WO2021027033A1 - Procédé de commande de grille ionique pour spectromètre à mobilité ionique - Google Patents

Procédé de commande de grille ionique pour spectromètre à mobilité ionique Download PDF

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Publication number
WO2021027033A1
WO2021027033A1 PCT/CN2019/108753 CN2019108753W WO2021027033A1 WO 2021027033 A1 WO2021027033 A1 WO 2021027033A1 CN 2019108753 W CN2019108753 W CN 2019108753W WO 2021027033 A1 WO2021027033 A1 WO 2021027033A1
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Prior art keywords
grid electrode
push
open
ion
shear
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PCT/CN2019/108753
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English (en)
Chinese (zh)
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倪凯
陈海
余泉
钱翔
王晓浩
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清华大学深圳国际研究生院
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Publication of WO2021027033A1 publication Critical patent/WO2021027033A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/0027—Methods for using particle spectrometers
    • H01J49/0031—Step by step routines describing the use of the apparatus
    • 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
    • H01J49/061—Ion deflecting means, e.g. ion gates

Definitions

  • the invention relates to the field of ion mobility spectroscopy, in particular to an ion gate control method for ion mobility spectrometers.
  • IMS Ion mobility spectroscopy
  • the switching of the state of the ion gate is usually realized by changing the voltage of the first grid electrode G1 and the second grid electrode G2: when the voltage difference between the first grid electrode G1 and the second grid electrode G2 is small, the ion When the gate is opened, ions can pass through; when the voltage difference between the first grid electrode G1 and the second grid electrode G2 is large, the ion gate is closed, and the ions near the ion gate will be hit on the ion gate with lower voltage, and the ions cannot Pass to achieve closure.
  • a large number of ions will accumulate near the low-voltage ion gate, and a blank area will be formed near the high-voltage ion gate due to lack of ions, resulting in uneven rear edges of the ion clusters.
  • the traditional ion gate timing control method is to apply a pulse signal of fixed width and amplitude on the ion gate grid.
  • the main problem of this control method is that the cutting shape of the ion cluster trailing edge is not ideal.
  • the main purpose of the present invention is to overcome the shortcomings of the prior art and propose an improved ion gate control method for ion mobility spectrometers to improve the flatness of the trailing edge of ion clusters, thereby improving the resolution of ion mobility spectra .
  • the ion gate includes a first grid electrode and a second grid electrode insulated from each other in an ion migration tube, the first grid electrode and the second grid electrode
  • the plane on which the two grid electrodes are located is perpendicular to the ion migration direction, wherein the first grid electrode and the second grid electrode are coplanar or the first grid electrode is opposite to the second grid electrode
  • the control method includes controlling a complete working cycle of the ion gate to go through the following stages:
  • Door opening stage keep the voltage of the first grid electrode at V 1 open , and keep the voltage of the second grid electrode at V 2 open , where the selection of V 1 open and V 2 open satisfies: The voltage difference allows ions in the ionization zone to pass through the ion gate and enter the migration zone;
  • Shearing stage the voltage of the first grid electrode is maintained at V 1 shear , and the voltage of the second grid electrode is maintained at V 2 shear , where the selection of V 1 shear and V 2 shear satisfies:
  • Repulsion stage maintain the voltage of the first grid electrode at V 1 push , and keep the voltage of the second grid electrode at V 2 push , where the selection of V 1 push and V 2 push satisfies: V 1 Push- V 2 push and V 1 cut- V 2 cut have the opposite sign, or V 1 push + V 2 push > V 1 open + V 2 open ;
  • the voltage of the first grid electrode is maintained at V 1 off
  • the voltage of the second grid electrode is maintained at V 2 off , where the selection of V 1 off and V 2 off meets:
  • the voltage difference prevents ions in the ionization zone from passing through the ion gate and entering the migration zone.
  • V 1 cut V 1 open ;
  • V 1 push V 1 open ;
  • V 1 off V 1 on ;
  • V 1 push V 1 close ;
  • V 2 push V 2 close .
  • the ion gate includes a first grid electrode and a second grid electrode insulated from each other in an ion migration tube, the first grid electrode and the second grid electrode
  • the plane on which the two grid electrodes are located is perpendicular to the ion migration direction, wherein the first grid electrode and the second grid electrode are coplanar or the first grid electrode is opposite to the second grid electrode
  • the control method includes controlling a complete working cycle of the ion gate to go through the following stages:
  • Door opening stage keep the voltage of the first grid electrode at V 1 open , and keep the voltage of the second grid electrode at V 2 open , where the selection of V 1 open and V 2 open satisfies: The voltage difference allows ions in the ionization zone to pass through the ion gate and enter the migration zone;
  • Shearing stage the voltage of the first grid electrode is maintained at V 1 shear , and the voltage of the second grid electrode is maintained at V 2 shear , where the selection of V 1 shear and V 2 shear satisfies:
  • Repulsion stage maintain the voltage of the first grid electrode at V 1 push , and keep the voltage of the second grid electrode at V 2 push , where the selection of V 1 push and V 2 push satisfies: V 1 Push- V 2 push has the opposite sign of V 1 cut- V 2 cut , or V 1 push + V 2 push ⁇ V 1 open + V 2 open ;
  • the voltage of the first grid electrode is maintained at V 1 off
  • the voltage of the second grid electrode is maintained at V 2 off , where the selection of V 1 off and V 2 off meets:
  • the voltage difference prevents ions in the ionization zone from passing through the ion gate and entering the migration zone.
  • the shear stage -1000 ⁇ V 1 -V 2 Shear Shear ⁇ -50, preferably -600 ⁇ V 1 -V 2 Shear Shear ⁇ -200.
  • V 1 cut V 1 open ;
  • V 1 push V 1 open ;
  • V 1 off V 1 on ;
  • V 1 push V 1 close ;
  • V 2 push V 2 close .
  • the present invention provides an improved ion gate control method.
  • a shearing phase and a repulsive phase are added between the opening and closing phases of the ion gate,
  • the electric field is used to influence the spatial distribution and temporal motion characteristics of ions.
  • the shearing stage realizes the rapid cutting of the trailing edge of the ion group
  • the repulsion stage realizes the overall shift of the ion group in the migration direction.
  • the ion gate control method of the present invention can make the shape of the trailing edge of the ion cluster more smooth, thereby improving the resolution of the ion mobility spectrum.
  • Figure 1a is a front view of a first grid electrode and a second grid electrode of an ion gate structure in an ion mobility spectrometer;
  • Figure 1b is a side view of a first grid electrode and a second grid electrode of an ion gate structure in an ion mobility spectrometer
  • Figure 1c is a side view of the first grid electrode and the second grid electrode of another ion gate structure in the ion mobility spectrometer;
  • FIG. 2 is a voltage timing diagram of a specific embodiment of the ion gate control method according to the present invention.
  • Fig. 3 is a voltage timing diagram of another specific embodiment of the ion gate control method according to the present invention.
  • the ion gate control method of the present invention is used to control the ion gate of an ion mobility spectrometer.
  • the ion mobility spectrometer includes an ion mobility tube (not shown), and ionization is sequentially formed inside the ion mobility tube along the ion migration direction. Zone, ion gate zone, migration zone.
  • the ion gate is located in the ion gate area, and includes a first grid electrode G1 and a second grid electrode G2 insulated from each other in the ion transfer tube, as shown in FIG. 1a.
  • the plane on which the first grid electrode G1 and the second grid electrode G2 are located is perpendicular to the ion migration direction.
  • first grid electrode G1 and the second grid electrode G2 are coplanar, as shown in FIG. 1b.
  • first grid electrode G1 is close to the ionization source (not shown) in the ion mobility spectrometer
  • the second grid electrode G2 is close to the detector (not shown) in the ion mobility spectrometer, as shown in FIG. 1c.
  • the first grid electrode G1 and the second grid electrode G2 are electrodes that can penetrate ions; the distance d between the first grid electrode G1 and the second grid electrode G2 usually satisfies 0 ⁇ d ⁇ 2mm, where d is 0 It shows that the first grid electrode G1 and the second grid electrode G2 are coplanar and are formed into a BN (Bradbury-Nielson) ion gate structure.
  • the ion transfer tube works in a positive polarity mode or a negative polarity mode.
  • the ion gate control method includes controlling a complete working cycle of the ion gate to go through four stages: a door opening phase, a shearing phase, a repulsion phase, and a door closing phase.
  • a shearing phase and a repulsive phase are added between the opening phase and the closing phase of the ion gate, that is, the sequence of a complete working cycle of the ion gate is: opening phase, shearing phase, pushing Repel stage, closing stage.
  • the shearing stage realizes the rapid cutting of the trailing edge of the ion group, while reducing the forward migration speed of the ion group, and even temporarily stops the forward migration of the ion group, reducing the axial stretching of the ion group during the shearing process;
  • the repulsion stage realizes the overall movement of the ion cluster along the migration direction, and uses the non-uniformity of the repelling electric field to realize the axial compression of the ion cluster.
  • the voltage applied to the ion gate grid during the repulsion phase and the closing phase can be the same, and its voltage must meet the constraints of the repulsion phase and the closing phase at the same time, which can combine the repulsion phase and the closing phase into one.
  • the method can realize separate and independent control of ion cluster cutting and separation processes, and on the other hand, it can reduce trailing edge tailing caused by ion gate cutting ion clusters, which is beneficial to improve the resolution ability of the ion mobility spectrometer.
  • an ion gate control method for an ion mobility spectrometer wherein the ion mobility tube operates in a positive polarity mode, that is, the direction of the electric field lines in the migration region is directed from the ionization source to the detector.
  • the ion gate control method includes controlling a complete working cycle of the ion gate to go through the following four stages:
  • V 1 shear + V 2 shear ⁇ V 1 open + V 2 open so that the average potential of the ion gate region in the shear phase is lower than the average potential of the ion gate region in the opening phase, and the ion clusters on the side of the migration region are subjected to the reverse of the migration electric field It slows down due to the applied force, stops the movement or even moves in the opposite direction, reducing the stretching of the ion clusters in the migration direction during the shearing stage. Therefore, the shearing stage realizes the rapid cutting of the trailing edge of the ion group, and some ions at the end of the ion group are annihilated on the ion gate with a lower voltage. At the same time, the forward migration speed of the ion group is reduced, and the forward migration of the ion group is even temporarily stopped. Even make it move in the opposite direction to reduce the axial stretching of ion clusters in the shearing process.
  • the selection of push and V 2 push satisfies: ⁇ V push has the opposite sign of ⁇ V shear , or V 1 push + V 2 push > V 1 open + V 2 open ; in the shearing stage, when the voltage of the first grid electrode G1 is less than the first
  • the potential of the second grid electrode G2 the positive ions will be gathered and annihilated at the first grid electrode G1, and the sign of ⁇ V push and ⁇ V shear is opposite, which means that the potential of the first grid electrode G1 is greater than the second grid electrode G1 at this time
  • the potential of the electrode G2 so the ions originally gathered near the first grid electrode G1 will be pushed to the second grid electrode G2 to achieve the purpose of repelling ion clusters
  • V 1 push + V 2 push > V 1 open + V 2 open it means that the average potential of the ion gate area in the repulsion phase is higher than the average potential of the ion gate area in the opening phase, and the ion clusters are subjected to the electric field line during the repulsion phase.
  • the positive thrust in the direction achieves the purpose of repelling ion clusters. Therefore, in the repulsion stage, a positive thrust is applied to the ion cluster in the direction of ion migration, and the ion cluster as a whole leaves the ion gate area and enters the migration zone; the repulsion stage realizes the overall movement of the ion cluster in the migration direction.
  • the inhomogeneity of the repulsive electric field is used to achieve axial compression of ion clusters.
  • V 1 and V 2 meet the following requirements: It can prevent ions in the ionization zone from passing through the ion gate and entering the migration zone. If it has been kept in the closing phase, after a long enough time (more than 1 second), the door into the ionization region through the ion drift region of ions striking the detector current generated in the absolute value
  • a voltage gradient different from the ion migration direction is formed to prevent ions in the ion gate region from entering the migration region.
  • E d is the electric field strength of the migration zone.
  • 50 ⁇ V shear ⁇ 1000 Preferably, 50 ⁇ V shear ⁇ 1000, more preferably, 200 ⁇ V shear ⁇ 600.
  • -1000 ⁇ V push ⁇ -50 Preferably, -600 ⁇ V push ⁇ -200.
  • -1000 ⁇ V off ⁇ -50 Preferably, -400 ⁇ V off ⁇ -80.
  • V 1 cut V 1 open .
  • V 1 push V 1 open .
  • V 1 off V 1 on .
  • the selection of V 1 push and V 1 off should meet the voltage selection conditions of the repulsion phase and the closing phase. This can combine the repulsion phase and the closing phase of the first grid electrode into one, further simplifying the control sequence.
  • the selection of V 2 push and V 2 close should meet the voltage selection conditions of the repulsion phase and the closing phase. This can combine the repulsion phase and the closing phase of the second grid electrode into one, further simplifying the control sequence.
  • an ion gate control method for an ion mobility spectrometer wherein the ion mobility tube operates in a negative polarity mode, that is, the direction of the electric field lines in the migration region is directed from the detector to the ionization source.
  • the difference between negative polarity mode and positive polarity mode is that positive ions move in positive polarity mode, and negative ions move in negative polarity mode.
  • the ion gate control method includes controlling a complete working cycle of the ion gate to go through the following four stages:
  • ⁇ V push has the opposite sign of ⁇ V shear , or V 1 push + V 2 push ⁇ V 1 open + V 2 open ; in the shearing stage, when the potential of the first grid electrode G1 is greater than the second The potential of the grid electrode G2, the negative ions will be gathered and annihilated at the first grid electrode G1, and the sign of ⁇ V push and ⁇ V shear is opposite, which means that the electric potential of the first grid electrode G1 is smaller than the second grid electrode G2 at this time, so The ions originally gathered near the first grid electrode G1 will be pushed to the second grid electrode G2 to achieve the purpose of repelling ion clusters.
  • V 1 push + V 2 push ⁇ V 1 open + V 2 open which means that the average potential of the ion gate area in the repulsion phase is less than the average potential of the ion gate area in the opening phase, and the ion clusters are subjected to the migration direction during the repulsion phase.
  • Forward thrust to achieve the purpose of repelling ion clusters Therefore, in the repulsion stage, a positive thrust is applied to the ion cluster in the direction of ion migration, and the ion cluster as a whole leaves the ion gate area and enters the migration zone; the repulsion stage realizes the overall movement of the ion cluster in the migration direction.
  • the inhomogeneity of the repulsive electric field is used to achieve axial compression of ion clusters.
  • V 1 and V 2 meet the following requirements: It can prevent ions in the ionization zone from passing through the ion gate and entering the migration zone. If it has been kept in the closing phase, after a long enough time (more than 1 second), the door into the ionization region through the ion drift region of ions striking the detector current generated in the absolute value
  • ) ⁇ V ⁇ ⁇ 0 where d is the distance between the first grid electrode G1 and the second grid electrode G2, and E d is the intensity of the migration electric field;
  • -1000 ⁇ V shear ⁇ -50 Preferably, -600 ⁇ V shear ⁇ -200.
  • 50 ⁇ V push ⁇ 1000 Preferably, 50 ⁇ V push ⁇ 1000, more preferably, 200 ⁇ V push ⁇ 600.
  • 50 ⁇ V off ⁇ 1000 Preferably, 50 ⁇ V off ⁇ 1000, more preferably, 80 ⁇ V off ⁇ 400.
  • V 1 cut V 1 open .
  • V 1 push V 1 open .
  • V 1 off V 1 on .
  • the selection of V 1 push and V 1 off should meet the voltage selection conditions of the repulsion phase and the closing phase. This can combine the repulsion phase and the closing phase of the first grid electrode into one, further simplifying the control sequence.
  • the selection of V 2 push and V 2 close should meet the voltage selection conditions of the repulsion phase and the closing phase. This can combine the repulsion phase and the closing phase of the second grid electrode into one, further simplifying the control sequence.
  • the shape of the first grid electrode G1 and the second grid electrode G2 may be one or more of a mesh electrode, a concentric ring electrode, a grid electrode, and a spiral wire electrode. The combination.
  • the parameters and conditions of the ion mobility spectrometer are respectively composed of a set of metal wire meshes parallel to each other and at equal distances.
  • the distance between adjacent metal wires is 2mm; the first grid electrode G1 and the second grid electrode G2 have the same wire diameter It is 0.1mm; the first grid electrode G1 and the second grid electrode G2 are coplanar and the distance between adjacent metal wires is 1mm.
  • the ion mobility spectrometer is working in positive polarity mode.
  • the method of the present invention is used to shape the trailing edge of ion clusters.
  • the timing diagram of the first grid electrode G1 and the second grid electrode G2 is shown in Fig. 2, and the specific parameters are as follows:
  • the voltage at each stage of the first grid electrode G1 and the second grid electrode G2 meets the following conditions, and the units are all volts (V):
  • V 2 cut V 2 open -400
  • V 2 push V 2 open +300;
  • V 2 off V 2 on +100
  • the duration of the repulsion phase ⁇ push 30 ⁇ s.
  • the parameters and conditions of the ion mobility spectrometer are respectively composed of a set of metal wire meshes parallel to each other and at equal distances.
  • the distance between adjacent metal wires is 2mm; the first grid electrode G1 and the second grid electrode G2 have the same wire diameter It is 0.1mm; the first grid electrode G1 and the second grid electrode G2 are coplanar and the distance between adjacent metal wires is 1mm.
  • the ion mobility spectrometer is working in positive polarity mode.
  • the method of the present invention is used to shape the trailing edge of ion clusters.
  • the timing diagram of the first grid electrode G1 and the second grid electrode G2 is shown in FIG. 3, and the specific parameters are as follows:
  • the voltage at each stage of the first grid electrode G1 and the second grid electrode G2 meets the following conditions, and the units are all volts (V):
  • V 2 cut V 2 open -400

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

Abstract

Procédé de commande de grille ionique pour un spectromètre à mobilité ionique. Le procédé comprend la commande, au moyen des tensions d'une première électrode de grille (G1) et d'une seconde électrode de grille (G2), d'un cycle de travail complet d'une grille ionique pour subir une étape d'ouverture de grille, une étape de cisaillement, une étape de répulsion et une étape de fermeture de grille, une coupure rapide d'un bord arrière d'un groupe ionique étant obtenue au niveau de l'étape de cisaillement, ce qui permet de réduire la tension axiale du groupe ionique pendant un processus de cisaillement ; et à l'étape de répulsion, la propulsion globale du groupe ionique dans une direction de migration est obtenue, et la compression axiale du groupe ionique est obtenue en utilisant la non-uniformité d'un champ électrique de répulsion. Le procédé présente les effets bénéfiques de pouvoir réaliser une commande indépendante séparée sur des processus de coupe et de séparation d'un groupe ionique et peut également réduire la fuite de bord arrière provoquée par une grille ionique coupant le groupe ionique, ce qui facilite une amélioration de la capacité de résolution d'un spectromètre à mobilité ionique.
PCT/CN2019/108753 2019-08-09 2019-09-27 Procédé de commande de grille ionique pour spectromètre à mobilité ionique WO2021027033A1 (fr)

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CN201910735917 2019-08-09
CN201910745716.7 2019-08-13
CN201910745716.7A CN110571126B (zh) 2019-08-09 2019-08-13 一种用于离子迁移谱仪的离子门控制方法

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CN112490108B (zh) * 2020-11-24 2021-07-27 中国科学院大连化学物理研究所 一种自动富集离子的离子门控制方法
CN113539781B (zh) * 2021-07-01 2023-07-25 中国科学院大连化学物理研究所 一种施加在bn型离子门上的脉冲电压波形

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CN108072690A (zh) * 2016-11-17 2018-05-25 中国科学院大连化学物理研究所 一种离子迁移谱和离子阱质谱联用装置及分析方法
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