CN114899077A - Integrated mass spectrum quadrupole rod - Google Patents

Integrated mass spectrum quadrupole rod Download PDF

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Publication number
CN114899077A
CN114899077A CN202210713544.7A CN202210713544A CN114899077A CN 114899077 A CN114899077 A CN 114899077A CN 202210713544 A CN202210713544 A CN 202210713544A CN 114899077 A CN114899077 A CN 114899077A
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CN
China
Prior art keywords
electrode
quadrupole
rods
rod
electrode rods
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Pending
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CN202210713544.7A
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Chinese (zh)
Inventor
胡立刚
王丁一
张亭亭
何滨
江桂斌
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Research Center for Eco Environmental Sciences of CAS
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Research Center for Eco Environmental Sciences of CAS
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Application filed by Research Center for Eco Environmental Sciences of CAS filed Critical Research Center for Eco Environmental Sciences of CAS
Priority to CN202210713544.7A priority Critical patent/CN114899077A/en
Publication of CN114899077A publication Critical patent/CN114899077A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/06Electron- or ion-optical arrangements
    • H01J49/062Ion guides
    • H01J49/063Multipole ion guides, e.g. quadrupoles, hexapoles
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/26Mass spectrometers or separator tubes
    • H01J49/34Dynamic spectrometers
    • H01J49/42Stability-of-path spectrometers, e.g. monopole, quadrupole, multipole, farvitrons
    • H01J49/4205Device types
    • H01J49/422Two-dimensional RF ion traps
    • H01J49/4225Multipole linear ion traps, e.g. quadrupoles, hexapoles

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Electron Tubes For Measurement (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention provides an integrated mass spectrum quadrupole rod, which comprises: the four electrode rods are arranged in parallel and are axially and uniformly distributed around the central line; and a plurality of fixing portions for supporting the four electrode rods at predetermined positions in the extending direction of the electrode rods; the electrode pole with fixed part integrated into one piece, the electrode pole includes: a core material and a conductive layer coated on a surface; the surface of the fixing part is coated with an insulating layer. According to the technical scheme, errors generated in assembling and production of the quadrupole rods are reduced through integral manufacturing of the quadrupole rods, and therefore the mass spectrometer applying the quadrupole rods can be used for screening ions in a preset mass-to-charge ratio range with high precision.

Description

Integrated mass spectrum quadrupole rod
Technical Field
The invention belongs to the technical field of mass spectrometry, and particularly relates to an integrated mass spectrometry quadrupole.
Background
The quadrupole coupled ICP-MS is a well established conventional trace analysis instrument. The quadrupole rods are a continuous mass filter consisting of two pairs of parallel electrode rods, and particles with different mass-to-charge ratios are separated by the interaction of a direct current electric field and an alternating current electric field. As a main accessory of the quadrupole rod, the machining and assembling precision of the electrode rod directly influences the precision and various performance indexes of the quadrupole rod mass spectrometer.
At present, a machining method of a quadrupole rod generally comprises the steps of machining four high-precision electrode rods and ceramic rings, and then manually assembling the four electrode rods and the ceramic rings which are machined into hyperboloids or circles into a complete quadrupole rod through a bolt structure according to a certain field radius. In order to ensure the function of the quadrupole rod, the existing quadrupole rod has high precision requirement, is difficult to realize mechanical batch production and has high production cost.
Disclosure of Invention
According to an embodiment of the present disclosure, an integrated mass spectrometry quadrupole is provided.
This integral type mass spectrum quadrupole rod includes: the four electrode rods are arranged in parallel and are rotationally and symmetrically distributed around the axis of the central line; a plurality of fixing portions for supporting the four electrode rods at predetermined positions in an extending direction of the electrode rods; the electrode pole with fixed part integrated into one piece, the electrode pole includes: a core material and a conductive layer coated on a surface; the surface of the fixing part is coated with an insulating layer.
Furthermore, the shape of the inner side outline of the electrode rod is any one of a single curve shape, a circle shape, an ellipse shape, a semi-circle shape or a semi-ellipse shape, and the end part of the electrode rod is provided with a through hole which is used for being connected with the conducting strip and used as an electric connection part.
Further, the core material is composed of a high molecular polymer containing a photocurable resin, polyimide, nylon powder, polycarbonate, and a ceramic compound containing alumina and zirconia.
Further, the conductive layer includes: the material of the conducting layer comprises single metal selected from gold, silver, copper and nickel and/or other metal and alloy materials with high conductivity and good stability; the smoothness of the conductive layer is equal to or lower than Ra 0.3 and the thickness of the conductive layer does not exceed 10 micrometers.
Further, an insulating layer is arranged on the surface of the fixing portion, and the insulating layer is made of an insulating material.
Further, the inner peripheral surface of the fixing portion is disposed outside the circumferential arrangement in which the 4 electrode rods are arranged, and is integrally connected to the electrode rods at a position where the inner peripheral surface of the fixing portion faces the outer side surfaces of the electrode rods.
Further, the coating includes: vacuum coating, electroplating, electroless plating, vapor deposition, thermal spraying, and plasma polymerization coating techniques.
Further, the core material and the fixing portion are integrally formed in a 3D printing mode.
According to the technical scheme, errors generated in assembling and production of the quadrupole rods are reduced through integral manufacturing of the quadrupole rods, and therefore the mass spectrometer applying the quadrupole rods can be used for screening ions in a preset mass-to-charge ratio range with high precision.
It should be understood that the statements herein reciting aspects are not intended to limit the critical or essential features of the embodiments of the present disclosure, nor are they intended to limit the scope of the present disclosure. Other features of the present disclosure will become apparent from the following description.
Drawings
The above and other features, advantages and aspects of various embodiments of the present disclosure will become more apparent by referring to the following detailed description when taken in conjunction with the accompanying drawings. The accompanying drawings are included to provide a further understanding of the present disclosure, and are not intended to limit the disclosure thereto, and the same or similar reference numerals will be used to indicate the same or similar elements, where:
FIG. 1 is a schematic diagram illustrating an integrated mass spectrometer quadrupole provided in an embodiment of the present invention;
FIG. 2 shows a schematic front view of an integrated mass spectrometer quadrupole provided by embodiments of the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present disclosure more clear, the technical solutions of the embodiments of the present disclosure will be described clearly and completely with reference to the drawings in the embodiments of the present disclosure, and it is obvious that the described embodiments are some, but not all embodiments of the present disclosure. All other embodiments, which can be derived by a person skilled in the art from the embodiments disclosed herein without making any creative effort, shall fall within the protection scope of the present disclosure.
In addition, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three kinds of relationships, for example, a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The mass spectrum quadrupole rod disclosed by the invention is provided with a core material which is integrally manufactured, and an insulating layer which is coated on a conducting layer and a fixing part of an electrode rod of the core material. Through the integral manufacture of the quadrupole rods, errors generated in the assembling and production of the quadrupole rods are reduced, and the mass spectrometer applying the quadrupole rods can be used for screening ions in a preset mass-to-charge ratio interval with high precision.
An embodiment of the present invention will be described below with reference to fig. 1 and 2. However, unless otherwise specified, the dimensions, materials, shapes, relative arrangement, and the like of the constituent components described in the embodiments do not limit the scope of the present invention.
[ structural arrangement ]
Fig. 1 and 2 illustrate an integrated mass spectrum quadrupole provided by an embodiment of the invention, which comprises an electrode rod 1 and a fixed part 2, wherein the electrode rod 1 and the fixed part 2 are manufactured in an integrated manner.
According to the embodiment of the invention, the integrated mass spectrum quadrupole rod comprises four electrode rods 1 which are arranged in parallel and are rotationally and symmetrically distributed around a central line axis, so that a structure that each electrode rod 1 is parallel to the central line axis and is arranged around the central line axis at an interval of 90 degrees, and a section symmetry axis of each electrode rod 1 points to the central line axis is formed. In the present embodiment, two fixing portions 2 are provided at predetermined positions in the extending direction of the electrode rods 1 with respect to the four electrode rods 1, and the four electrode rods 1 are supported. The inner peripheral surface of the fixing portion 2 is provided outside the circumferential row in which the 4 electrode rods 1 are arranged, and is integrally connected to the respective electrode rods 1 at a position where the inner peripheral surface of the fixing portion 2 faces the outer side surfaces of the respective electrode rods 1, and the opposing arrangement of the four electrode rods 1 is maintained by the plurality of fixing portions 2 provided at predetermined positions in the extending direction of the electrode rods 1. The fixing part 2 and the main bodies of the four electrode rods 1 are integrally formed by using the same material, and the fixing part 2 forms an avoiding gap which is concave towards the outer peripheral side at the gap between the four electrode rods 1.
The shape of the electrode rod 1 is selected from any one of a cylinder, a column, and a single-curve column, and the cross-sectional inner contour shape may be preferably any one of a single-curve shape, a circular shape, an elliptical shape, a semicircular shape, and a semi-elliptical shape, and it is particularly preferable that the cross-sectional inner contour shape is a single-curve shape. And the surface is provided with a through hole 5 which is used for being connected and fixed with the conducting strip as an electric connection part.
The electrode rod 1 includes: the electrode rod comprises a core material and a conductive layer 3 coated on the surface of the core material, a fixing part 2 comprises the core material and an insulating layer 4 coated on the surface of the core material, and the core material of the electrode rod 1 and the core material part of the fixing part 2 are integrally molded.
The core material is composed of a polymer such as a photocurable resin, polyimide, nylon powder, polycarbonate, or the like, and a ceramic compound such as alumina, zirconia, and the core material is in the shape selected from any one of a cylinder, and a single-curved cylinder, and may preferably have any one of a single-curved shape, a circular shape, an elliptical shape, a semicircular shape, and a semi-elliptical shape in cross section inside contour, and particularly preferably has a single-curved shape in cross section inside contour.
In the present embodiment, before the electrode rod 1 is coated with the conductive layer 3, the surface of the core material is subjected to ultrasonic cleaning to remove excess manufacturing material remaining on the surface of the core material. And then drying the core material at the temperature of 80 ℃ lower than the melting point of the core material, so that the burning damage to the core material is avoided while the residual moisture caused by cleaning is removed.
In this embodiment, the material of the conductive layer 3 includes metal and alloy materials with high conductivity and good stability, such as gold, silver, copper and nickel, and the smoothness of the surface of the conductive layer 3 is equal to or less than Ra 0.3, and the thickness is less than 10 micrometers.
In the present embodiment, the material of the insulating layer 4 is an insulating material, preferably rubber.
In the present embodiment, the application of the conductive layer of the electrode rod 1 includes: vacuum coating, electroplating, electroless plating, vapor deposition, thermal spraying, and plasma polymerization.
In the present embodiment, the core material and the fixing portion 2 are integrally formed by a 3D printing method.
[ operating conditions ]
Alternating current and direct current with high frequency change generated by a radio frequency power supply are respectively applied to the conducting layers 3 on the surfaces of the two pairs of electrode rods 1, the four electrode rods 1 carry direct current voltage and superposed radio frequency voltage, the electrode rods 1 of the opposite pair are equipotential, and the potentials of the two pairs of electrode rods 1 are opposite to each other to form a dynamic hyperbolic electric field. Meanwhile, the fixed part 2 supports the four electrode rods 1 and keeps the relative positions of the four electrode rods fixed, so that the stability of mass-to-charge ratio screening parameters is guaranteed. When ions with mass-to-charge ratios higher or lower than a preset value enter a dynamic hyperbolic electric field, ions which accord with the preset mass-to-charge ratio stably oscillate, pass through a quadrupole rod and reach a monitor to be detected, and ions which do not accord with the preset mass-to-charge ratio leave the electric field due to unstable oscillation and cannot reach the monitor.
According to the embodiment of the disclosure, the following technical effects are achieved:
in the embodiment, the quadrupole rods comprise four electrode rods 1 which are arranged in parallel and are rotationally and symmetrically distributed around the axis of the central line; and a plurality of fixing portions 2 for supporting the four electrode rods 1 at predetermined positions in the extending direction of the electrode rods 1 to generate a dynamic hyperbolic electric field for screening ions having a predetermined mass-to-charge ratio.
In the present embodiment, since the fixing portion 2 and the main bodies of the four electrode rods 1 are integrally molded using the same material, it is possible to form the fixing portion 2 with a relief notch recessed toward the outer peripheral side at the gap between the four electrode rods 1. Therefore, the influence of the radio frequency voltage on the fixing part 2 can be reduced as much as possible, and the heat generation of the fixing part 2 can be reduced.
In the present embodiment, the inner cross-sectional shape of the electrode rod 1 is preferably a single curved surface. The cross section shape in the single curved surface can provide the most stable hyperbolic electric field, and further stable screening of ions with preset mass-to-charge ratios is ensured.
In this embodiment, the end of the electrode rod 1 is provided with a through hole 5 serving as an electrical connection part for connecting with a conductive sheet, a conductive layer 3 is formed on the inner wall of the through hole together with the electrode rod 1, and a connecting pin is inserted into the through hole 5 to electrify the electrode rod 1, so that the plating layer of the conductive layer 3 inside the hole is easier and more uniform, stable output of alternating current and direct current with high frequency change is ensured, stable screening of preset mass-to-charge ratio ions is further ensured, and the stability of the electrode rod 1 in long-term use is ensured.
In the present embodiment, the core material is composed of a polymer such as a photocurable resin, polyimide, nylon powder, or polycarbonate, and a ceramic compound such as alumina or zirconia. The material is convenient for using the 3D printer to integrally form and manufacture the quadrupole rods.
In this embodiment, the material of the conductive layer 3 includes a single metal selected from gold, silver, copper, and nickel, and/or other metals and alloy materials with high conductivity and good stability, so as to ensure stable output of alternating current and direct current with high frequency variation, and further ensure stable screening of ions with a predetermined mass-to-charge ratio.
In the embodiment, the surface of the fixing portion 2 is coated with the insulating layer 4, and the insulating layer 4 is made of an insulating material and used for isolating interference of alternating current and direct current with high frequency change, so that overheating and surface voltage reduction of the core materials of the fixing portion 2 and the electrode rod 1 are avoided, and further screening of a dynamic hyperbolic electric field on ions with a preset mass-to-charge ratio is ensured.
In the present embodiment, the electrode rod 1 and the fixing portion 2 are integrally formed, and thus, a splicing error caused by splicing the electrode rods 1 and the fixing portion 2 and a batch error caused by batch manufacturing are reduced in separate manufacturing. The reduction of concatenation error and batch error has improved the quadrupole rod precision, and then ensures that operating condition's quadrupole rod can accurate screening accord with predetermine the ion of quality/charge ratio and pass through the quadrupole rod to be detected as the signal.
In this embodiment, the coating includes: vacuum plating, electroplating, chemical plating, vapor deposition, thermal spraying and plasma polymerization plating techniques are used for obtaining a conductive layer 3 with smoothness equal to or lower than Ra 0.3 and thickness not more than 10 micrometers, so as to ensure uniform resistance distribution in the extending direction of an electrode rod 1, reduce overheating caused by high voltage, ensure stable output of alternating current and direct current with high-frequency change and further ensure stable screening of ions with preset mass-to-charge ratio.
In this embodiment, the integrally formed mass spectrum quadrupole rods can be manufactured by 3D printing and integrally forming, and the angle of the model should be controlled during manufacturing so that the four electrode rods 1 are perpendicular to the printing platform, thereby avoiding the generation of support points on the surfaces of the electrode rods 1 and further damaging the shapes of the electrode rods 1.
The manufacturing process of the quadrupole rod reduces the production cost and the processing difficulty, and further improves the production efficiency.
In the description of the present specification, the terms "connect", "mount", "fix", and the like are to be understood broadly, for example, "connect" may be a fixed connection, a detachable connection, or an integral connection; may be directly connected or indirectly connected through an intermediate. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In the description of the present application, the description of the terms "one embodiment," "some embodiments," etc. means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (8)

1. An integrated mass spectrometry quadrupole, comprising:
the four electrode rods are arranged in parallel and are rotationally and symmetrically distributed around the axis of the central line; and
a plurality of fixing portions for supporting the four electrode rods at predetermined positions in an extending direction of the electrode rods;
the electrode rod and the fixing part are integrally formed,
the electrode rod includes: a core material and a conductive layer coated on a surface;
the surface of the fixing part is coated with an insulating layer.
2. The integrated mass spectrometry quadrupole rod of claim 1, wherein the inner profile of the electrode rod is any one of a single curve, a circle, an ellipse, a semicircle or a semi-ellipse, and the end of the electrode rod is provided with a through hole for connecting with a conductive sheet as an electrical connection part.
3. The integrated mass spectrometry quadrupole rod of claim 1, wherein the core material is composed of a high molecular polymer comprising a photocurable resin, a polyimide, a nylon powder, a polycarbonate, and a ceramic compound comprising alumina and zirconia.
4. The integral mass spectrometer quadrupole rod of claim 1, wherein the conductive layer comprises:
the material of the conducting layer comprises single metal selected from gold, silver, copper and nickel and/or other metal and alloy materials with high conductivity and good stability;
the smoothness of the conductive layer is equal to or lower than Ra 0.3 and the thickness of the conductive layer does not exceed 10 micrometers.
5. The integral mass spectrometer quadrupole rod of claim 1, wherein an insulating layer is disposed on a surface of the stationary portion, and the insulating layer comprises a rubber-based insulating layer.
6. The integrated mass spectrometry quadrupole rod of claim 1, wherein the fixing portion is integrally connected to the 4 electrode rods on an inner circumferential side, and a relief notch is formed between two adjacent electrode rods and is recessed toward the outer circumferential side.
7. The integral mass spectrometry quadrupole of claim 1, wherein the coating comprises: vacuum coating, electroplating, electroless plating, vapor deposition, thermal spraying, and plasma polymerization coating techniques.
8. The integral mass spectrometry quadrupole of claim 1, wherein the core material and the anchor portion are integrally formed by 3D printing.
CN202210713544.7A 2022-06-22 2022-06-22 Integrated mass spectrum quadrupole rod Pending CN114899077A (en)

Priority Applications (1)

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CN202210713544.7A CN114899077A (en) 2022-06-22 2022-06-22 Integrated mass spectrum quadrupole rod

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Application Number Priority Date Filing Date Title
CN202210713544.7A CN114899077A (en) 2022-06-22 2022-06-22 Integrated mass spectrum quadrupole rod

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CN114899077A true CN114899077A (en) 2022-08-12

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024006608A1 (en) * 2022-07-01 2024-01-04 Massachusetts Institute Of Technology Quadrupole mass filters and related systems and methods
GB2623188A (en) * 2022-09-28 2024-04-10 Micromass Ltd A multipole rod support and a multipole rod assembly comprising the same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024006608A1 (en) * 2022-07-01 2024-01-04 Massachusetts Institute Of Technology Quadrupole mass filters and related systems and methods
GB2623188A (en) * 2022-09-28 2024-04-10 Micromass Ltd A multipole rod support and a multipole rod assembly comprising the same

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