US3886365A - Multiconfiguration ionization source - Google Patents

Multiconfiguration ionization source Download PDF

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Publication number
US3886365A
US3886365A US391721A US39172173A US3886365A US 3886365 A US3886365 A US 3886365A US 391721 A US391721 A US 391721A US 39172173 A US39172173 A US 39172173A US 3886365 A US3886365 A US 3886365A
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US
United States
Prior art keywords
source
chamber
ionization
electron
opening
Prior art date
Legal status (The legal status 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 status listed.)
Expired - Lifetime
Application number
US391721A
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English (en)
Inventor
William P Kruger
John A Michnowicz
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HP Inc
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Hewlett Packard Co
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 Hewlett Packard Co filed Critical Hewlett Packard Co
Priority to US391721A priority Critical patent/US3886365A/en
Priority to GB3521874A priority patent/GB1450320A/en
Priority to CA206,890A priority patent/CA1008976A/en
Priority to DE19742439711 priority patent/DE2439711B2/de
Priority to CH1145774A priority patent/CH582424A5/xx
Priority to FR7428982A priority patent/FR2246059B1/fr
Priority to JP9832774A priority patent/JPS5321873B2/ja
Priority to US05/568,499 priority patent/US3992632A/en
Application granted granted Critical
Publication of US3886365A publication Critical patent/US3886365A/en
Priority to US05/914,660 priority patent/USRE30171E/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • H01J49/147—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers with electrons, e.g. electron impact ionisation, electron attachment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • H01J49/145—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using chemical ionisation

Definitions

  • a hollow i 1 Flledi g- 9 1973 chamber including an ion source and a source of sam- [21] APPL No: 391,721 ple molecules receives a hollow, slidable cylindrical member having a chemical ionization chamber within it. Orifices in the chamber and the cylindrical member I Cl 250/423; 250/427 connect the chemical ionization source chamber to [51 1 Int. Cl. the electron sgurce and to the sample molecule ource Field of Search 250/424, 423, 427 when the cylindrical member is pulled to one position.
  • the slidable cylindrical member and the inside UNITED STATES PATENTS walls of the chamber define the ionization region to 3.115591 12/1963 Brunnee a. 250/423 WhiCh the electron mum and the Sample molecule 3355.587 11/1967 j k n 25 7 source are directly connected.
  • the ionization source can be changed 3.553. 1/197!
  • Commonly used sources are the electron impact source and the chemical ionization source.
  • the first one has a large electron entrance, :1 large ion exit. and an ionization region where the incoming electrons fragment as well as ionize vapor molecules thus providing a large quantity of information which does not necessarily give clear indication of the identity of a substance.
  • the chemical ionization source has, on the other hand, a small electron entrance, a small ion exit, and an ionization region where the pres sure can be maintained at such levels that ionmolecule collisions are extremely likely to occur, such collisions leading to ready identification of the molecular weight of a substance.
  • An object of this invention is to permit changing between the electron impact and the chemical ionization configurations with minimal interruption of operation of the mass spectrometer.
  • this inven tion provides an ionization source with two distinct ion ization chambers, one which operates as an electron impact ionization source and the other as a chemical ionization source.
  • the invention may be used with a mass spectrometer and changes in configuration can be made easily and quickly.
  • the main elements of the invention include a hollow chamber having a plurality of orifices transverse to the longitudinal axis of the chamber. One of the orifices contains an electron source, and another one is a gaseous sample inlet.
  • a hollow slidable cylindrical member having smaller transverse orifices than those in the hollow chamber fits inside the hollow chamber.
  • the cylindrical member has two electrode inserts separated from each other along the longitudinal axis and defining a first ionization region between them and the inside walls of the hollow cylindrical member, This region is connected to the sample inlet orifice and to the electron source orifice when the hollow cylinder is in a first position.
  • a second ionization region is defined by the inside walls of the hollow chamber, the outer electrode insert of the cylindrical member, and the open end of the hollow chamber, when the cylindrical member is in a second position. This second region is directly connected to the electron source orifice and to the sample inlet.
  • the source operates as a chemical ionization source and when the cylindrical member is in the second position, the source operates as an electron impact source.
  • the position of the cylindrical member can be changed quickly and easily by simply pushing or pulling a handle attached to the cylinder.
  • FIG. 1 shows a cross-sectional view of the preferred embodiment of the present invention in the chemical ionization configuration.
  • FIG. 2 shows the apparatus of FIG. I in the electron impact configuration.
  • FIGS. I and 2 show a vacuum envelope I4 which is connected to an ordinary vacuum pump through a port 9 for evacuating air from the envelope.
  • An ion chamber I6, which may be a stainless steel tube. is supported within envelope I4 by a support member I2 and has orifices, l7, I7 and 23 transverse to its longitudinal axis.
  • Orifice [7 contains a filament 18 near the periphery of ion chamber 16 and near an end 19 of ion chamber I6.
  • Orifice 23 is an inlet for samples to be ionized.
  • the ion chamber 16 has a preferably cylindrical bore 24 along the longitudinal axis. Filament orifice I7 intersects bore 24 near end 19.
  • a hollow member 28 fits slidably inside bore 24, which member may be made of stainless steel tubingv Electrode inserts 35 and 36 are supported by and fastened to the inside of slide member 28 by insulators preferably made of ceramic. Insert 35 is located at end 21 of member 28 and has a passage 34 through it. Insert 36 is spaced apart fom insert 35 and has a passage 39 through it. A connector 38 passes through passage 39 and engages passage 34 in insert 35 when member 28 has been moved to the left as shown in FIG. 2. A spring 40 attaches connector 38 to a base block 42, and this block is in turn affixed to but electrically insulated from chamber 16. Slide member 28 has a slot 44 through which base block 42 passes. The external surface of hollow member 28 is preferably hardened to prevent galling or binding with chamber 16.
  • a handle 48 attaches to end 53 of hollow member 28 and is used to displace this member from the first position to the second position as shown in FIGS. 1 and 2 respectively.
  • a bellows 46 surrounds handle 48 and connects the end 53 of hollow member 28 with a wall 55 of vacuum envelope 14.
  • a support member 12 surrounds the bellows 46 and affixes the chamber 16 to wall 55.
  • a pivot axle between a support member 71 and an arm 72 permits pulling or pushing arm 72, which is connected to handle 48, for placing cylinder 28 in either the chemical ionization configuration as shown in FIG. I or the electron impact configuration as shown in FIG. 2.
  • Arm 72 is connected to handle 48 by a Vernier screw arrangement 73 for making fine alignment adjustments of electron passage 32 with filament orifice 17.
  • electrode inserts 35 and 36 and the inner periphery of hollow member 28 define a first ionization region 30 when hollow member 28 is to the right, as in FIG. 1.
  • a second ionization region 30' is defined by the interior walls of chamber body 16, the electrode insert 35 to the left, and the open end I9 of chamber 16 to the right.
  • a passage 32 through the wall of hollow member 28 permits entry of electrons into the ionization region 30 from orifice 17 when hollow member 28 is to the rightv
  • a sample inlet 23 through the walls of ion chamber 16 permits entry of an ionization sample into ionization region 30 when cylinder 28 is to the left as shown in FIG. 2.
  • Sample inlet 23, and sample inlet 20 passing through the walls of hollow member 28, permit entry of an ionization sample into ionization region 30, when hollow member 28 is to the right as shown in FIG. 1.
  • a passage 34 permits exit of ions from the ionization region 30 to an ion lens assembly 26.
  • Both passages 32 and 34 may have a conical configuration to improve entry of the electrons through the first passage and exit ofthe ions through the second passage.
  • Passages 32 and 34, the electron entrance and ion exit passages respectively of the chemical ioniza tion chamber. are much smaller than the respective passages 17 and 2] of the electron impact chamber. The smaller size of passages 32 and 34 permits maintaining a higher pressure in ionization region 30 than in ionization region 30'.
  • Magnets 52 and 52' are located adjacent to filament l8 and to an electron collector 50, respectively. which is disposed on the periphery of chamber [6 diametrically opposed to filament 18. The magnets direct an electron beam from the filament to the collector.
  • the ion lens assembly 26, adjacent to end 19, extends away from chamber 16 and. when the appropriate potentials are applied, focuses ions emerging from ionization re gions 30 and 30 into a mass filter for analysis (not shown).
  • a potential source 70 is connected to insert 35 by connector 38 to maintain insert 35 at a potential for re pelling ions when the hollow member 28 is to the left. as shown in FlG. 2.
  • connector 38 engages only insert 36 to maintain a repelling potential on this insert. which insert b now becomes a repeller electrode.
  • the ionization source When the hollow cylindrical member is to the left the ionization source is operating in the electron im pact configuration where the pressure inside ionization region 30' is about l Torr; the ionization electrons have energies of about 70 eV; and mean-free-paths of about 2 X l0 inches.
  • the electrons in this configuration fragment the sample molecules and produce many ions whose mass'to-charge ratios do not necessarily correspond to the molecular weight of the sample.
  • the ionization source When the hollow cylindrical member is to the right, the ionization source is operating in the chemical ioniza tion configuration where the pressure in ionization re gion 30 is up to 1.0 Torr; the ionization electrons have energies of about 100 to 500 eV; and short mean-freepaths of about 2 X inches.
  • the electrons in this configuration do not fragment the sample molecules as much as in the electron impact configuration. but produce an abundance of ions whose mass-tocharge ratio corresponds more accurately to the molecular weight of the sample.
  • a multiconfiguration. multimode ionization source comprising:
  • a chamber having walls surrounding an internal cavity and mounted within the envelope. said chamber having a plurality of openings;
  • an electron source disposed exterior to the chamber for supplying electrons to the chamber through a first of said openings
  • sample inlet means for supplying a gaseous sample through a second of said openings for reaction with the electrons inside the chamber to create ions. said ions exiting through a third of said openings;
  • aperture control means for changing the size of the first and third openings for changing the pressure ofthe sample in the chamber. thereby changing the operating mode of the source from a first to a sec ond ionization mode;
  • ion repelling means disposed inside the chamber for repeliing ions out of the chamber through the third opening.
  • the aperture control means comprises a movable member within the chamber. said member having an electron opening smaller than said first opening and also having an ion opening smaller than said third opening:
  • said electrons from the source pass through the electron opening and the first opening when said movable member is in a first position
  • said electrons pass through only the first opening and said ions pass through only the third opening when the movable member is in a second position.
  • a multiconfiguration ionization source as in claim 3 including:
  • a bellows having a first end attached to the handle end of the cylinder and by a second end to a wall of the vacuum tight envelope;
  • a handle surrounded by the bellows one end of said handle attaches to the cylinder while the other end of the the handle protrudes through said vacuum tight envelope wall.
  • a multiconfiguration ionization source as in claim 4 wherein there is an electron collector opposite the electron source. and wherein there are magnets disposed adjacent the electron source and the electron collector to direct the electrons from the electron source.
  • a first and second repeller electrode mounted in and electrically insulated from the hollow slidable cylinder'.
  • a connector connectable to a source of potential for making an electrical connection with the first repeller electrode when the slidable cylinder is in the first position and with the second repeller electrode when the slidable cylinder is in the second position.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Electron Tubes For Measurement (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Sources, Ion Sources (AREA)
US391721A 1973-08-27 1973-08-27 Multiconfiguration ionization source Expired - Lifetime US3886365A (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
US391721A US3886365A (en) 1973-08-27 1973-08-27 Multiconfiguration ionization source
GB3521874A GB1450320A (en) 1973-08-27 1974-08-09 Multiconfiguration ionization source
CA206,890A CA1008976A (en) 1973-08-27 1974-08-13 Multiconfiguration ionization source
DE19742439711 DE2439711B2 (de) 1973-08-27 1974-08-19 Ionenquelle
CH1145774A CH582424A5 (de) 1973-08-27 1974-08-22
FR7428982A FR2246059B1 (de) 1973-08-27 1974-08-23
JP9832774A JPS5321873B2 (de) 1973-08-27 1974-08-27
US05/568,499 US3992632A (en) 1973-08-27 1975-04-16 Multiconfiguration ionization source
US05/914,660 USRE30171E (en) 1973-08-27 1978-06-12 Multiconfiguration ionization source

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US391721A US3886365A (en) 1973-08-27 1973-08-27 Multiconfiguration ionization source

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US05/568,499 Continuation US3992632A (en) 1973-08-27 1975-04-16 Multiconfiguration ionization source
US05/914,660 Continuation USRE30171E (en) 1973-08-27 1978-06-12 Multiconfiguration ionization source

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US3886365A true US3886365A (en) 1975-05-27

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US391721A Expired - Lifetime US3886365A (en) 1973-08-27 1973-08-27 Multiconfiguration ionization source

Country Status (7)

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US (1) US3886365A (de)
JP (1) JPS5321873B2 (de)
CA (1) CA1008976A (de)
CH (1) CH582424A5 (de)
DE (1) DE2439711B2 (de)
FR (1) FR2246059B1 (de)
GB (1) GB1450320A (de)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3992632A (en) * 1973-08-27 1976-11-16 Hewlett-Packard Company Multiconfiguration ionization source
US4037108A (en) * 1975-04-03 1977-07-19 Helmut Jordan Ion source with capability of changing between operation modes
US4105916A (en) * 1977-02-28 1978-08-08 Extranuclear Laboratories, Inc. Methods and apparatus for simultaneously producing and electronically separating the chemical ionization mass spectrum and the electron impact ionization mass spectrum of the same sample material
EP0060075A2 (de) * 1981-03-06 1982-09-15 Finnigan Corporation Ionisator mit auswechselbarer Ionisationskammer
US4377745A (en) * 1978-12-01 1983-03-22 Cherng Chang Mass spectrometer for chemical ionization, electron impact ionization and mass spectrometry/mass spectrometry operation
US4447728A (en) * 1982-02-05 1984-05-08 Finnigan Corporation Ionizer including discharge ion source and method
US5302827A (en) * 1993-05-11 1994-04-12 Mks Instruments, Inc. Quadrupole mass spectrometer
US5331158A (en) * 1992-12-07 1994-07-19 Hewlett-Packard Company Method and arrangement for time of flight spectrometry
US6646257B1 (en) 2002-09-18 2003-11-11 Agilent Technologies, Inc. Multimode ionization source
US20040079881A1 (en) * 2002-09-18 2004-04-29 Fischer Steven M. Multimode ionization source
US20050211911A1 (en) * 2002-09-18 2005-09-29 Fischer Steven M Apparatus and method for sensor control and feedback
US20060038122A1 (en) * 2004-08-19 2006-02-23 Linden H B Ion source with adjustable ion source pressure combining ESI-, FI-, FD-, LIFDI- and MALDI-elements as well as hybrid intermediates between ionization techniques for mass spectrometry and/or electron paramagnetic resonance spectrometry
US20080116369A1 (en) * 2006-11-17 2008-05-22 Mccauley Edward B Method and apparatus for selectively performing chemical ionization or electron ionization

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5165882U (de) * 1974-11-18 1976-05-24
JPS51115073U (de) * 1975-03-14 1976-09-18
JPS5815899Y2 (ja) * 1975-04-24 1983-03-31 株式会社島津製作所 シツリヨウブンセキケイヨウイオンゲン
JPS55171837U (de) * 1979-05-26 1980-12-10
JPS60165863U (ja) * 1985-02-27 1985-11-02 株式会社島津製作所 質量分析装置

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3115591A (en) * 1959-06-22 1963-12-24 Atlas Werke Ag Ion source for mass spectrometer
US3355587A (en) * 1951-01-28 1967-11-28 Jenckel Ludolf Gas analysis apparatus comprising plural ionization chambers with different ionizing electron beam energy levels in the chambers
US3405263A (en) * 1966-01-14 1968-10-08 Exxon Research Engineering Co Dual mass spectrometer ion source comprising field ionization and electron bombardment sources and the method of use
US3553452A (en) * 1969-02-17 1971-01-05 Us Air Force Time-of-flight mass spectrometer operative at elevated ion source pressures
US3555272A (en) * 1968-03-14 1971-01-12 Exxon Research Engineering Co Process for chemical ionization for intended use in mass spectrometry and the like
US3582645A (en) * 1966-11-19 1971-06-01 Varian Mat Gmbh Combined field and impact ionization source for mass spectrometers

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3355587A (en) * 1951-01-28 1967-11-28 Jenckel Ludolf Gas analysis apparatus comprising plural ionization chambers with different ionizing electron beam energy levels in the chambers
US3115591A (en) * 1959-06-22 1963-12-24 Atlas Werke Ag Ion source for mass spectrometer
US3405263A (en) * 1966-01-14 1968-10-08 Exxon Research Engineering Co Dual mass spectrometer ion source comprising field ionization and electron bombardment sources and the method of use
US3582645A (en) * 1966-11-19 1971-06-01 Varian Mat Gmbh Combined field and impact ionization source for mass spectrometers
US3555272A (en) * 1968-03-14 1971-01-12 Exxon Research Engineering Co Process for chemical ionization for intended use in mass spectrometry and the like
US3553452A (en) * 1969-02-17 1971-01-05 Us Air Force Time-of-flight mass spectrometer operative at elevated ion source pressures

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3992632A (en) * 1973-08-27 1976-11-16 Hewlett-Packard Company Multiconfiguration ionization source
US4037108A (en) * 1975-04-03 1977-07-19 Helmut Jordan Ion source with capability of changing between operation modes
US4105916A (en) * 1977-02-28 1978-08-08 Extranuclear Laboratories, Inc. Methods and apparatus for simultaneously producing and electronically separating the chemical ionization mass spectrum and the electron impact ionization mass spectrum of the same sample material
US4377745A (en) * 1978-12-01 1983-03-22 Cherng Chang Mass spectrometer for chemical ionization, electron impact ionization and mass spectrometry/mass spectrometry operation
EP0060075A2 (de) * 1981-03-06 1982-09-15 Finnigan Corporation Ionisator mit auswechselbarer Ionisationskammer
EP0060075A3 (en) * 1981-03-06 1982-12-08 Finnigan Corporation Ionizer having interchangeable ionization chamber
US4388531A (en) * 1981-03-06 1983-06-14 Finnigan Corporation Ionizer having interchangeable ionization chamber
US4447728A (en) * 1982-02-05 1984-05-08 Finnigan Corporation Ionizer including discharge ion source and method
US5331158A (en) * 1992-12-07 1994-07-19 Hewlett-Packard Company Method and arrangement for time of flight spectrometry
US5302827A (en) * 1993-05-11 1994-04-12 Mks Instruments, Inc. Quadrupole mass spectrometer
USRE35701E (en) * 1993-05-11 1997-12-30 Mks Instruments, Inc. Quadrupole mass spectrometer
US20040079881A1 (en) * 2002-09-18 2004-04-29 Fischer Steven M. Multimode ionization source
US6646257B1 (en) 2002-09-18 2003-11-11 Agilent Technologies, Inc. Multimode ionization source
US20050211911A1 (en) * 2002-09-18 2005-09-29 Fischer Steven M Apparatus and method for sensor control and feedback
US7078681B2 (en) 2002-09-18 2006-07-18 Agilent Technologies, Inc. Multimode ionization source
US7091483B2 (en) 2002-09-18 2006-08-15 Agilent Technologies, Inc. Apparatus and method for sensor control and feedback
US20070023675A1 (en) * 2002-09-18 2007-02-01 Fischer Steven M Multimode ionization source
US7488953B2 (en) 2002-09-18 2009-02-10 Agilent Technologies, Inc. Multimode ionization source
EP1507282A3 (de) * 2003-08-13 2005-07-27 Agilent Technologies Inc. (a Delaware Corporation) Multimode-Ionenquelle.
US20060038122A1 (en) * 2004-08-19 2006-02-23 Linden H B Ion source with adjustable ion source pressure combining ESI-, FI-, FD-, LIFDI- and MALDI-elements as well as hybrid intermediates between ionization techniques for mass spectrometry and/or electron paramagnetic resonance spectrometry
GB2418774A (en) * 2004-08-19 2006-04-05 Bernhard Hans Linden Multimode ion source
GB2418774B (en) * 2004-08-19 2008-09-24 Bernhard Hans Linden Ion source combining esi-, fi-, fd- lifdi- and maldi elements
US20080116369A1 (en) * 2006-11-17 2008-05-22 Mccauley Edward B Method and apparatus for selectively performing chemical ionization or electron ionization
US7791042B2 (en) 2006-11-17 2010-09-07 Thermo Finnigan Llc Method and apparatus for selectively performing chemical ionization or electron ionization

Also Published As

Publication number Publication date
JPS5321873B2 (de) 1978-07-05
FR2246059A1 (de) 1975-04-25
CA1008976A (en) 1977-04-19
JPS5047688A (de) 1975-04-28
FR2246059B1 (de) 1978-11-10
CH582424A5 (de) 1976-11-30
DE2439711B2 (de) 1977-09-15
DE2439711A1 (de) 1975-04-10
GB1450320A (en) 1976-09-22

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