WO1999021212A1 - Spectrometre de mobilite ionique a piegeage d'echantillons pour detecteur ambulatoire de molecules - Google Patents

Spectrometre de mobilite ionique a piegeage d'echantillons pour detecteur ambulatoire de molecules Download PDF

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Publication number
WO1999021212A1
WO1999021212A1 PCT/US1998/022092 US9822092W WO9921212A1 WO 1999021212 A1 WO1999021212 A1 WO 1999021212A1 US 9822092 W US9822092 W US 9822092W WO 9921212 A1 WO9921212 A1 WO 9921212A1
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WO
WIPO (PCT)
Prior art keywords
sample
reaction region
ims
ion mobility
vapor
Prior art date
Application number
PCT/US1998/022092
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English (en)
Inventor
Lawrence Haley
Govindanunny Thekkadath
Original Assignee
Ids Intelligent Detection Systems, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ids Intelligent Detection Systems, Inc. filed Critical Ids Intelligent Detection Systems, Inc.
Priority to CA002306761A priority Critical patent/CA2306761A1/fr
Priority to EP98953728A priority patent/EP1025577A1/fr
Priority to JP2000517437A priority patent/JP2001521268A/ja
Publication of WO1999021212A1 publication Critical patent/WO1999021212A1/fr

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622Ion mobility spectrometry

Definitions

  • the present invention relates generally to ion mobility spectrometers and, particularly, to a novel sample trapping ion mobility spectrometer device for portable molecular detection.
  • IMS ion mobility spectrometers
  • Sample transport into a conventional IMS device 10 is normally performed by converting the sample into a vapor and injecting the vapor sample in a carrier gas into the sample inlet 12.
  • a part of the sample is ionized in an ionizer device 16 and the rest of the sample is carried out of the IMS via a sample outlet port 14.
  • a description of existing ion mobility spectrometer devices of this design may be found in issued U.S. Patent No. 3,621,240 to Cohen, U.S. Patent No. 4,311,669 to Spangler, U.S. Patent No. 3,845,301 to Thekkadath, and U.S. Patent No. 5,083,019 to Spangler.
  • the sample is introduced via the sample inlet port 12 in a condensed form into the reaction region, such as reaction region 15 of the IMS device 10 of Figure 1, and then directly vaporized for subsequent ionization and detection.
  • care is taken to remove residual samples after ionization by providing a continuous flow of the carrier and drift gas 20 and by keeping the IMS at a high enough temperature with respect to the sample condensation temperature.
  • the sample is efficiently carried out of the IMS device 10 via the drift and sample output port 14, and the history of the sample injection is removed.
  • the IMS and the inlet and outlet ports have to be kept at temperatures as high as 200 to 250 degrees Celsius to avoid the condensation of the sample in the inlet port or in the IMS.
  • the condensation can lead to contamination of the system and loss in efficiency of detection.
  • the vapor pressures of the compounds in the IMS are high enough that ionization of the compound in the vapor form produces enough number of ions for detection as a signal above noise.
  • the temperature of the IMS and the inlet and outlet ports are kept high enough so as to remove the residual vapors from the IMS.
  • IMS device which deliberately operates at a temperature low enough such that the sample vapors introduced into the IMS actually condense in the IMS after their introduction.
  • a low temperature IMS device is hereinafter characterized as a low power consumption IMS device.
  • a "cold" IMS device which deliberately operates at a temperature low enough such that the sample vapors introduced into the IMS actually condense in the IMS in a fraction of a second after their introduction.
  • the deliberate trapping of the vapors in the IMS effectively removes the sample from the ionization process because after condensation, the vapor pressure of the compound at the operating temperature of the IMS is so low as to be negligible. Since the compound is no longer present in the vapor form, ion production no longer takes place at a sufficient rate as to be detectable.
  • the process of sample introduction in such a cold IMS is different from sample introduction in conventional IMS devices.
  • the sample is first transported in the vapor form to the entrance of the reaction region at a temperature several tens of degrees higher than the temperature of the reaction region and the temperature of the carrier gas flowing in the reaction region.
  • the sample vapor encounters the colder gas in the region and starts to cool down.
  • the reactant ions present in the reaction region rapidly convert a portion of the vapor sample into product ions which are subsequently swept away by an electric field into a drift region.
  • the rest of the sample condenses on the walls of the reaction region and is no longer available for ionization reactions in the vapor phase.
  • the IMS of the present invention operates at essentially ambient temperatures, thus, making it ideal for hand-held and portable types of drug and explosive detection systems powered, for example, by batteries.
  • FIG. 1 illustrates an Ion Mobility Spectrometer (IMS) device of conventional design.
  • Figure 2 is an illustrative cross -sectional view of the low power IMS device according to the invention.
  • Figure 3 is a schematic diagram of an example hand-held drug detection system implementing the low power, sample trapping IMS device of the invention.
  • Figures 4 (a) and 4 (b) depict a process flow diagram for the sample trapping IMS of the invention implemented in a battery powered portable molecular detection system.
  • FIG. 2 depicts the process of sample introduction and ionization in the cold IMS device 100 of the invention.
  • the reaction region 102 is essentially cylindrical having an ionizing source 111 at one end of the cylinder and an electrode assembly 112 at the other end of the cylinder for creating an electric field that will transport the ions to the drift region 103.
  • two gas inlet ports 106, 107 and a gas outlet port 105 are shown.
  • a first gas flow 121 input from gas inlet port 106 is the drift gas flow comprising a buffer gas such as air or nitrogen which starts at the detector end 104 of the IMS 100 and flows into the reaction region 102 and out through the gas outlet port 105.
  • a drift gas flow rate is of a value required to keep the drift region free of any unwanted vapors and to provide a constant background buffer gas for the ions to drift in.
  • this drift gas flow rate may be about lOcc/min.
  • a second gas flow 122 input from gas inlet port 107 provided near the top end of the reaction region 102 has a dual purpose: 1) for carrying the reactant gas which is required to provide an efficient reaction pathway for the sample species; and, 2) for functioning as an "air curtain" to prevent the condensing sample species from condensing on the ionization source end.
  • the exit of this gas flow is additionally via the outlet port 105.
  • a third flow 123 is the sample flow containing vapors of the sample substance.
  • the sample inlet 116 for receiving and directing the sample gas flow 123 is normally at the same temperature as the reaction region 102 and the gas flowing into the inlet has the same temperature as that of the other two gas flows 121,122.
  • FIG. 2 illustrates a pulsed direct current source 125 for heating the sample inlet 116.
  • the temperature to which the sample inlet port 116 is heated preferably is a function of time and the nature of the sample. For example, when analyzing the drugs cocaine and heroin, the temperature may be ramped from about 50° C to about 230° C in six seconds. The ramp is typically proportional to the square of the time elapsed but in general is a function programmed into the computer including a steady temperature (usually 180° C) .
  • the inlet tube is designed in such a way that there are no cold spots on it, especially at the location 118 where the inlet tube 116 joins the reaction region.
  • the vapors of the sample e.g., drugs
  • the inlet tube is then cooled rapidly, i.e., the heat source is removed within seconds, to prevent any further injection of the sample into the reaction region.
  • the sample vapor in the reaction region 102 is then subjected to reactions with the charged species present in the region 102.
  • the nature of the reactions and their ionization rates depend upon the ionizing species from the ionizing source 111, and the compound being ionized. In general, the reactions occur on a time scale in the order of microseconds, with the sample vapors still in their vapor state. Condensation of the vapors on the walls of the tube starts to take place only after several tens of milliseconds after their introduction into the reaction region 102 and may be varied by adjusting the flow rates of the various gas streams in the reaction region.
  • an electric field of the correct polarity and magnitude is established between the reaction 102 and drift regions 103 to pulse the ions into the drift region.
  • This pulse VI is typically applied to the electrode 111 with respect to the voltage V2 on electrode 112 and has a relative amplitude with respect to V2 of several hundred volts and a duration of 200 to 500 microseconds.
  • the constituents of the ion packet are separated by their mobility in the drift region as in any IMS device, typically using an electric field created by ring electrodes at different potentials indicated as V3 , V4,...,V7 in Figure 2.
  • the detection of the separated ion packets can also be done conventionally as in a typical IMS or can be injected into other apparatus using electric fields for further processing. It should be noted that ion injection into the drift region 103 may also be carried out using the Nielson-Bradbury shutter 125 as shown in the conventional IMS device ( Figure 1) .
  • the sample may be removed from the reaction region 102 by cooling the reaction region 102 and keeping its temperature lower than the temperature of the sample.
  • Means for cooling the reaction region 102 may include thermo-electric cooling or, using maintaining a drift gas 121 at a cooler temperature. This temperature reduction reduces the vapor pressure of the sample in the reaction region to a low enough value so as to be negligible for producing measurable quantities of ions, as required by the invention.
  • Another way of achieving this is to provide adsorbing media 130 for the sample vapor on the inside walls of the reaction region such as shown in Figure 2. Once the sample reaches the adsorber, it is trapped and the net effect is the same as a lowering of the sample temperature, and thus its vapor pressure.
  • the sample inlet drive 116 shown in Figure 2 is normally used in a pulsed mode in order to reduce the loading of the reaction region with too much sample.
  • the inlet tube 116 comprises a gas chromatographic column which normally sits at a low temperature so that the sample is trapped at the inlet end of the column. The column may then be heated at a certain rate using a pulsed direct electric current through the column if it is metallic or by an indirect means, e.g., infra-red or hot air envelope, if it is non-metallic. This causes the sample to travel down the column into the drift region of the IMS for analyzation as described above.
  • the IMS analyzes each constituent at a different time and thus the IMS mobility spectra will vary in time. Once the sample is analyzed, the column is rapidly cooled and prepared for trapping the next sample in the column.
  • reaction region 102 acts as a condensing location for the sample, it eventually becomes loaded with the condensed sample and becomes unusable.
  • the reaction region electrode 111 is made in such a way that it has an inner condensing liner 117 which, when loaded with sufficient sample residue, can easily be replaced with a new one. Under normal circumstances of sampling, replacement of the inner condensing liner 117 may occur only after several thousand hours of operation since each sample is only a few ten to a few hundred nanograms in weight.
  • FIG 3 is a schematic diagram of an example hand-held (portable) drug detection system implementing the low power, sample trapping IMS device of the invention.
  • power to the sample trapping IMS system 100 may be provided by a battery 150, for example, a 12V battery.
  • a column heating and sampling gas input system 180 is controlled by a microprocessor-based control system depicted in Figure 3 as computer system 175 comprising Digital I/O, analog I/O, a keyboard, CPU, and display.
  • the sample inlet itself 116 is depicted in Figure 3 as a GC column with a sample intake system 180 comprising a sealed rotatable preconcentrator device having sampling media 180 including, for example, target sample adsorbent material, and having a first sample input end 181 and a second heater end 182.
  • the preconcentrator device is a sealed container in which the sampling media rotating between a first sample input end 181 in communication with a computer controlled sampling pump system 170 for periodically retrieving samples to be analyzed, and the second end 182 in communication with the GC column inlet 116 where a gas flow containing desorbed sample is injected into the inlet port or GC column 116.
  • FIGs 4 (a) and 4 (b) depict a process flow diagram 200 for the sample trapping IMS of the invention implemented in a battery powered portable molecular detection system.
  • a first step 202 is to check the battery state, and, at step 204, to determine whether the battery voltage is normal. If the battery voltage is not normal, the operator is so warned at step 206 and the process terminates at step 208. If the battery voltage is sufficient, the portable detection device displays a device ready indication at step 210 and waits for the sampling signal 215 from the CPU system 175 ( Figure 3) at step 217.
  • the computer controlled sampling pump system 170 is calibrated and a gas flow for the IMS and column is started at step 220.
  • sampling cycle is then executed at step 225 as will be described in further detail with reference to Figure 4 (b) .
  • step 230 the results at the output of the IMS detector are analyzed and displayed, and the process returns to step 202 for the next sample cycle.
  • the first step is to seal the preconcentrator housing, and, at step 253, to start the sampling pump system 170 ( Figure 3) .
  • the preconcentrator is terminated, and at step 259, the housing seal is broken and the preconcentrator wheel device rotated to place the sample media containing the adsorbed sample to the GC column input end 182.
  • a heated gas flow is input to the preconcentrator at the IMS/GC column sample inlet end 182 to enable desorption and injection of the sample to the column.
  • the heating and desorption time is dependent upon a variety of factors including: the type of target sample compound, e.g., explosives, narcotics, etc., and the sample adsorbing material employed, etc.
  • the desorption and injection port heaters are turned off for a predetermined amount of time.
  • the column or IMS inlet port is heated, in the manner as described herein, for example, by pulse d.c. current applied directly to the column or inlet port.
  • the GC column may be subjected to computer- controlled pulsed d.c.
  • the temperature of the GC column is monitored using a thermocouple attached to it (not shown) and the heating of the column is regulated by the CPU 175 by varying the pulse width of the current flowing through the metal part of the column.
  • the sample trapping action of the trapping IMS system 100 of the invention gathers its data for a controlled time period that depends upon the retention time of the compound within the GC column, i.e., the time it takes the target compound to travel to the trapping IMS column as the GC column is heated.
  • the pulsed current for supplying heat to the GC column or inlet 116 ( Figure 3) , is terminated, and the process returns to step 230, Figure 4(a). Further details regarding the operation of the programmed sampling and the "heat -on-demand" sampling technique, may be found in commonly owned, co- pending U.S.
  • the advantage of the cold IMS and the heat- on- demand sampling technique is in the savings in power as opposed to conventionally heating the IMS and the sampling device continuously so as to keep the device at operating temperatures of typically 200° Celsius, e.g., for drugs.
  • Typical power savings are in the order of 10 to 20 watts, which is very important for a battery operated IMS devices.
  • Another advantage is the increased resolution of the IMS since the diffusion broadening of the IMS signal peaks is reduced at the lower temperatures (the peak width being proportional to the square root of the absolute temperature of the drift gas) .
  • the resolution of the IMS is increased by thirty percent (30%) .

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  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
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Abstract

L'invention concerne un spectromètre de mobilité ionique (IMS) (100) 'froid' qui fonctionne délibérément à une température suffisamment basse pour que des vapeurs échantillonnées se condensent, c'est-à-dire soient piégées, dans le dispositif IMS (100) après leur introduction avec une garniture de condensation (117) dans une région de réaction (102) du dispositif IMS (100). Le piégeage délibéré des vapeurs dans le dispositif IMS (100) enlève de manière active l'échantillon du procédé d'ionisation parce qu'après la condensation, la pression de la vapeur du composé à la température de fonctionnement du dispositif IMS (100) est négligeable. Etant donné que le composé n'est plus présent sous forme de vapeur, la production ionique n'est plus effectuée à une vitesse suffisante pour être détectée.
PCT/US1998/022092 1997-10-22 1998-10-20 Spectrometre de mobilite ionique a piegeage d'echantillons pour detecteur ambulatoire de molecules WO1999021212A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CA002306761A CA2306761A1 (fr) 1997-10-22 1998-10-20 Spectrometre de mobilite ionique a piegeage d'echantillons pour detecteur ambulatoire de molecules
EP98953728A EP1025577A1 (fr) 1997-10-22 1998-10-20 Spectrometre de mobilite ionique a piegeage d'echantillons pour detecteur ambulatoire de molecules
JP2000517437A JP2001521268A (ja) 1997-10-22 1998-10-20 携帯分子検出用試料捕捉イオン移動度分光計

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US6268297P 1997-10-22 1997-10-22
US60/062,682 1997-10-22

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Cited By (27)

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WO2002071053A2 (fr) 2001-03-05 2002-09-12 The Charles Stark Draper Laboratory, Inc. Procede et dispositif de chromatographie couplee a la spectrometrie de mobilite ionique a forme d'onde asymetrique a champ eleve (faims)
US6481263B1 (en) 1998-02-11 2002-11-19 Intelligent Detection Systems, Inc. Hand-held detection system using GC/IMS
US6690004B2 (en) 1999-07-21 2004-02-10 The Charles Stark Draper Laboratory, Inc. Method and apparatus for electrospray-augmented high field asymmetric ion mobility spectrometry
US6806463B2 (en) 1999-07-21 2004-10-19 The Charles Stark Draper Laboratory, Inc. Micromachined field asymmetric ion mobility filter and detection system
US6815669B1 (en) 1999-07-21 2004-11-09 The Charles Stark Draper Laboratory, Inc. Longitudinal field driven ion mobility filter and detection system
US7045776B2 (en) 2001-06-30 2006-05-16 Sionex Corporation System for collection of data and identification of unknown ion species in an electric field
US7274015B2 (en) 2001-08-08 2007-09-25 Sionex Corporation Capacitive discharge plasma ion source
WO2008074987A1 (fr) * 2006-12-20 2008-06-26 Smiths Detection-Watford Limited Appareil de détection et préconcentrateurs
US7619214B2 (en) 1999-07-21 2009-11-17 The Charles Stark Draper Laboratory, Inc. Spectrometer chip assembly
US7841906B2 (en) 2008-07-04 2010-11-30 Smiths Group Plc Electrical connectors
US8022360B2 (en) 2006-12-20 2011-09-20 Smiths Detection-Watford Limited Gas pre-concentrator for detection apparatus
US8217344B2 (en) 2007-02-01 2012-07-10 Dh Technologies Development Pte. Ltd. Differential mobility spectrometer pre-filter assembly for a mass spectrometer
US8222595B2 (en) 2006-10-19 2012-07-17 Smiths Detection-Watford Limited Spectrometer apparatus
US8668870B2 (en) 2006-12-20 2014-03-11 Smiths Detection-Watford Limited Ion mobility spectrometer which controls carrier gas flow to improve detection
US8734722B2 (en) 2006-12-20 2014-05-27 Smiths Detection-Watford Limited Detection apparatus accompanying preconcentrated pulsed analyte via an aperture
WO2015097462A1 (fr) * 2013-12-24 2015-07-02 Micromass Uk Limited Ims à onde progressive à contre-courant de gaz
CN110412114A (zh) * 2013-08-08 2019-11-05 史密斯探测-沃特福特有限公司 用于浮质检测的方法和便携式离子迁移谱仪
GB2574327A (en) * 2018-05-31 2019-12-04 Micromass Ltd Bench-top time of flight mass spectrometer
US11355331B2 (en) 2018-05-31 2022-06-07 Micromass Uk Limited Mass spectrometer
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US11879470B2 (en) 2018-05-31 2024-01-23 Micromass Uk Limited Bench-top time of flight mass spectrometer
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Cited By (42)

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Publication number Priority date Publication date Assignee Title
US6481263B1 (en) 1998-02-11 2002-11-19 Intelligent Detection Systems, Inc. Hand-held detection system using GC/IMS
US6815668B2 (en) 1999-07-21 2004-11-09 The Charles Stark Draper Laboratory, Inc. Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry
US7075068B2 (en) 1999-07-21 2006-07-11 The Charles Stark Draper Laboratory, Inc. Method and apparatus for electrospray augmented high field asymmetric ion mobility spectrometry
US6690004B2 (en) 1999-07-21 2004-02-10 The Charles Stark Draper Laboratory, Inc. Method and apparatus for electrospray-augmented high field asymmetric ion mobility spectrometry
US6806463B2 (en) 1999-07-21 2004-10-19 The Charles Stark Draper Laboratory, Inc. Micromachined field asymmetric ion mobility filter and detection system
US6815669B1 (en) 1999-07-21 2004-11-09 The Charles Stark Draper Laboratory, Inc. Longitudinal field driven ion mobility filter and detection system
US7619214B2 (en) 1999-07-21 2009-11-17 The Charles Stark Draper Laboratory, Inc. Spectrometer chip assembly
US7547879B2 (en) 1999-07-21 2009-06-16 The Charles Stark Draper Laboratory, Inc. Longitudinal field driven ion mobility filter and detection system
US7462825B2 (en) 1999-07-21 2008-12-09 The Charles Stark Draper Laboratory, Inc. Method and apparatus for electrospray-augmented high field asymmetric ion mobility spectrometry
US7211791B2 (en) 1999-07-21 2007-05-01 The Charles Stark Draper Laboratory, Inc. Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry
US7365316B2 (en) 1999-07-21 2008-04-29 The Charles Stark Draper Laboratory Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry
WO2002071053A2 (fr) 2001-03-05 2002-09-12 The Charles Stark Draper Laboratory, Inc. Procede et dispositif de chromatographie couplee a la spectrometrie de mobilite ionique a forme d'onde asymetrique a champ eleve (faims)
WO2002071053A3 (fr) * 2001-03-05 2003-01-03 Draper Lab Charles S Procede et dispositif de chromatographie couplee a la spectrometrie de mobilite ionique a forme d'onde asymetrique a champ eleve (faims)
US7045776B2 (en) 2001-06-30 2006-05-16 Sionex Corporation System for collection of data and identification of unknown ion species in an electric field
US7274015B2 (en) 2001-08-08 2007-09-25 Sionex Corporation Capacitive discharge plasma ion source
US8222595B2 (en) 2006-10-19 2012-07-17 Smiths Detection-Watford Limited Spectrometer apparatus
US8405023B2 (en) 2006-10-19 2013-03-26 Smiths Detection-Watford Limited Spectrometer apparatus
US8648296B2 (en) 2006-10-19 2014-02-11 Smiths Detection-Watford Limited Spectrometer apparatus
US8022360B2 (en) 2006-12-20 2011-09-20 Smiths Detection-Watford Limited Gas pre-concentrator for detection apparatus
US8158933B2 (en) 2006-12-20 2012-04-17 Smiths Detection-Watford Limited Detector apparatus and pre-concentrator
WO2008074987A1 (fr) * 2006-12-20 2008-06-26 Smiths Detection-Watford Limited Appareil de détection et préconcentrateurs
US8668870B2 (en) 2006-12-20 2014-03-11 Smiths Detection-Watford Limited Ion mobility spectrometer which controls carrier gas flow to improve detection
US8734722B2 (en) 2006-12-20 2014-05-27 Smiths Detection-Watford Limited Detection apparatus accompanying preconcentrated pulsed analyte via an aperture
US9513256B2 (en) 2006-12-20 2016-12-06 Smiths Detection-Watford Limited Ion mobility spectrometer which controls carrier gas flow to improve detection
US9664657B2 (en) 2006-12-20 2017-05-30 Smiths Detection—Watford Limited Pulsed admission of analyte to detection apparatus
US8217344B2 (en) 2007-02-01 2012-07-10 Dh Technologies Development Pte. Ltd. Differential mobility spectrometer pre-filter assembly for a mass spectrometer
US7841906B2 (en) 2008-07-04 2010-11-30 Smiths Group Plc Electrical connectors
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US9939408B2 (en) 2013-12-24 2018-04-10 Micromass Uk Limited Travelling wave IMS with counterflow of gas
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EP1025577A1 (fr) 2000-08-09
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