned in the capillary 32; the fourth recess 22 extends in a direction parallel to the extending direction of the discharge electrode 31, and the tip communicates with the first recess 21 such that the connection electrode 61 relatively moves into the first recess 21 within the fourth recess 22 and contacts the discharge electrode 31;
The guide member, as shown in fig. 3, comprises an upper part 51 and a lower part 52 which are arranged up and down, and the upper part 51 and the lower part 52 are fixed together through a connecting member such as a screw, so that the guide member can be conveniently detached; the lower side of the upper part 51 has a second groove 71, and the connection electrode 61 is disposed at the upper part and extends into the second groove 71; the lower part 52 is provided with a third groove 81 arranged opposite to the second groove 71, the third groove 81 comprises a first part 811, a slope 812 and a second part 813, the second part 813 is higher than the first part 811, the distance between the upper wall of the second part 813 and the bottom wall of the second groove 71 is not less than the thickness of the substrate, so that the substrate is clamped between the second part and the second groove to prevent up-and-down shaking; the width of the third recess 81 matches, e.g. is equal to, or slightly larger than, the width of the base body so that the connection electrode can enter the first recess accurately.
To further improve the reliability of the fixation, to prevent the shaking in the up-down direction, a pair of protrusions 43 are oppositely provided at both sides of the body 11, and the protrusions 43 are adapted to pass through the connection electrode 61; the extension 12, the pair of protrusions 43 and the first groove 21 are sequentially disposed; the distance between the upper wall of the second portion 813 and the bottom wall of the second groove 71 is not less than (preferably equal to) the sum of the thicknesses of the body 11 and the pair of projections 43.
In order to prevent the shaking in the left-right direction, further, a lower side of the upper portion has a first blocking portion, which is formed as a side wall of the second groove, and is blocked by the first blocking portion when the pair of protrusions moves in the second groove.
In order to further prevent rocking in the left-right direction, the body 11 has a second stopper 42, and the extension 12, the first groove 21, and the second stopper 42 are disposed in this order such that the distance between the surface of the first stopper that contacts the pair of protrusions to the surface of the connection electrode that contacts the second stopper is equal to the distance between the surface of the pair of protrusions that faces away from the second stopper to the surface of the second stopper that faces against the pair of protrusions; when the connection electrode 61 relatively moves within the first recess 21, it is blocked by the second blocking portion 42.
In order to facilitate pushing and pulling of the base body by hand, further, a side portion of the body 11 remote from one end of the discharge electrode 31 has a protrusion 41, and the protrusion 41 and the second groove 71 are located at the same side of the body, so that the protrusion 41 is easily pushed and pulled by hand.
In order to facilitate the contact between the connection electrode and the discharge electrode, further, the end 33 of the discharge electrode in the first groove is spherical, the bottom of the first groove 21 is provided with a fifth groove matched with the end of the discharge electrode, and the end 33 is completely positioned in the first groove 21.
In order to avoid contact between the connection electrode and the capillary tube during the relative movement, further, the distance from the central axis of the discharge electrode to the bottom wall of the fourth groove is not smaller than the radius of the extension portion.
The working method of the ion source provided by the embodiment of the invention comprises the following steps:
(A1) Immersing one end of the capillary tube into a sample solution, wherein the sample solution enters the end of the capillary tube but is not contacted with a discharge electrode in the capillary tube;
the base body snaps into the first portion of the third recess of the guide,
(A2) The finger presses the protruding part and pushes the base body to move, and the base body slides up the slope and enters the second part;
the connecting electrode passes between the pair of projections and relatively moves in the fourth groove;
(A3) The connecting electrode enters the first groove and is contacted with the discharge electrode in the first groove; the base body (comprising a pair of protrusions) is clamped between the second part and the second groove, so that the base body is prevented from shaking in the up-down direction;
Meanwhile, the pair of protrusions are blocked by the side wall of the second groove, and the connection electrode 61 is blocked by the second blocking portion, preventing the base from shaking in the left-right direction;
the direct-current high voltage is connected through the connecting electrode, the discharging electrode discharges, the solution in the capillary is ionized, and the solution is sprayed out of the capillary and enters mass spectrometry;
When the electrode is replaced, the convex part is pressed by hands, the substrate is pulled outwards, and the connecting electrode is separated from the discharge electrode.
Example 2
Application of the ion source according to embodiment 1 of the present invention to a pulsed dc ion source.
In this application example, the length of the capillary tube extending out of the extension is 10mm-15mm, the outer diameter is 1mm-2mm, and the inner diameter is 0.5mm-1.5mm; the distance from the end of the discharge electrode extending out of the extension part to the end of the capillary extending out of the extension part is 5mm-10mm, and the diameter is 0.2mm-1mm; the inner diameter of the capillary tube becomes smaller along the direction of the capillary tube away from the body, and the inner diameter of the end part is 10-200 mu m; the end part of the discharge electrode in the first groove is spherical, and the bottom of the fourth groove is provided with a fifth groove matched with the end part of the discharge electrode; the protruding part is arc-shaped, the second blocking part is rectangular and is positioned on the same side of the body; the distance from the central axis of the discharge electrode to the bottom wall of the fourth groove is not smaller than the radius of the extension part, namely, the outer edge of the extension part is flush with the bottom wall of the fourth groove, so that the contact of the connecting electrode and the substrate with the capillary tube is prevented when the connecting electrode and the substrate relatively move; the distance between the upper wall of the second portion and the bottom wall of the second recess is equal to the sum of the thicknesses of the body and the pair of protrusions, and the distance between the surface of the first blocking portion, which contacts the pair of protrusions, to the surface of the connection electrode, which contacts the second blocking portion, is equal to the distance between the surface of the pair of protrusions, which faces away from the second blocking portion, to the surface of the second blocking portion, which faces the pair of protrusions.
Example 3
The ion source of example 3 of the present invention is different from example 1 in that:
the pair of projections is not provided, and the distance from the upper wall of the second portion to the bottom wall of the second recess is equal to the thickness of the body.
Example 4
The ion source of example 4 of the present invention is different from example 1 in that:
The fourth groove is not arranged any more, and the characteristic that the width of the third groove is matched with the width of the matrix (such as equal width) is utilized, so that the matrix cannot shake back and forth when moving in the third groove, and the connecting electrode can accurately enter the first groove.

Claims (10)

1. An ion source comprising a capillary and a discharge electrode; the method is characterized in that: the ion source further comprises:
A base body having a body and an extension portion, the discharge electrode being insulated from the base body; one end of the capillary tube is fixed in the extension part, and the other end extends out of the extension part; the body is provided with a first groove, one end of the discharge electrode is exposed in the first groove, and the other end of the discharge electrode is positioned in the capillary tube;
A guide member including upper and lower portions disposed up and down; the lower side of the upper part is provided with a second groove, and the connecting electrode is arranged on the upper part and extends into the second groove; the lower part is provided with a third groove which is arranged opposite to the second groove; the third groove comprises a first part, a slope and a second part which are sequentially arranged, and the second part is higher than the first part; the distance between the upper wall of the second part and the bottom wall of the third groove is not smaller than the thickness of the body.
2. The ion source of claim 1, wherein: the substrate further comprises:
A pair of protrusions, which are oppositely arranged at two sides of the body, and are suitable for connecting the passage of the electrode; the extension part, the pair of protrusions and the first groove are sequentially arranged; the distance between the upper wall of the second portion and the bottom wall of the second recess is not less than the sum of the thicknesses of the body and the pair of projections.
3. The ion source of claim 2, wherein: the lower side of the upper portion has a first blocking portion that is blocked by the first blocking portion when the pair of protrusions move within the second groove.
4. The ion source of claim 3, wherein: the side wall of the second groove forms the first blocking portion.
5. The ion source of claim 3, wherein: the body is provided with a second blocking part, and the extending part, the first groove and the second blocking part are sequentially arranged; when the connection electrode moves relatively in the first groove, the connection electrode is blocked by the second blocking portion.
6. The ion source of claim 5, wherein: the distance between the surface of the first blocking part, which is contacted with the pair of protrusions, and the surface of the connecting electrode, which is contacted with the second blocking part, is equal to the distance between the surface of the pair of protrusions, which is opposite to the second blocking part, and the surface of the second blocking part, which faces the pair of protrusions.
7. Use of an ion source according to any of claims 1-6 in a pulsed dc ion source.
8. A method of operating an ion source according to any one of claims 1 to 6, the method comprising the steps of:
(A1) A first portion for positioning the substrate within the third recess;
(A2) Pushing the substrate, sliding the substrate up the ramp and into the second portion;
the connecting electrode and the matrix relatively move;
(A3) The connecting electrode enters the first groove and is contacted with the discharge electrode in the first groove; the base is captured between the second portion and the second recess.
9. The method of claim 8, wherein: a pair of projections on the base moves between the second portion and the second recess with the base passing between the pair of projections located opposite each other.
10. The method of claim 8, wherein: in the step (A3), the side walls of the second recess block the movement of the pair of projections, and the connection electrode is blocked by the second blocking portion on the base body; the side wall, the pair of protrusions, the connection electrode and the second blocking portion are arranged in order.
CN201910626284.8A 2019-07-11 2019-07-11 Ion source, working method and application thereof Active CN110233094B (en)

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CN112993637B (en) * 2021-04-26 2021-09-10 宁波华仪宁创智能科技有限公司 Gas-electricity integrated interface device, mass spectrum system and maintenance method

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US7122791B2 (en) * 2004-09-03 2006-10-17 Agilent Technologies, Inc. Capillaries for mass spectrometry
CN201185172Y (en) * 2006-12-29 2009-01-21 东华理工大学 Surface desorption atmospheric chemical ionization source
JP6106864B1 (en) * 2016-09-21 2017-04-05 ヒューマン・メタボローム・テクノロジーズ株式会社 Ion source adapter
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