CA2440429A1 - Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry - Google Patents

Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry Download PDF

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Publication number
CA2440429A1
CA2440429A1 CA002440429A CA2440429A CA2440429A1 CA 2440429 A1 CA2440429 A1 CA 2440429A1 CA 002440429 A CA002440429 A CA 002440429A CA 2440429 A CA2440429 A CA 2440429A CA 2440429 A1 CA2440429 A1 CA 2440429A1
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ion
section
filter
flow path
electrodes
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CA002440429A
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French (fr)
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CA2440429C (en
Inventor
Raanan A. Miller
Erkinjon G. Nazarov
Gary A. Eiceman
Evgeny Krylov
Boris Tadjikov
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Charles Stark Draper Laboratory Inc
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    • 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
    • G01N27/624—Differential mobility spectrometry [DMS]; Field asymmetric-waveform ion mobility spectrometry [FAIMS]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D59/00—Separation of different isotopes of the same chemical element
    • B01D59/44—Separation by mass spectrography
    • 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
    • G01N27/623—Ion mobility spectrometry combined with mass spectrometry
    • 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
    • G01N27/64—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 using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/0013—Miniaturised spectrometers, e.g. having smaller than usual scale, integrated conventional components
    • H01J49/0018—Microminiaturised spectrometers, e.g. chip-integrated devices, MicroElectro-Mechanical Systems [MEMS]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/0022—Portable spectrometers, e.g. devices comprising independent power supply, constructional details relating to portability
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N2030/0095—Separation specially adapted for use outside laboratory, e.g. field sampling, portable equipments
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • G01N30/7206—Mass spectrometers interfaced to gas chromatograph

Abstract

Method and apparatus for chromatographic high field asymmetric waveform ion mobility spectrometry, including a gas chromatographic analyzer section intimately coupled with an ionization section, an ion filter section, and an ion detection section, in which the sample compounds are at least somewhat separated prior to ionization, and ion filtering proceeds in a planar chambe r under influence of high field asymmetric periodic signals, with detection integrated into the flow path, for producing accurate, real-time, orthogonal data for identification of a broad range of chemical compounds.

Claims (75)

1. A system for generating data for characterizing a chemical species in a gas sample, comprising an inlet section, an ionization section, an ion filtering section, an output section for ion species detection, a control section, and a section for gas chromatographic (GC) analysis of a gas sample, the GC
section coupled to the inlet section, and the ionization section disposed for ionizing a gas sample from the GC section, the ionized sample passing to an ion filter in the ion filter section, and the control section applying a high field asymmetric period voltage and a control function to the ion filtering section to control species in the sample that are passed by the ion filter to the output section for detection.
2. The system of claim 1, wherein the ion filter section comprises at least one substrate and the ion filter comprises at least one planar electrode on the substrate, wherein the electrode is isolated from the output section by the substrate.
3. The system of claim 1, wherein the ion filter section comprises a pair of insulated substrates and the ion filter comprises at pair of planar electrodes, one on each a substrate.
4. The system of claim 1 further comprising:
a planar housing defining a flow path between the inlet section and the output section, the housing formed with at least a pair of substrates that extend along the flow path, the ion filter disposed in the flow path, the filter including at least one pair of filter electrodes, at least one on each substrate across from each other on the flow path; and the control section configured to apply an asymmetric periodic voltage to the ion filter electrodes for controlling the travel of ions through the filter.
5. The system of claim 1 further comprising a planar chamber defining a flow path, wherein the GC section separates the gas sample prior to ionization, and filtering proceeds in the planar chamber under influence of the high field asymmetric periodic signals, with detection integrated into the flow path, for producing accurate, real-time, orthogonal data for identification of a chemical species in the sample.
6. The system of claim 1 wherein the GC further comprises a capillary column for delivering the gas sample into the inlet, the gas sample includes a compound-containing carrier gas at a first flow rate.
7. The system of claim 6 wherein the inlet section, ionization section, ion filtering section, and output section communicate via a flow path, further comprising a drift gas source, the drift gas source supplying a drift gas into the inlet to carry the compound-containing carrier gas along the flow path to the output section.
8. The system of claim 7 further comprising a drift gas tube, wherein the capillary column is housed within the drift gas tube, the capillary column having a column outlet delivering the carrier gas and the drift gas flow surrounding the carrier gas flow at the column outlet.
9. The system of claim 8 further comprising a coupling, the coupling enabling receipt of the drift gas tube at the inlet with the capillary tube emptying into the inlet section from within the drift gas tube.
10. The system of claim 1 wherein the inlet section, ionization section, ion filtering section, and output section are formed on a planar surface, the planar surface defining a flow path along a longitudinal axis for the flow of ions in a gas sample from the ionization section, through the filter section, to the output section, wherein the output section comprises a detector for the detection of multiple ion species simultaneously.
11. The system of claim 10 wherein detector comprises a plurality of electrodes for detection of positive and negative ion species simultaneously.
12. The system of claim 1 further comprising an ionizer for ionizing the sample and for creating reactant ions, the reactant ions reacting with the ionized sample to create reactant ion data peaks, wherein the control section further comprises a circuit for extraction of retention time data from the sample by evaluation of the reactant ion data peaks.
13. The system of claim 1 further comprising apparatus for generation of complementary data for evaluation of a chemical compound in the sample, that data including retention time and another variable.
14. The system of claim 13 wherein the said another variable is intensity of the detected ion species.
15. The system of claim 14 further comprising a display coupled to the output section for display of at least two dimensional data representative of detected species.
16. The system of claim 15 wherein the control section further comprises pattern recognition part for identification of an ion species according to data detected at the output section.
17. The system of claim 16 wherein said data includes differential mobility spectra and retention time data.
18. The system of claim 1 further comprising an isolation part joining the ion filtering section, and output section, ions being delivered to the ion filter from the ionization section via a flow path, the isolation part facilitating non-conductive connection of the ion filter and the output section.
19. The system of claim 1 wherein the ion filtering section is further characterized a providing a short drift tube for rapid travel of filtered ions to the output part for detection.
20. The system of claim 19 wherein the ion filter further including a pair of electrodes, the electrodes facing each other across the flow drift tube.
21. The system of claim 19 wherein the ion filter further including a pair of electrodes, wherein the control section applies the high field asymmetric period voltage and control function as a control field to pair of electrodes to control species in the sample that are passed by the ion filter to the output section for detection, the drift tube defining a first flow path region for application of the control field to ions in the ion filter, the ion filter being located in the first flow path region, the output section comprising an ion detector region, the drift tube defining a second flow path region, the isolation part being located in the second flow path region after the first region and before the detector region; the ion filter part passing ions in the drift tube under influence of the control field, and ions that are passed by the filter part traveling through the isolation part to the detector region for detection, the isolation part isolating the control field from the detector region.
22. The system of claim 21 further comprising a pair of substrates, the substrates defining the drift tube, wherein the electrodes are electrically insulated and the substrates are electrically insulating.
23. The system of claim 22 wherein the substrates are planar.
24. The system of claim 1 further comprising:
at least pair of substrates defining between them a flow path for the flow of ions, ;
a plurality of electrodes, including a pair of ion filter electrodes disposed in the flow path between the inlet section and output section, one filter electrode associated with each substrate, the ion filter configured for receiving samples comprised of a variety of ion species and the filter electrodes cooperating with the control section applying to control the ions, the ion filter simultaneously passing a selected plurality of ion species to the detector part from the sample.
25. The system of claim 24 wherein the output part further comprises a detector part, the detector part enabling simultaneous detection of the selected plurality of ion species passed by the filter.
26. The system of claim 25 wherein the control section provides separate independent outputs at the detector part, the outputs providing signals representative of species detected simultaneously from within the samples.
27. The system of claim 26 wherein the detector part is formed with at least a pair of detector electrodes disposed in the flow path, at least one detector electrode is formed on a substrate, the detector electrodes carrying signals to the independent outputs representative of the detected ion species, one detector electrode being held at a first level and the second detector electrode being held at a second level for simultaneous detection of different ion species passed by the filter.
28. The system of claim 1 wherein the inlet section, ionization section, ion filtering section, and output section define between them a flow path for the flow of ions, further comprising a plurality of electrodes, including a pair of ion filter electrodes disposed in the flow path between the inlet section and output section.
29. The system of claim 28 wherein the plurality of electrodes comprises an array of electrodes formed in the flow path.
30. The system of claim 1 wherein the plurality of electrodes comprises an array of ion filters formed in the flow path, wherein each ion filter has its own flow channel, each flow channel being doped with a selected dopant for compound identification.
31. The system of claim 1 wherein the trajectory of an ion passing through the ion filter is regulated by control section, wherein the output section further comprises a detector, the detector comprising a plurality of electrodes in sequence to form a segmented detector, downstream from the ion filter, its segments separated along the flow path to detect ions spatially according to their trajectories.
32. The system of claim 1 wherein the inlet section, ionization section, ion filtering section, and output section define a flow path, further comprising a plurality of electrodes defined in the flow path to form an arrangement of electrodes, the plurality defining at least one filter electrode associated with each substrate to form an ion filter section.
33. The system of claim 32 further comprising a pair of substrates, wherein the ion filter comprises at least a pair of filter electrodes formed on the substrates, the substrates having at least an insulated surface along the flow path located between the filter electrodes and the output section.
34 The system of claim 33 further comprising a plurality of dedicated flow paths communicating with the output section, wherein the arrangement of elects odes comprises an array of filter electrode pairs associated with the dedicated flow paths.
35. The system of claim 33 further comprising a plurality of dedicated flow paths, wherein the arrangement of electrodes comprises an array of detector electrodes in the output part and in communication with the dedicated flow paths.
36. The system of claim 33 wherein the arrangement of electrodes comprises at least one pair of detector electrodes, one associated with each substrate, wherein the input part further comprises an ionization region and further comprising at least one electrode in the ionization region.
37. The system of claim 33 wherein the arrangement of electrodes further forms a segmented detector with several segments, each segment formed with at least one electrode on a substrate, the segments being formed in a longitudinal sequence along the flow path in the output part.
38. The system of claim 33 wherein the electronics part is further configured sweep the applied controlling signals through a predetermined range according to the species being filtered.
39. The system of claim 33 wherein the substrates form a device housing, the device housing supporting the input part, flow path, output part, electrodes, and electronics part.
40. The system of claim 33 further comprising a flow pump for drawing a gas sample through the flow path from the input part to the output part.
41. The system of claim 33 further comprising a third substrate, wherein the substrates are planar and define two flow paths.
42. The system of claim 41 wherein the input part includes an ionization source for the ionization of gas samples drawn by the flow pump, further comprising a second pump for recirculation of air in at least one flow path.
43. The system of claim 1 further comprising:
a spacer extending along a longitudinal axis defining a flow path between the inlet section and output section and the ion filter disposed in the flow path and including a pair of spaced filter electrodes, the control section including an electrical controller for applying an asymmetric periodic voltage across the ion filter electrodes and for generating a control field, the control field controlling the paths of ions traveling through the filter along the longitudinal axis toward the output section.
44. The system of claim 43 wherein the spacer cooperate with the electrodes to form a device housing enclosing the flow path.
45. The system of claim 43 wherein the outlet further comprises a detection area, the spacer defining a flow path extension extending along the longitudinal axis and connecting the input to the detection area, ions passed by the filter traveling to the detection area for detection.
46. The system of claim 45 wherein the detection area includes at least a pair of detector electrodes, further comprising an isolation part separating the ion filter from the detector, the isolating part isolating the control field from the detector electrodes.
47. The system of claim 43 wherein the spacer further defines longitudinal extensions, the flow path extending between the longitudinal extensions and extending along the spacer longitudinal axis.
48. The system of claim 43 further comprising a pair of substrates, the substrates cooperating with the spacer for defining the flow path between the inlet and outlet, the substrates further defining the filter electrodes facing each other across the flow path.
49. The system of claim 48 wherein the substrate has insulating surfaces that define an electrically insulated flow path portion between the inlet and the outlet, the outlet further comprising an ion detector.
50. The system of claim 43 wherein the spacer is silicon and defines confining electrodes in the flow path, further including a detector downstream from the ion filter for detecting ions traveling from the filter under control of the confining electrodes.
51. The system of claim 43 wherein the outlet further includes a detector, the detector formed with at least a pair of electrodes for detection of ions in the flow path, wherein the controller further defines electronic leads for applying signals to the electrodes.
52. The system of claim 43 wherein the outlet defines an array of detectors, the detectors formed each with a pair of electrodes disposed in the flow path for detection of ion species passed by the filter.
53. The system of claim 43 wherein the outlet comprises a detector, the detector comprising a pair of ion detector electrodes, wherein the electronics part is further configured to simultaneously independently enable detection of different ion species, the detected ions being representative of different detected ion species detected simultaneously by the detector, the electronics part including separate output leads from each detector electrode.
54. The system of claim 43 in which the outlet comprises a detector having a plurality of electrode segments, the segments separated along the flow path to spatially separate detection of ions according to their trajectories.
55. The system of claim 43 wherein the ion filter comprises an array of filters, each filter comprising a pair of electrodes in the flow path.
56. The system of claim 43 wherein the flow path is planar.
57. The system of claim 43 further comprising a source of ions at the inlet, a pump communicating with the flow path for driving of the ions through the filter.
58. The system of claim 43 further comprising a heater, in the flow path, for heating the flow path and purging neutralized ions.
59. The system of claim 58 wherein the heater comprises a pair of electrodes, the electrodes having at least one additional function.
60. The system of claim 59 wherein the heater electrodes include the ion filter electrodes.
61. The system of claim 60 wherein the electrical controller is configured to selectively apply a current through the filter electrodes to generate heat.
62. The system of claim 1 further comprising:
a pair of spaced substrates defining between them a flow path between the inlet and an output sections, the ion filter disposed in the path, further including at least a pair of spaced filer electrodes, the filter comprising at least one of the electrodes on each substrate, the control section further comprising a heater for heating the flow path.
63. The system of claim 62 wherein pair of the electrodes on the substrates is used as a heat source for the heater, the control section configured to deliver a heater signal to the heater source.
64. The system of claim 62 a pair of spaced substrates defining between them a flow path between the inlet and an output sections, the ion filter disposed in the path, further including at least a pair of spaced detector electrodes at least one of the detector electrodes on each substrate, the control section further comprising a heater for heating the flow wherein the control section uses the detector electrodes as a heat source.
65. The system of claim 1 wherein the control function is a duty cycle control function generated by the control section, a flow path extending between the inlet and output sections, the ion filter disposed in the flow path, the control section selectively adjusting the duty cycle of the asymmetric periodic voltage with the duty cycle control function to enable ion species from the inlet section to be separated, with desired species being passing through the ion filter for detection.
66. The ion mobility filter of claim 65 wherein the asymmetric periodic voltage is not compensated with a bias voltage, further including a detector downstream from the ion filter for detecting ion species that are passed by the filter.
67. A method for generating data for characterizing a chemical species in a gas sample, in a system having a flow path that defines an ion inlet, an output, and an ion mobility filter in the flow path between the inlet and the output, the filter passing ions flowing from the inlet to the output, the method comprising the steps of:
separating a gas sample with a GC and eluding the separated sample in a carrier gas to the ion inlet, ionizing the sample and applying a drift gas to the sample and carrying the ionized sample to the ion filter, applying an asymmetric periodic voltage to the ion filter for controlling the path of ions in the ionized sample while in the filter, and passing species through the ion filter for detection at the output part.
68. The method of claim 67 further comprising the steps of:
adjusting the duty cycle of the asymmetric periodic voltage to enable ion species to be separated according to their mobilities, and passing species through the filter according to the duty cycle for detection at the output part.
69. A method of analysis of compounds in chromatography, including:
separating chromatographically a gas mixture to be analyzed in a chromatographic column, ionizing the gas mixture, passing the ionized gas to a field asymmetric ion mobility spectrometer and passing components of the separated mixture through a high field asymmetric ion mobility filter, and detecting ions in the mixture according to their mobilities.
70. The method of claim 69 further comprising the step of applying a drift gas to the eluded sample to increase the flow volume and velocity of the ions through the spectrometer.
71. The method of claim 70 wherein the sample is eluded from the outlet of a capillary column of a GC, further comprising the step of surrounding the capillary column outlet with the flowing drift gas.
72. The method of claim 69 wherein the system has an ionizer for ionizing the sample and creating reactant ions, the reactant ions reacting with the ionized sample to create reactant ion data peaks, further comprising the step of obtaining GC retention time by monitoring the fluctuation in intensity of the reactant ion data peaks.
73. The method of claim 69 further comprising the steps of detecting positive and negative ions simultaneously by passing ions at high RF.
74. The method of claim 69 wherein the system has an ionizer for ionizing the sample, further comprising the step of processing detection data and obtaining retention time, compensation voltage and intensity, and relating this to the sample to identify its species.
75 A sensor system for characterizing a chemical species in a gas sample, comprising"
an inlet section, an ionization section, an ion filtering section, an output section for ion species detection, a control section, and a section for gas chromatographic (GC) analysis of a gas sample, the GC
section coupled to the inlet section, and the ionization section disposed for ionizing a gas sample from the GC section, the ionized sample passing to the ion filter section, the control section applying a high field asymmetric period voltage and a control function to the ion filter to control species in the sample that are passed by the filter to the output section for detection, a planar housing defining a flow path between a sample input part and an output part, the housing formed with at least a pair of substrates that extend along the flow path, an ion filter disposed in the flow path, the filter including at least one pair of filter electrodes, at least one on each substrate across from each other on the flow path, and the control section having a control part configured to apply an asymmetric periodic voltage to the ion filter electrodes for controlling the travel of ions through the filter.
CA2440429A 2001-03-05 2002-03-04 Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry Expired - Lifetime CA2440429C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US09/799,223 US6815668B2 (en) 1999-07-21 2001-03-05 Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry
US09/799,223 2001-03-05
PCT/US2002/006266 WO2002071053A2 (en) 2001-03-05 2002-03-04 Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry

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CA2440429A1 true CA2440429A1 (en) 2002-09-12
CA2440429C CA2440429C (en) 2012-07-10

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US (5) US6815668B2 (en)
EP (1) EP1377820A2 (en)
JP (1) JP4063673B2 (en)
AU (1) AU2002306623A1 (en)
CA (1) CA2440429C (en)
WO (1) WO2002071053A2 (en)

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US20050029443A1 (en) 2005-02-10
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US20050017163A1 (en) 2005-01-27
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US7176453B2 (en) 2007-02-13
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