WO2006129101A1 - Ion mobility spectrometer systems - Google Patents

Ion mobility spectrometer systems Download PDF

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Publication number
WO2006129101A1
WO2006129101A1 PCT/GB2006/002017 GB2006002017W WO2006129101A1 WO 2006129101 A1 WO2006129101 A1 WO 2006129101A1 GB 2006002017 W GB2006002017 W GB 2006002017W WO 2006129101 A1 WO2006129101 A1 WO 2006129101A1
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WO
WIPO (PCT)
Prior art keywords
cell
dopants
gas
vapour
region
Prior art date
Application number
PCT/GB2006/002017
Other languages
French (fr)
Inventor
Michael Edward Huxham
Stephen Paul Watts
Original Assignee
Smiths Detection-Watford Limited
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 Smiths Detection-Watford Limited filed Critical Smiths Detection-Watford Limited
Publication of WO2006129101A1 publication Critical patent/WO2006129101A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating 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
    • G01N27/622—Ion mobility spectrometry
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/34—Dynamic spectrometers
    • H01J49/40—Time-of-flight spectrometers

Definitions

  • This invention relates to ion mobility spectrometer systems of the kind having an IMS cell with an inlet by which a vapour or gas to be analysed is supplied to a first region towards one end of the cell.
  • IMS systems are often used to detect substances such as explosives, drugs, blister and nerve agents or the like.
  • An IMS system typically includes a detector cell to which a sample of air containing a suspected substance is supplied as a gas or vapour. The cell operates at or near atmospheric pressure and contains electrodes energized to produce a voltage gradient along the cell. Molecules in the sample of air are ionized, such as by means of a radioactive source or by corona discharge, and are admitted into the drift region of the cell by an electrostatic gate at one end. The ionized molecules drift to the opposite end of the cell at a speed dependent on the mobility of the ion. By measuring the time of flight along the cell it is possible to identify the ion. It is common practice to add a reagent or dopant to the cell. The reagent is selected so that it combines with the substance of interest to produce a larger molecule that moves more slowly and can be more readily distinguished from other substances.
  • IMS systems are described in GB 2324407, GB 2324875, GB2316490, GB2323165 and US 4551624.
  • IMS systems are known where selectivity and interferent rejection is improved by using two separate IMS cells each doped with a different, single reagent.
  • US 6459079 describes a system with a positive and a negative cell, which are each supplied with a different reagent.
  • US 6495824 describes a system where one of several different reagents can be supplied to the cell in response to detection of a suspect substance.
  • US6825460 describes an IMS system having a molecular sieve for drying and cleaning recirculated gases, which is impregnated with a dopant.
  • WO2004/ 102611 describes an IMS system where several different reagents can be supplied selectively to drift gas flowing against the ion flow through a single IMS cell.
  • an object of the present invention to provide an alternative IMS system.
  • an ion mobility spectrometer system of the above-specified kind characterised in that the system includes an arrangement for supplying at least two dopants to the first region such that the vapour or gas supplied to the cell is exposed to both dopants.
  • the system preferably includes two dopant reservoirs containing different dopants and connected to the IMS cell such that the vapour or gas to be analysed is exposed to the dopants before it is ionized.
  • the cell may include a selective barrier between the ionization region and the inlet, and the two dopants may be supplied to the cell between the selective barrier and the inlet.
  • the system preferably includes a molecular sieve and a pump connected in a drift gas flow path extending between opposite ends of a drift region of the cell so as to flow air along the drift region against the flow of ions, the dopants being supplied to the cell independently of the drift gas flow path.
  • One of the dopants may be acetone and one of the dopants may be ammonia.
  • a method of analysing a gas or vapour including the steps of ionizing the gas or vapour, gating resultant ion species, applying an electric field to cause the gated species to drift along a region, timing the passage of the ion species along the drift region and providing an output indicative of the nature of the gas or vapour according to the time of passage along the drift region, characterised in that the gas or vapour is exposed to a plurality of dopant chemicals prior to being gated and being subject to the electric field.
  • FIG 1 shows the system schematically
  • Figure 2 is a simplified spectrum showing a typical system response.
  • the system includes an IMS drift cell 1 having an inlet manifold 2 with an inlet port 3 and a dopant port 4. Sample air to be analysed is supplied to the inlet port 3.
  • the dopant port 4 is connected to two dopant reservoirs 5A and 5B containing two different dopants, such as acetone and ammonia, which are effective to add low concentrations of both dopants together to the sample inlet region of the cell 1.
  • the interior of the manifold 2 opens into the left-hand end of the interior of the cell via a selective barrier 6 such as a semi-permeable membrane, or of any other form that allows passage of the molecules of interest whilst excluding the majority of other molecules.
  • the barrier 6 could be non-selective, such as a pinhole, as described in WO93/01485.
  • the sample to be analysed may be supplied to the cell 1 by some other interface, such as of the kind described in EP596978.
  • the barrier 6 communicates with an ionisation region 7 including an ionisation source such as a radiation source or a corona discharge.
  • an ionisation source such as a radiation source or a corona discharge.
  • a Bradbury Nielson gating grid 8 which controls passage of ionised molecules into a drift region 9 formed by a series of drift electrodes 10a.
  • a collector plate 11 at the right-hand end of the cell collects ions passed through the drift region 9 and provides an output to a processor
  • the processor 20 which also controls the gate 8 and various other functions of the system.
  • the processor 20 times the passage of the ion species along the drift region and provides an output to a display
  • the cell 1 has an inlet 30, by which recirculated, cleaned, dried drift air is supplied to the interior of the cell, where it travels from right to left and flows out via an exhaust outlet 31 close to the gating grid 8 in the ionisation region 7.
  • Air is supplied to the inlet 30 by means of a pump 32 having an inlet 33 connected to the exhaust outlet 31, and having an outlet 34 connected to the cell inlet 30 via an molecular sieve 40.
  • the sieve 40 cleans and dries the air exhausted from the drift chamber 9. It can be seen that the dopants in the reservoirs 5 A and 5B are supplied to the cell independently of the drift gas flow path provided by the pump 32 and sieve 40. By doping in this region, ionization takes place on chemicals that have been exposed to the dopants.
  • the sample gas entering the cell 1 at the inlet 2 is exposed to the presence of both dopants during its passage along the cell.
  • the presence of two dopants in the inlet region has been found to yield multiple product ion peaks, for both the monomer and dimer of a common simulant (DPM).
  • the product ion peaks can be attributed to acetone-clustered and ammonia-clustered ions.
  • adding two dopants can yield material-specific fingerprint spectra.
  • the processor 20 is appropriately programmed to identify specific spectra and provide an alarm or other output accordingly to the display 21. In this way, selectivity can be improved in an IMS system having only one cell. The ability of a system of the present invention to identify chemical agents is, therefore, enhanced.
  • Figure 2 shows a spectrum produced by a system doped with acetone and ammonia in response to DPM. Peaks A, B and C are reactant ion peaks. Peak D is a peak produced by DPM monomer (ammonia). Peak E is a peak produced by DPM monomer (acetone). Peak F is a peak produced by DPM dimer (ammonia). Peak G is a peak produced by DPM dimer (acetone).
  • the dopants could be supplied to any region of the IMS cell towards the sample inlet, such as to the ionisation region.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Electrochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

An ion mobility spectrometer has a drift chamber (9) with a collector electrode (11) at one end and a pump (32) circulating a drift gas against the ion flow direction. Ions are admitted to the drift chamber (9) from an ionization region (7) by a gate (8). Gas or vapour to be analyzed is exposed to two different dopant chemicals in reservoirs (5A and 5B) connected to the spectrometer in the region of the ionization chamber (7), such as on the inlet side of a membrane (6), so that ionization takes place on the analyte gas or vapour after exposure to the dopants.

Description

ION MOBILITY SPECTROMETER SYSTEMS
This invention relates to ion mobility spectrometer systems of the kind having an IMS cell with an inlet by which a vapour or gas to be analysed is supplied to a first region towards one end of the cell.
IMS systems are often used to detect substances such as explosives, drugs, blister and nerve agents or the like. An IMS system typically includes a detector cell to which a sample of air containing a suspected substance is supplied as a gas or vapour. The cell operates at or near atmospheric pressure and contains electrodes energized to produce a voltage gradient along the cell. Molecules in the sample of air are ionized, such as by means of a radioactive source or by corona discharge, and are admitted into the drift region of the cell by an electrostatic gate at one end. The ionized molecules drift to the opposite end of the cell at a speed dependent on the mobility of the ion. By measuring the time of flight along the cell it is possible to identify the ion. It is common practice to add a reagent or dopant to the cell. The reagent is selected so that it combines with the substance of interest to produce a larger molecule that moves more slowly and can be more readily distinguished from other substances.
Examples of IMS systems are described in GB 2324407, GB 2324875, GB2316490, GB2323165 and US 4551624. IMS systems are known where selectivity and interferent rejection is improved by using two separate IMS cells each doped with a different, single reagent. US 6459079 describes a system with a positive and a negative cell, which are each supplied with a different reagent. US 6495824 describes a system where one of several different reagents can be supplied to the cell in response to detection of a suspect substance. US6825460 describes an IMS system having a molecular sieve for drying and cleaning recirculated gases, which is impregnated with a dopant. WO2004/ 102611 describes an IMS system where several different reagents can be supplied selectively to drift gas flowing against the ion flow through a single IMS cell.
It is an object of the present invention to provide an alternative IMS system. According to one aspect of the present invention there is provided an ion mobility spectrometer system of the above-specified kind, characterised in that the system includes an arrangement for supplying at least two dopants to the first region such that the vapour or gas supplied to the cell is exposed to both dopants. '
The system preferably includes two dopant reservoirs containing different dopants and connected to the IMS cell such that the vapour or gas to be analysed is exposed to the dopants before it is ionized. The cell may include a selective barrier between the ionization region and the inlet, and the two dopants may be supplied to the cell between the selective barrier and the inlet. The system preferably includes a molecular sieve and a pump connected in a drift gas flow path extending between opposite ends of a drift region of the cell so as to flow air along the drift region against the flow of ions, the dopants being supplied to the cell independently of the drift gas flow path. One of the dopants may be acetone and one of the dopants may be ammonia.
According to another aspect of the present invention there is provided a method of analysing a gas or vapour including the steps of ionizing the gas or vapour, gating resultant ion species, applying an electric field to cause the gated species to drift along a region, timing the passage of the ion species along the drift region and providing an output indicative of the nature of the gas or vapour according to the time of passage along the drift region, characterised in that the gas or vapour is exposed to a plurality of dopant chemicals prior to being gated and being subject to the electric field.
An IMS system according to the present invention, will now be described, by way of example, with reference to the accompanying drawing, in which:
Figure 1 shows the system schematically; and
Figure 2 is a simplified spectrum showing a typical system response.
The system includes an IMS drift cell 1 having an inlet manifold 2 with an inlet port 3 and a dopant port 4. Sample air to be analysed is supplied to the inlet port 3. The dopant port 4 is connected to two dopant reservoirs 5A and 5B containing two different dopants, such as acetone and ammonia, which are effective to add low concentrations of both dopants together to the sample inlet region of the cell 1. The interior of the manifold 2 opens into the left-hand end of the interior of the cell via a selective barrier 6 such as a semi-permeable membrane, or of any other form that allows passage of the molecules of interest whilst excluding the majority of other molecules. Alternatively, the barrier 6 could be non-selective, such as a pinhole, as described in WO93/01485. Instead of a barrier, the sample to be analysed may be supplied to the cell 1 by some other interface, such as of the kind described in EP596978.
The barrier 6 communicates with an ionisation region 7 including an ionisation source such as a radiation source or a corona discharge. To the right of the ionisation region 7 a Bradbury Nielson gating grid 8, which controls passage of ionised molecules into a drift region 9 formed by a series of drift electrodes 10a. A collector plate 11 at the right-hand end of the cell collects ions passed through the drift region 9 and provides an output to a processor
20, which also controls the gate 8 and various other functions of the system. The processor 20 times the passage of the ion species along the drift region and provides an output to a display
21, or other utilisation means, indicative of the nature of the sample.
At its right-hand end, the cell 1 has an inlet 30, by which recirculated, cleaned, dried drift air is supplied to the interior of the cell, where it travels from right to left and flows out via an exhaust outlet 31 close to the gating grid 8 in the ionisation region 7. Air is supplied to the inlet 30 by means of a pump 32 having an inlet 33 connected to the exhaust outlet 31, and having an outlet 34 connected to the cell inlet 30 via an molecular sieve 40. The sieve 40 cleans and dries the air exhausted from the drift chamber 9. It can be seen that the dopants in the reservoirs 5 A and 5B are supplied to the cell independently of the drift gas flow path provided by the pump 32 and sieve 40. By doping in this region, ionization takes place on chemicals that have been exposed to the dopants.
In operation, the sample gas entering the cell 1 at the inlet 2 is exposed to the presence of both dopants during its passage along the cell. The presence of two dopants in the inlet region has been found to yield multiple product ion peaks, for both the monomer and dimer of a common simulant (DPM). The product ion peaks can be attributed to acetone-clustered and ammonia-clustered ions. Thus, adding two dopants can yield material-specific fingerprint spectra. The processor 20 is appropriately programmed to identify specific spectra and provide an alarm or other output accordingly to the display 21. In this way, selectivity can be improved in an IMS system having only one cell. The ability of a system of the present invention to identify chemical agents is, therefore, enhanced.
Figure 2 shows a spectrum produced by a system doped with acetone and ammonia in response to DPM. Peaks A, B and C are reactant ion peaks. Peak D is a peak produced by DPM monomer (ammonia). Peak E is a peak produced by DPM monomer (acetone). Peak F is a peak produced by DPM dimer (ammonia). Peak G is a peak produced by DPM dimer (acetone).
The dopants could be supplied to any region of the IMS cell towards the sample inlet, such as to the ionisation region.

Claims

1. An ion mobility spectrometer system having an IMS cell (1) with an inlet (3) by which a vapour or gas to be analysed is supplied to a first region (2) towards one end of the cell, characterised in that the system includes an arrangement (5 A and 5B) for supplying at least two dopants to the first region (2) such that the vapour or gas supplied to the cell is exposed to both dopants.
2. A system according to Claim 1, characterised in that the system includes two dopant reservoirs (5 A and 5B) containing different dopants and connected to the IMS cell (1) such that the vapour or gas to be analysed is exposed to the dopants before it is ionized.
3. A system according to Claim 1 or 2, characterised in that the cell (1) includes a selective barrier (6) between an ionization region (7) and the inlet (3), and that the two dopants are supplied to the cell (1) between the selective barrier (6) and the inlet (3).
4. A system according to any one of the preceding claims, characterised in that the system includes a molecular sieve (40) and a pump (32) connected in a drift gas flow path extending between opposite ends of a drift region (9) of the cell (1) so as to flow air along the drift region (9) against the flow of ions, and that the dopants are supplied to the cell (1) independently of the drift gas flow path.
5. A system according to any one of the preceding claims, characterised in that the one of the dopants is acetone.
6. A system according to any one of the preceding claims, characterised in that one of the dopants is ammonia.
7. A method of analysing a gas or vapour including the steps of ionizing the gas or vapour, gating resultant ion species, applying an electric field to cause the gated species to drift along a region, timing the passage of the ion species along the drift region and providing an output indicative of the nature of the gas or vapour according to the time of passage along the drift region, characterised in that the gas or vapour is exposed to a plurality of dopant chemicals prior to being gated and being subject to the electric field.
PCT/GB2006/002017 2005-06-02 2006-06-01 Ion mobility spectrometer systems WO2006129101A1 (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2451160A (en) * 2007-07-19 2009-01-21 Draeger Safety Ag & Co Kgaa Determining an analyte or mixture of analyte substances in the presence of a mixture of dopants using an ion mobility spectrometer.
WO2010006536A1 (en) * 2008-07-16 2010-01-21 同方威视技术股份有限公司 Ion mobility spectrometer
WO2010051241A1 (en) * 2008-10-27 2010-05-06 Smiths Detection - Toronto Ltd. Ammonium salts as ims positive mode calibrants/reactants
EP2075578A3 (en) * 2007-12-31 2010-10-20 GE Homeland Protection, Inc. Apparatus and method for generating ammonia gas for use in an ion mobility spectrometer
WO2010135899A1 (en) * 2009-05-25 2010-12-02 同方威视技术股份有限公司 Trace detection device and analysis method therefor
WO2011035633A1 (en) 2009-09-25 2011-03-31 同方威视技术股份有限公司 Ion mobility spectrometer detection method and apparatus using dopant
WO2011060607A1 (en) 2009-11-20 2011-05-26 同方威视技术股份有限公司 Ion mobility spectrometer and method for improving the detection sensitivity thereof
EP2517795A1 (en) * 2009-12-24 2012-10-31 Nuctech Company Limited Filter, filtering method using the filter and trace apparatus
US20130140455A1 (en) * 2011-05-27 2013-06-06 Dsa Detection Llc Multi-dopant permeation tube
GB2497862A (en) * 2011-12-20 2013-06-26 Draegerwerk Ag & Co Kgaa Enhancement of analyte detection by formation of dimer analytes in IMS
CN103871823A (en) * 2012-12-12 2014-06-18 中国科学院大连化学物理研究所 Membrane-inlet ion mobility spectrometer doped with organic solvent

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US4551624A (en) * 1983-09-23 1985-11-05 Allied Corporation Ion mobility spectrometer system with improved specificity
US5283199A (en) * 1990-06-01 1994-02-01 Environmental Technologies Group, Inc. Chlorine dioxide monitor based on ion mobility spectrometry with selective dopant chemistry
US20020088936A1 (en) * 1999-06-23 2002-07-11 Breach James Andrew Ion mobility spectrometers
US6459079B1 (en) * 2000-07-11 2002-10-01 The United States As Represented By The Secretary Of The Navy Shipboard chemical agent monitor-portable (SCAMP)
WO2004102611A2 (en) * 2003-05-13 2004-11-25 Smiths Group Plc Ims systems
WO2005001464A1 (en) * 2003-06-25 2005-01-06 Smiths Group Plc Ion mobility system comprising two ims cells operated at different polarities

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4551624A (en) * 1983-09-23 1985-11-05 Allied Corporation Ion mobility spectrometer system with improved specificity
US5283199A (en) * 1990-06-01 1994-02-01 Environmental Technologies Group, Inc. Chlorine dioxide monitor based on ion mobility spectrometry with selective dopant chemistry
US20020088936A1 (en) * 1999-06-23 2002-07-11 Breach James Andrew Ion mobility spectrometers
US6459079B1 (en) * 2000-07-11 2002-10-01 The United States As Represented By The Secretary Of The Navy Shipboard chemical agent monitor-portable (SCAMP)
WO2004102611A2 (en) * 2003-05-13 2004-11-25 Smiths Group Plc Ims systems
WO2005001464A1 (en) * 2003-06-25 2005-01-06 Smiths Group Plc Ion mobility system comprising two ims cells operated at different polarities

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2451160B (en) * 2007-07-19 2009-07-15 Draeger Safety Ag & Co Kgaa Determining an analyte substance with ion mobility spectrometry using a mixture of dopants
GB2451160A (en) * 2007-07-19 2009-01-21 Draeger Safety Ag & Co Kgaa Determining an analyte or mixture of analyte substances in the presence of a mixture of dopants using an ion mobility spectrometer.
EP2075578A3 (en) * 2007-12-31 2010-10-20 GE Homeland Protection, Inc. Apparatus and method for generating ammonia gas for use in an ion mobility spectrometer
WO2010006536A1 (en) * 2008-07-16 2010-01-21 同方威视技术股份有限公司 Ion mobility spectrometer
US8405024B2 (en) 2008-07-16 2013-03-26 Nuctech Company Limited Ion mobility spectrometer
WO2010051241A1 (en) * 2008-10-27 2010-05-06 Smiths Detection - Toronto Ltd. Ammonium salts as ims positive mode calibrants/reactants
US8461517B2 (en) 2008-10-27 2013-06-11 Smiths Detection Montreal Inc. Ammonium salts as IMS positive mode calibrants/reactants
US8309918B2 (en) 2009-05-25 2012-11-13 Nuctech Company Limited Trace detector and analytical method for trace detector
WO2010135899A1 (en) * 2009-05-25 2010-12-02 同方威视技术股份有限公司 Trace detection device and analysis method therefor
WO2011035633A1 (en) 2009-09-25 2011-03-31 同方威视技术股份有限公司 Ion mobility spectrometer detection method and apparatus using dopant
DE112010000007B4 (en) * 2009-09-25 2012-12-13 Nuctech Co. Ltd. Ion mobility spectrometer detection method and ion mobility spectrometer detection system using dopants
DE112010000007T5 (en) 2009-09-25 2011-06-22 Nuctech Co. Ltd. Ion mobility spectrometer detection method using dopants
US8237110B2 (en) 2009-09-25 2012-08-07 Nuctech Company Limited Ion mobility spectrometer detection method using dopants
US8716656B2 (en) 2009-11-20 2014-05-06 Nuctech Company Limited Ion mobility spectrometer and method for improving the detection sensitivity thereof
WO2011060607A1 (en) 2009-11-20 2011-05-26 同方威视技术股份有限公司 Ion mobility spectrometer and method for improving the detection sensitivity thereof
DE112010004489T5 (en) 2009-11-20 2012-10-04 Nuctech Company Limited Ion mobility spectrometer and method for improving its detection sensitivity
EP2517795A1 (en) * 2009-12-24 2012-10-31 Nuctech Company Limited Filter, filtering method using the filter and trace apparatus
EP2517795A4 (en) * 2009-12-24 2013-07-03 Nuctech Co Ltd Filter, filtering method using the filter and trace apparatus
US8679409B2 (en) 2009-12-24 2014-03-25 Nuctech Company Limited Filter device, filter method and trace detector
US20130140455A1 (en) * 2011-05-27 2013-06-06 Dsa Detection Llc Multi-dopant permeation tube
US9275842B2 (en) * 2011-05-27 2016-03-01 Dsa Detection Llc Multi-dopant permeation tube
US9589778B2 (en) 2011-05-27 2017-03-07 Dsa Detection Llc Multi-dopant permeation tube with two chambers for introducing dopants into a spectrometry system
GB2497862A (en) * 2011-12-20 2013-06-26 Draegerwerk Ag & Co Kgaa Enhancement of analyte detection by formation of dimer analytes in IMS
US8604422B2 (en) 2011-12-20 2013-12-10 Dragerwork AG & Co. KGaA Identification of analytes by an ion mobility spectrometer with formation of dimer analytes
GB2497862B (en) * 2011-12-20 2014-03-05 Draegerwerk Ag & Co Kgaa Identification of analytes by an ion mobility spectrometer with formation of dimer analytes
CN103871823A (en) * 2012-12-12 2014-06-18 中国科学院大连化学物理研究所 Membrane-inlet ion mobility spectrometer doped with organic solvent

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