CN106340435A - Pulse field enrichment ion migration tube - Google Patents

Pulse field enrichment ion migration tube Download PDF

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Publication number
CN106340435A
CN106340435A CN201510397889.6A CN201510397889A CN106340435A CN 106340435 A CN106340435 A CN 106340435A CN 201510397889 A CN201510397889 A CN 201510397889A CN 106340435 A CN106340435 A CN 106340435A
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China
Prior art keywords
ion
voltage
gate
pulsed
electrode assembly
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CN201510397889.6A
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Chinese (zh)
Inventor
陈创
李海洋
王卫国
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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Priority to CN201510397889.6A priority Critical patent/CN106340435A/en
Publication of CN106340435A publication Critical patent/CN106340435A/en
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Abstract

The invention relates to a pulse field enrichment ion migration tube. The pulse field enrichment ion migration tube is characterized in that high-voltage pulse, which is synchronized to ion gate open pulse, is applied to a pulse electrode set between an ion source and an ion gate, the movement speed of ions is greatly improved during a period of opening the ion gate, and more ions are enabled to pass the ion gate; and meanwhile, spatial focusing is carried out on an ion cluster passed the ion gate by using the difference, which is caused by the high-voltage pulse, in electric field intensity at two sides of the ion gate, and the original resolution of the iron migration tube is maintained.

Description

A kind of pulsed field is enriched with transference tube
Technical field
The present invention relates to a kind of pulsed field is enriched with transference tube.It is characterized in that, by from Apply on the pulsed electrode of setting between component and ion gate and the synchronization of ion gate unbalanced pulse High-voltage pulse, the period opened in ion gate, greatly improves the movement velocity of ion, makes more Many ions can pass through ion gate;Meanwhile, using the ion gate both sides caused by high-voltage pulse The difference of electric field intensity, to carrying out space-focusing by the ion cluster of ion gate, keeps ion The original resolution of migration tube.
Background technology
Ion gate is an important composition part of migration time ion mobility spectrometry instrument, its to from It is finally detected that the utilization ratio of sub- migration tube reaction zone intermediate ion determines ion mobility spectrometry The intensity of ion signal.Low ion utilization ratio often results in poor signal to noise ratio.
Bradbury-nielsen ion gate (bng) is widely used one in ion mobility spectrometry Plant ion gate.At present, the method having occurred in that multiple making bng, including etching, machine Silk etc. worn by tool braiding, micromachined and pcb plate.Generally, bng is by with interdigital altogether Face is placed and two groups of tinsels of mutually insulated are constituted.By applying not on this two groups of tinsels Same voltage, can produce the electricity perpendicular with direction of an electric field in migration area between adjacent wire , this electric field can the ion in blocking reaction area enter in migration area.
In order to ensure that transference tube has preferable resolution capability, in a controlling cycle, Bng type ion gate mostly just open very short a period of time allow reaction zone ion pass through simultaneously Enter in migration area, for example, every 20ms inward swinging door 200 μ s.This means in reaction zone Ion only 1% can enter in migration area and be separated and detected, remaining 99% ion It is consumed in eventually and on ion gate electrode assemblie.In addition, emptying effect is bng Caused by structurally and operationally principle inherent feature of type ion gate.Close the door in ion gate When, the electric field between adjacent wire can be to ion gate plane with external diffusion.This diffusion is made Become the deformity of electric field in the reaction zone adjacent with ion gate and migration area, increase the reality of ion gate Border cuts width, causes the actual opening time of ion gate to be less than its nominal opening time.This will enter One step is lowered into the ratio of reaction zone intermediate ion.
In addition, high intense pulsed electric field has the efficient performance trapping ion.By its control with ion gate System combines, and is favorably improved ion gate to transference tube reaction zone intermediate ion using effect Rate.
Content of the invention:
It is an object of the invention to improving the profit to transference tube reaction zone intermediate ion for the ion gate With efficiency, thus improving the signal noise ratio that detection pole detects signal, and the detection obtaining Sensitivity.
To achieve these goals, the technical solution used in the present invention is: in ion source and ion Between door, setting is applied with the pulsed electrode of pulse voltage, improves pulse during ion gate opens the door The electric field intensity in region between electrode and ion gate, make to be present in the ion in this region quickly through Ion gate enters in migration area.
Particularly as follows:
A kind of pulsed field is enriched with transference tube, and described transference tube is a hollow cavity, Cavity two ends are respectively provided with reactive ion generator ion source and ion reception device farad Disk;It is located between ion source and Faraday plate in inside cavity and ion gate is set, by cavity Part becomes two regions, constitutes reaction zone, ion gate and method wherein between ion source and ion gate Draw composition migration area between disk;It is characterized in that: reaction zone inside setting can by from The pulsed electrode of son, pulsed electrode is parallel with ion gate, constitutes between pulsed electrode and ion gate Pulsed field ion enrichment area.
Ion source, pulsed electrode, ion gate and farad chassis are arranged at ion with coaxial manner and move Move in pipe;
Ion gate is parallel to each other in plane first by being in same plane or be in two Gate electrode assembly and the second gate electrode assembly composition, the first gate electrode assembly and the second gate electrode group Part mutually insulated is oppositely arranged, and the axial distance between first electrode assembly and ion source is less than etc. Axial distance between second electrode assembly and ion source;
In the first prefixed time interval, ion gate the first gate electrode assembly applies the first electricity Pressure, ion gate second electrode assembly applies second voltage, and pulsed electrode applies tertiary voltage, 4th voltage is applied on ion source;Wherein, second voltage makes ion gate close higher than first voltage, 4th voltage is higher than tertiary voltage, and tertiary voltage is higher than second voltage, the ion warp in ion source Pulsed electrode enters the pulsed field ion enrichment area between pulsed electrode and ion gate;
In the second prefixed time interval, ion gate the first gate electrode assembly applies the 5th electricity Pressure, ion gate the second gate electrode assembly applies the 6th voltage, and pulsed electrode applies the 7th electricity Pressure, ion source applies the 8th voltage;Wherein, the 6th voltage makes ion gate equal to the 5th voltage Open, the 7th voltage be higher than the 6th voltage and the 8th voltage, in pulsed field ion enrichment area from Son by compressed enriched and enters in migration area, and in ion source, the new ion being formed is prevented from entering Pulsed field ion enrichment area.
First voltage is equal to the 5th voltage, and the 4th voltage is equal to the 8th voltage;
The value of the first prefixed time interval is more than zero, and the value of the second prefixed time interval is between zero-sum Between the 50% of the value of the first prefixed time interval;
Voltage gradient in pulsed field ion enrichment area is 1 times of voltage gradient in migration area and arrives 100 times.
Pulsed electrode be one of mesh electrode, ring electrode, electrodes or two kinds with On.
First gate electrode assembly and the second gate electrode assembly are in same plane, the first gate electrode Assembly and the second gate electrode assembly are electrodes, concentric ring shaped electrodes, zigzag shape electrode One of;
Or, the first gate electrode assembly and the second gate electrode assembly be respectively at two be parallel to each other flat On face, the first gate electrode assembly and second together or differs, and is mesh electrode, concentric annular One of electrode, electrodes, zigzag shape electrode or two or more.
Drift gas entrance is provided with migration area, reaction zone is provided with sample inlet and tail gas goes out Mouthful;
Sample to be detected is carried by sample gas and enters reaction zone and reactive ion through sample inlet Reaction generates product ion, and drift gas enters into migration area through drift gas entrance and migration area is blown Sweep, final sum sample gas flow out transference tube through offgas outlet together.
The invention has the advantage that
Its sensitivity can be carried while not reducing ion mobility spectrometry resolution capability by the present invention High more than 20 times;This invention need not make any hardware to existing migration time transference tube On improvement, simple it is adaptable to the ion source of different structure and operating principle.
The present invention is further detailed explanation below in conjunction with the accompanying drawings:
Brief description:
Fig. 1, a kind of pulsed field enrichment transference tube.Wherein: 1 ion source;2—— Bradbury-nielsen ion gate;3 Faraday plates;4 reaction zones;5 migrations Area;6 offgas outlet;7 sample inlets;8 drift gas entrances;9 pulse electricity Pole;10 pulsed field ion enrichment areas.
Fig. 2,5ppbv acetone is enriched with transference tube and conventional ion migration in pulsed field The ion peak-to-peak signal being formed in pipe.Wherein the very first time is spaced apart 40ms, the second Preset Time It is spaced 150 μ s.
Specific embodiment:
Embodiment 1
As shown in figure 1, a kind of pulsed field enrichment transference tube is a hollow circuit cylinder cavity, Cavity two ends be respectively provided with the reactive ion generator ion source 1 of column and column from Sub- reception device Faraday plate 3;It is located between ion source and Faraday plate in inside cavity and arrange Bradbury-nielsen ion gate 2, inside cavity is divided into two regions, wherein ion source Constitute reaction zone 4 and ion gate between, between ion gate and Faraday plate, constitute migration area 5; It is characterized in that: in the inside of reaction zone, annular pulse electrode 9, pulsed electrode and ion are set Door is parallel, constitutes pulsed field ion enrichment area 10 between pulsed electrode and ion gate.
Ion source, pulsed electrode, ion gate and farad chassis are arranged at ion with coaxial manner and move Move in pipe;
Ion gate is by lattice-shaped the first gate electrode assembly being in same plane and lattice-shaped Two gate electrode assemblies are constituted, two gate electrode assembly mutually insulateds composition staggered relatively Bradbury-nielsen type ion gate;
In the first prefixed time interval, ion gate the first gate electrode assembly applies the first electricity Pressure, ion gate second electrode assembly applies second voltage, and pulsed electrode applies tertiary voltage, 4th voltage is applied on ion source;Wherein, second voltage makes ion gate close higher than first voltage, 4th voltage is higher than tertiary voltage, and tertiary voltage is higher than second voltage, the ion warp in ion source Pulsed electrode enters the pulsed field ion enrichment area between pulsed electrode and ion gate;
In the second prefixed time interval, ion gate the first gate electrode assembly applies the 5th electricity Pressure, ion gate second electrode assembly applies the 6th voltage, and pulsed electrode applies the 7th voltage, 8th voltage is applied on ion source;Wherein, the 6th voltage makes ion gate open equal to the 5th voltage, 7th voltage is higher than the 6th voltage and the 8th voltage, and the ion in pulsed field ion enrichment area is pressed Contracting is enriched with and enters in migration area, and in ion source, the new ion being formed is prevented from entering pulsed field Ion enrichment area.
First voltage is equal to the 5th voltage, and the 4th voltage is equal to the 8th voltage;
The value of the first prefixed time interval is 0~100ms, and the value of the second prefixed time interval is 10~500 μ s;
Voltage gradient in pulsed field ion enrichment area is 1 times of voltage gradient in migration area and arrives 15 times.
Drift gas entrance 8 is provided with migration area, reaction zone is provided with sample inlet 7 and tail gas Outlet 6;
Sample to be detected is carried by sample gas and enters reaction zone and reactive ion through sample inlet Reaction generates product ion, and drift gas enters into migration area through drift gas entrance and migration area is blown Sweep, final sum sample gas flow out transference tube through offgas outlet together.
Application examples
Pulsed field is enriched with transference tube.The length of migration area is 7.2cm, migration area electric-field strength Spend for 338v/cm, temperature is 100 DEG C, sample gas and drift gas are purify air, sample Gas velocity 10ml/min, floats gas velocity 200ml/min, and ion source is 10mci (millicurie In)63Ni source, ion gate is spacing 1mm, string diameter 0.1mm Bradbury-nielsen type ion gate, pulsed electrode is the ring electrode of internal diameter 14mm, arteries and veins The length rushing field ion enrichment region is 8mm, and the first prefixed time interval is 40ms, the Two prefixed time interval are 150 μ s;Voltage on first prefixed time interval internal ion-source is 3780v, the voltage on pulsed electrode is 2970v, and the voltage of ion gate first electrode assembly is 2700v, the voltage of second electrode assembly is 2780v;Second prefixed time interval internal ion-source On voltage be 3780v, the voltage on pulsed electrode be 5970v, ion gate first electrode The voltage of assembly is 2700v, and the voltage of second electrode assembly is 2700v, 5ppbv acetone The ion signal peak being formed is as shown on Fig. 2.
Traditional ion transference tube.The length of migration area is 7.2cm, and migration area electric field intensity is 338 V/cm, temperature is 100 DEG C, and sample gas and drift gas are purify air, sample gas flow velocity 10 Ml/min, floats gas velocity 200ml/min, and ion source is 10mci's (millicurie)63ni Source, ion gate is spacing 1mm, the bradbury-nielsen type ion of string diameter 0.1mm Door, pulsed electrode is the ring electrode of internal diameter 14mm, the axial direction of pulsed electrode and ion gate Distance is 8mm, and the first prefixed time interval is 20ms, in the second prefixed time interval is 150μs;Voltage on first prefixed time interval internal ion-source is 3780v, on pulsed electrode Voltage be 2970v, the voltage of ion gate first electrode assembly is 2700v, second electrode The voltage of assembly is 2780v;Voltage on second prefixed time interval internal ion-source is 3780 V, the voltage on pulsed electrode is 2970v, and the voltage of ion gate first electrode assembly is 2700 V, the voltage of second electrode assembly is 2700v, and the ion signal peak that 5ppbv acetone is formed is such as Shown under Fig. 2.

Claims (6)

1. a kind of pulsed field is enriched with transference tube, and described transference tube is a hollow cavity, It is respectively provided with reactive ion generator ion source and ion reception device method at cavity two ends Draw disk;It is located between ion source and Faraday plate in inside cavity and ion gate is set, by cavity Inside is divided into two regions, wherein between ion source and ion gate constitute reaction zone, ion gate and Migration area is constituted between Faraday plate;It is characterized in that: the inside setting in reaction zone can be passed through The pulsed electrode of ion, pulsed electrode is parallel with ion gate, structure between pulsed electrode and ion gate Become pulsed field ion enrichment area.
2. pulsed field according to claim 1 enrichment transference tube it is characterised in that:
Ion source, pulsed electrode, ion gate and farad chassis are arranged at ion with coaxial manner and move Move in pipe;
Ion gate is parallel to each other in plane first by being in same plane or be in two Gate electrode assembly and the second gate electrode assembly composition, the first gate electrode assembly and the second gate electrode group Part mutually insulated is oppositely arranged, and the axial distance between first electrode assembly and ion source is less than etc. Axial distance between second electrode assembly and ion source;
In the first prefixed time interval, ion gate the first gate electrode assembly applies the first electricity Pressure, ion gate second electrode assembly applies second voltage, and pulsed electrode applies tertiary voltage, 4th voltage is applied on ion source;Wherein, second voltage makes ion gate close higher than first voltage, 4th voltage is higher than tertiary voltage, and tertiary voltage is higher than second voltage, the ion warp in ion source Pulsed electrode enters the pulsed field ion enrichment area between pulsed electrode and ion gate;
In the second prefixed time interval, ion gate the first gate electrode assembly applies the 5th electricity Pressure, ion gate the second gate electrode assembly applies the 6th voltage, and pulsed electrode applies the 7th electricity Pressure, ion source applies the 8th voltage;Wherein, the 6th voltage makes ion gate equal to the 5th voltage Open, the 7th voltage be higher than the 6th voltage and the 8th voltage, in pulsed field ion enrichment area from Son by compressed enriched and enters in migration area, and in ion source, the new ion being formed is prevented from entering Pulsed field ion enrichment area.
3. pulsed field according to claim 2 enrichment transference tube it is characterised in that:
First voltage is equal to the 5th voltage, and the 4th voltage is equal to the 8th voltage;
The value of the first prefixed time interval is more than zero, and the value of the second prefixed time interval is between zero-sum Between the 50% of the value of the first prefixed time interval;
Voltage gradient in pulsed field ion enrichment area is 1 times of voltage gradient in migration area and arrives 100 times.
4. pulsed field according to claim 1 enrichment transference tube it is characterised in that: Pulsed electrode is one of mesh electrode, ring electrode, electrodes or two or more.
5. pulsed field according to claim 2 enrichment transference tube it is characterised in that:
First gate electrode assembly and the second gate electrode assembly are in same plane, the first gate electrode Assembly and the second gate electrode assembly are electrodes, concentric ring shaped electrodes, zigzag shape electrode One of;
Or, the first gate electrode assembly and the second gate electrode assembly be respectively at two be parallel to each other flat On face, the first gate electrode assembly and the second gate electrode assembly are mesh electrode, concentric ring shaped electrodes, One of electrodes, zigzag shape electrode or two or more.
6. pulsed field according to claim 2 enrichment transference tube it is characterised in that:
Drift gas entrance is provided with migration area, reaction zone is provided with sample inlet and tail gas goes out Mouthful;
Sample to be detected is carried by sample gas and enters reaction zone and reactive ion through sample inlet Reaction generates product ion, and drift gas enters into migration area through drift gas entrance and migration area is blown Sweep, final sum sample gas flow out transference tube through offgas outlet together.
CN201510397889.6A 2015-07-08 2015-07-08 Pulse field enrichment ion migration tube Pending CN106340435A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109659219A (en) * 2017-10-12 2019-04-19 中国科学院大连化学物理研究所 A kind of the ion door gear and control method of no ion discrimination
CN109839426A (en) * 2017-11-28 2019-06-04 中国科学院大连化学物理研究所 Method that is a kind of while improving transference tube interior air-flow and temperature uniformity
CN109887826A (en) * 2017-12-06 2019-06-14 中国科学院大连化学物理研究所 A kind of conical transference tube of space-focusing
CN111755315A (en) * 2020-07-07 2020-10-09 湘潭大学 Device and method for improving sensitivity and resolution of ion mobility spectrometry

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1544931A (en) * 2003-11-20 2004-11-10 中国科学院安徽光学精密机械研究所 Storing type photo-ionisation ion migration mass spectrum
US20090166530A1 (en) * 2007-12-27 2009-07-02 Yuanjing Li Ion mobility spectrometer and method thereof
CN102931046A (en) * 2011-08-09 2013-02-13 中国科学院大连化学物理研究所 Spatial focusing ion gate component and spatial focusing ion migration tube

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1544931A (en) * 2003-11-20 2004-11-10 中国科学院安徽光学精密机械研究所 Storing type photo-ionisation ion migration mass spectrum
US20090166530A1 (en) * 2007-12-27 2009-07-02 Yuanjing Li Ion mobility spectrometer and method thereof
CN102931046A (en) * 2011-08-09 2013-02-13 中国科学院大连化学物理研究所 Spatial focusing ion gate component and spatial focusing ion migration tube

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109659219A (en) * 2017-10-12 2019-04-19 中国科学院大连化学物理研究所 A kind of the ion door gear and control method of no ion discrimination
CN109839426A (en) * 2017-11-28 2019-06-04 中国科学院大连化学物理研究所 Method that is a kind of while improving transference tube interior air-flow and temperature uniformity
CN109887826A (en) * 2017-12-06 2019-06-14 中国科学院大连化学物理研究所 A kind of conical transference tube of space-focusing
CN109887826B (en) * 2017-12-06 2020-09-15 中国科学院大连化学物理研究所 Conical ion migration tube with space focusing function
CN111755315A (en) * 2020-07-07 2020-10-09 湘潭大学 Device and method for improving sensitivity and resolution of ion mobility spectrometry

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Application publication date: 20170118