US20090283674A1 - Efficient Atmospheric Pressure Interface for Mass Spectrometers and Method - Google Patents
Efficient Atmospheric Pressure Interface for Mass Spectrometers and Method Download PDFInfo
- Publication number
- US20090283674A1 US20090283674A1 US11/833,209 US83320907A US2009283674A1 US 20090283674 A1 US20090283674 A1 US 20090283674A1 US 83320907 A US83320907 A US 83320907A US 2009283674 A1 US2009283674 A1 US 2009283674A1
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- United States
- Prior art keywords
- transfer tube
- ion transfer
- interface
- sidewall
- ion
- Prior art date
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- 238000000034 method Methods 0.000 title description 18
- 238000012546 transfer Methods 0.000 claims abstract description 86
- 150000002500 ions Chemical class 0.000 claims description 154
- 239000011148 porous material Substances 0.000 claims description 5
- 238000000451 chemical ionisation Methods 0.000 claims description 3
- 238000000132 electrospray ionisation Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 238000004807 desolvation Methods 0.000 abstract description 9
- 230000007935 neutral effect Effects 0.000 description 14
- 230000009467 reduction Effects 0.000 description 5
- 230000032258 transport Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
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- 230000000694 effects Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/062—Ion guides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J3/00—Details of electron-optical or ion-optical arrangements or of ion traps common to two or more basic types of discharge tubes or lamps
- H01J3/14—Arrangements for focusing or reflecting ray or beam
Definitions
- This application is directed to ion inlet sections of mass spectrometers, ion transfer tube assemblies, ion transfer tubes, and methods of transporting ions from an atmospheric pressure ion source into a vacuum chamber of a mass spectrometer.
- U.S. Pat. No. 4,977,320 to Chowdhury et al. and others have relied upon the strong flow of gas that accompanies the sample spray through the capillary tube from an atmospheric pressure region into the vacuum region to help focus the droplets toward a center of the capillary tube.
- U.S. Pat. No. 5,157,260 to Mylchreest et al. teaches use of tube lenses at an exit end of the capillary tube for focusing ions.
- Others have utilized electrodes at various locations to focus and/or urge ions toward an orifice of a skimmer or other ion optical element to cause ions to enter lower pressure regions of mass spectrometers.
- an interface for a mass spectrometer in accordance with embodiments of the present invention includes an ion transfer tube having an inlet end opening to a high pressure chamber and an outlet end opening to a low pressure chamber.
- the high and low pressure chambers may be provided by any regions that have respective higher and lower pressures relative to each other.
- the high pressure chamber may be an ion source chamber and the low pressure chamber may be a first vacuum chamber.
- the ion transfer tube has at least one sidewall surrounding an interior region and extending along a central axis between the inlet end and the outlet end.
- the ion transfer tube has a plurality of passageways formed in the sidewall. The passageways permit the flow of gas from the interior region to a reduced-pressure region exterior to the sidewall.
- embodiments of the present invention include an ion transfer tube for receiving and transporting ions from a source in a high pressure region to ion optics in a reduced pressure region of a mass spectrometer.
- the ion transfer tube includes an inlet end, an outlet end, and at least one sidewall surrounding an interior region and extending along a central axis between the inlet end and the outlet end.
- the ion transfer tube may also include an integral vacuum chamber tube at least partially surrounding and connected to the ion transfer tube.
- the integral vacuum chamber tube isolates a volume immediately surrounding at least a portion of the ion transfer tube at a reduced pressure relative to the interior region.
- the sidewall has a structure that provides at least one passageway formed in the sidewall.
- the at least one passageway permits a flow of gas from the interior region to the volume exterior to the sidewall.
- the structure and passageway are inside the integral vacuum chamber tube.
- the structure of the sidewall may include a plurality of passageways.
- embodiments of the present invention include a method of transporting ions from an ion source region to a first vacuum chamber.
- the method includes admitting from the ion source region, a mixture of ions and gas to an inlet end of an ion transfer tube.
- the method also includes removing a portion of the gas through a plurality of passageways located intermediate the inlet end and an outlet end of the ion transfer tube.
- the method further includes causing the ions and the remaining gas to exit the ion transfer tube through the outlet end into the first vacuum chamber.
- the method may also include sensing a reduction in latent heat in the ion transfer tube due to at least one of removal of the portion of the background gas and an associated evaporation, and increasing an amount of heat applied to the ion transfer tube through a heater under software or firmware control.
- the embodiments of the present invention have the advantage of reduced flow of gas through an exit end of the ion transfer tube.
- the reduced flow through the exit end of the ion transfer tube decreases the energy with which the ion bearing gas expands as it leaves the ion transfer tube.
- the ions have a greater chance of traveling on a straight line through an aperture of a skimmer immediately downstream.
- reduction of the flow in at least a portion of the ion transfer tube may have the effect of increasing the amount of laminar flow in that portion of the ion transfer tube. Laminar flow is more stable so that the ions can remain focused and travel in a straight line for passage through the relatively small aperture of a skimmer.
- FIG. 1 is a diagrammatic view of an example mass spectrometer with which the embodiments of the present invention may be incorporated.
- FIG. 2 is a diagrammatic view of an inlet assembly in accordance with an embodiment of the present invention.
- FIG. 3 is a diagrammatic view of an inlet assembly in accordance with another embodiment of the present invention.
- FIG. 4 is a diagrammatic partial perspective view of an ion transfer tube in accordance with the embodiment of FIG. 3 .
- the ions are energetically moved throughout a volume of the flowing gas. It is postulated that because of this energetic and turbulent flow and the resultant mixing effect on the ions, the ions are not focused to a desirable degree and it is difficult to separate the ions from the neutral gas under these flow conditions. Thus, it is difficult to separate out a majority of the ions and move them downstream while the neutral gas is pumped away. Rather, many of the ions are carried away with the neutral gas and are lost.
- the hypothesis associated with embodiments of the present invention is that to the extent that the flow can be caused to be laminar along a greater portion of an ion transfer tube, the ions can be kept focused to a greater degree.
- One way to provide the desired laminar flow is to remove the neutral gas through a sidewall of the ion transfer tube so that the flow in an axial direction and flow out the exit end of the ion transfer tube is reduced. Also, by pumping the neutral gas out of the sidewalls to a moderate degree, the boundary layer of the gas flowing axially inside the ion transfer tube becomes thin, the velocity distribution becomes fuller, and the flow becomes more stable.
- One way to increase the throughput of ions or transport efficiency in atmospheric pressure ionization interfaces is to increase the conductance by one or more of increasing an inner diameter of the ion transfer tube and decreasing a length of the ion transfer tube.
- the inner diameter of the ion transfer tube can be made relatively large and at the same time flow out of the exit end of the ion transfer tube can be reduced to improve the flow characteristic for keeping ions focused toward a center of the gas stream.
- the neutral gas can be more readily separated from the ions, and the ions can be more consistently directed through the orifice of a skimmer into the ion optics and analyzer sections downstream. The result is improved transport efficiency and increased instrument sensitivity.
- FIG. 1 shows an example mass spectrometer 12 having an ion source 15 in a source chamber 16 and an interface 18 between the high pressure source chamber 16 and a lower pressure first vacuum chamber 19 .
- the ion source 15 may be, without limitation, an electrospray ionization source, a chemical ionization source, another liquid sample based atmospheric pressure ionization source, or any other source.
- the interface 18 may include an ion transfer tube portion 21 and an ion guide portion 24 with separate or shared pumping stages. Ions from the source 15 are introduced into the transfer tube portion 21 and move along an ion path generally on a central axis 25 through one or more additional sections to a detector 27 .
- the sections may include one or more of each of ion guides, filters, collision cells, and analyzers, as indicated by q 0 , Q 1 , q 2 , and Q 3 .
- the devices in each of these sections may be operated by an electronic controller 30 under software and/or firmware control to perform the needed functions for analysis of sample ions in the mass spectrometer 12 .
- a skimmer lens 33 separates the ion transfer tube portion 21 from the ion guide portion 24 of the interface 18 .
- an ion transfer tube 36 may be supported near its entrance end 39 on a chamber wall 42 between the source chamber 16 and the first vacuum chamber 19 . While FIG. 2 shows the ion transfer tube 36 with an inlet or entrance end opening in direct communication with the ion source 15 , it is to be understood that one or more reduced pressure chambers may be placed intermediate the ion source 15 and the ion transfer tube 36 . The one or more reduced pressure chambers may or may not have one or more additional ion transfer tubes therein.
- sidewall 45 of the ion transfer tube extends axially from the entrance end 39 to an exit end 48 and is surrounded by a heater 51 .
- the heater 51 may be placed in direct contact or otherwise in any kind of thermal contact with the ion transfer tube 36 .
- the skimmer lens 33 may have an aperture positioned proximate to the outlet or exit end 48 of the ion transfer tube 36 .
- a tube lens or other focusing lens 52 may be disposed between the exit end 48 of the ion transfer tube 36 and the skimmer lens 33 .
- An ion guide 54 may be located in a second vacuum chamber 57 downstream from the first vacuum chamber 19 .
- vacuum chamber may include any reduced pressure chamber or region that has a pressure that is lower than atmospheric pressure.
- High pressure and low pressure as used herein denote relative pressures in respective regions and are not to be limited to pressures relative to atmospheric or any other threshold pressure.
- Each of the first and second vacuum chambers 19 , 57 may be pumped by the same or separate vacuum pumps as indicated by arrows 58 , 59 .
- an interface 62 in accordance with another embodiment of the invention may include a third vacuum chamber 65 formed integrally as a unit with an ion transfer tube 68 , as shown in FIG. 3 .
- Walls create an enclosure that forms the third vacuum chamber 65 and at least partially surrounds an inner tube 71 that may be structurally analogous to the ion transfer tube 36 described with regard to the embodiment of FIG. 2 above.
- a separate pump or a pump in common with pump(s) of one or more of the first and second vacuum chambers 19 , 57 may be operably connected with the third vacuum chamber 65 in order to pump gas from within an interior region 74 inside the ion transfer tube 68 out through a sidewall 77 of the ion transfer tube 68 .
- the sidewall 77 of the ion transfer tube 68 extends axially from an entrance end 78 to an exit end 79 . Also, the sidewall 77 is surrounded by a heater 51 .
- the heater 51 may be placed in direct contact or otherwise in any kind of thermal contact with the ion transfer tube, as described with regard to the embodiment of FIG. 2 .
- FIG. 4 is a diagrammatic partial perspective view of the ion transfer tube 68 of FIG. 3 .
- the inner tube 71 and the interior region 74 may be substantially the same as the ion transfer tube 36 and an interior region thereof, in accordance with the embodiment of FIG. 2 .
- the sidewall 77 has one or more passageways 80 for fluid communication between the interior region 74 and an exterior region within the enclosure created by an enclosure sidewall 83 and enclosure end walls 86 , 87 , which walls form the third vacuum chamber 65 .
- neutral gas is pumped from within the interior region 74 and out through the passageways 80 of the sidewall 77 into the third vacuum chamber 65 where it is pumped away.
- the third vacuum chamber 65 encompasses a reduced-pressure region that is located within the enclosure and extends around the sidewall 77 .
- the enclosure is disposed within the first vacuum chamber 19 and communicates with a pump 91 that may be separate or in common with other pumps in the system.
- the ion transfer tube 36 of the embodiment of FIG. 2 may have similar structure in which the sidewall 45 has passageways 80 , and the neutral gas is pumped away by a pump in fluid communication with the first vacuum chamber 19 .
- a sensor 93 may be connected to the ion transfer tube 68 and to the controller 30 for sending a signal indicating a temperature of the sidewall 77 or some part of the ion transfer tube 68 back to the controller 30 . It is to be understood that a plurality of sensors may be placed at different positions to obtain a temperature profile.
- the senor(s) 93 may thus be connected to the ion transfer tube 68 for detecting a reduction in heat as gas is pumped through the plurality of passageways 80 in the sidewall 77 of the ion transfer tube 68 .
- the sensor(s) 93 may also be connected to the ion transfer tube 36 and controller 51 in the embodiment of FIG. 2 for heat reduction detection and control.
- the third vacuum chamber 65 may be utilized to introduce a flow of gas through the sidewall 71 and into an interior region 74 of the ion transfer tube 68 instead of removing the background gas, as described above. This may be achieved by adjusting the pressure in the third chamber 65 to be between atmospheric pressure and the pressure in the interior region 74 .
- By introducing a flow of gas through passageways 80 into the interior region 74 more turbulent flow conditions may be created in which sample droplets are disrupted. The more turbulent flow conditions may thus cause the sample droplets to be broken up into smaller droplets. This disruption of the droplets is an external force disruption, as opposed to a coulomb explosion type disruption which also breaks up the droplets.
- both removal and addition of gas may be applied in one ion transfer tube.
- the chamber 65 could be divided into plural regions with respective removal and addition of gas in a series of the plural regions.
- an alternating series of external force and coulomb explosion disruptions can be implemented to break up the droplets of the sample.
- the sidewall 45 of the ion transfer tube 36 and the sidewall 77 that forms at least a part of the inner tube 71 in the embodiments of FIGS. 1-4 may be formed from a material that includes one or more of a metal frit, a metal sponge, a permeable ceramic, and a permeable polymer.
- the passageways 80 may be defined by the pores or interstitial spaces in the material.
- the pores or interstices in the material of the sidewalls may be small and may form a generally continuous permeable element without discrete apertures.
- the passageways may take the form of discrete apertures or perforations formed in the sidewalls 45 , 77 of ion transfer tubes 36 , 68 .
- the passageways may be configured by through openings that have one or more of round, rectilinear, elongate, uniform, and non-uniform configurations.
- Embodiments of the present invention include a method of transporting ions from a source region into a vacuum region, a method of separating and removing a background gas from a mixture of the background gas and sample ions, and a method of desolvating a sample in an interface.
- One or more of the methods may include heating the ion transfer tube to promote evaporation of residual liquid solvent admitted into the ion transfer tube.
- the methods may include the step of removing at least a portion of the gas by providing a reduced-pressure region exterior to an inner tube of the ion transfer tube.
- the methods may also include sensing a reduction in latent heat in the ion transfer tube due to at least one of removal of the portion of the background gas and an associated evaporation.
- a subsequent step to sensing may be the step of increasing an amount of heat applied to the ion transfer tube through a heater under software or firmware control.
- the methods may include reducing a pressure in at least a portion of the ion transfer tube interior region such that desolvation is increased.
- the methods may include reducing the energy of a free jet expansion of the gas leaving the outlet or exit end of the ion transfer tube.
- the methods may also include reducing a velocity of a second downstream portion of the background gas that moves axially out an outlet or exit end of the ion transfer tube relative to a velocity of a first upstream portion of the background gas entering the ion transfer tube.
- the method may also include increasing a proportion of laminar flow along a length of the ion transfer tube.
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
- Sampling And Sample Adjustment (AREA)
Priority Applications (24)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US11/833,209 US20090283674A1 (en) | 2006-11-07 | 2007-08-02 | Efficient Atmospheric Pressure Interface for Mass Spectrometers and Method |
GB0909034.1A GB2456284B (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
DE112007002661.8T DE112007002661B4 (de) | 2006-11-07 | 2007-11-07 | Ionentransferanordnung |
CA2668762A CA2668762C (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
CA2668829A CA2668829C (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
CA2668763A CA2668763C (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
JP2009535623A JP2010508643A (ja) | 2006-11-07 | 2007-11-07 | イオン移送装置 |
CN201210111145XA CN102768936A (zh) | 2006-11-07 | 2007-11-07 | 离子迁移装置 |
PCT/EP2007/009642 WO2008061628A2 (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
US12/513,939 US7982183B2 (en) | 2006-11-07 | 2007-11-07 | Ion transfer tube with spatially alternating DC fields |
DE112007002694T DE112007002694T5 (de) | 2006-11-07 | 2007-11-07 | Ionentransferanordnung |
US12/513,944 US8148679B2 (en) | 2006-11-07 | 2007-11-07 | Efficient atmospheric pressure interface for mass spectrometers and method |
PCT/EP2007/009640 WO2008055667A2 (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
DE112007002686.3T DE112007002686B4 (de) | 2006-11-07 | 2007-11-07 | Ionentransferanordnung |
PCT/EP2007/009641 WO2008055668A2 (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
US12/513,954 US8148680B2 (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement with spatially alternating DC and viscous ion flow |
GB0909035.8A GB2456720B (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
CN2007800490189A CN101606220B (zh) | 2006-11-07 | 2007-11-07 | 离子迁移装置 |
JP2009535622A JP5197618B2 (ja) | 2006-11-07 | 2007-11-07 | イオン移送装置及びその方法 |
GB0909032A GB2456283B (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement |
CN2007800490085A CN101606219B (zh) | 2006-11-07 | 2007-11-07 | 离子迁移装置 |
JP2009535621A JP5011393B2 (ja) | 2006-11-07 | 2007-11-07 | イオン移送装置 |
JP2012043734A JP5575165B2 (ja) | 2006-11-07 | 2012-02-29 | イオン移送装置及びその方法 |
US13/413,568 US8642949B2 (en) | 2006-11-07 | 2012-03-06 | Efficient atmospheric pressure interface for mass spectrometers and method |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US85773706P | 2006-11-07 | 2006-11-07 | |
US11/833,209 US20090283674A1 (en) | 2006-11-07 | 2007-08-02 | Efficient Atmospheric Pressure Interface for Mass Spectrometers and Method |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US12/513,939 Continuation-In-Part US7982183B2 (en) | 2006-11-07 | 2007-11-07 | Ion transfer tube with spatially alternating DC fields |
Publications (1)
Publication Number | Publication Date |
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US20090283674A1 true US20090283674A1 (en) | 2009-11-19 |
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ID=39321490
Family Applications (4)
Application Number | Title | Priority Date | Filing Date |
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US11/833,209 Abandoned US20090283674A1 (en) | 2006-11-07 | 2007-08-02 | Efficient Atmospheric Pressure Interface for Mass Spectrometers and Method |
US12/513,944 Active 2028-04-25 US8148679B2 (en) | 2006-11-07 | 2007-11-07 | Efficient atmospheric pressure interface for mass spectrometers and method |
US12/513,954 Active 2028-04-20 US8148680B2 (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement with spatially alternating DC and viscous ion flow |
US13/413,568 Active US8642949B2 (en) | 2006-11-07 | 2012-03-06 | Efficient atmospheric pressure interface for mass spectrometers and method |
Family Applications After (3)
Application Number | Title | Priority Date | Filing Date |
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US12/513,944 Active 2028-04-25 US8148679B2 (en) | 2006-11-07 | 2007-11-07 | Efficient atmospheric pressure interface for mass spectrometers and method |
US12/513,954 Active 2028-04-20 US8148680B2 (en) | 2006-11-07 | 2007-11-07 | Ion transfer arrangement with spatially alternating DC and viscous ion flow |
US13/413,568 Active US8642949B2 (en) | 2006-11-07 | 2012-03-06 | Efficient atmospheric pressure interface for mass spectrometers and method |
Country Status (7)
Cited By (7)
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US8610054B2 (en) | 2009-05-01 | 2013-12-17 | Shimadzu Corporation | Ion analysis apparatus and method of use |
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US20190237314A1 (en) * | 2015-08-21 | 2019-08-01 | PharmaCadence Analytical Services, LLC | Novel methods of evaluating performance of an atmospheric pressure ionization system |
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