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EP0000865B1 - Source d'ions comportant une chambre d'ionisation pour l'ionisation chimique - Google Patents

Source d'ions comportant une chambre d'ionisation pour l'ionisation chimique Download PDF

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Publication number
EP0000865B1
EP0000865B1 EP78100259A EP78100259A EP0000865B1 EP 0000865 B1 EP0000865 B1 EP 0000865B1 EP 78100259 A EP78100259 A EP 78100259A EP 78100259 A EP78100259 A EP 78100259A EP 0000865 B1 EP0000865 B1 EP 0000865B1
Authority
EP
European Patent Office
Prior art keywords
ionization chamber
ionization
primary particles
chamber
substance
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
Application number
EP78100259A
Other languages
German (de)
English (en)
Other versions
EP0000865A1 (fr
Inventor
Gerhard Weiss
Gerhard Dipl.-Phys. Weisz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bruker Daltonics GmbH and Co KG
Original Assignee
Bruken Franzen Analytik GmbH
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 Bruken Franzen Analytik GmbH filed Critical Bruken Franzen Analytik GmbH
Publication of EP0000865A1 publication Critical patent/EP0000865A1/fr
Application granted granted Critical
Publication of EP0000865B1 publication Critical patent/EP0000865B1/fr
Expired legal-status Critical Current

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Classifications

    • 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

  • the invention relates to an ion source with an ionization chamber for the chemical ionization of substance vapors by ion-molecule reactions using ionizing primary particles and a reactant gas, with inlet openings for supplying the ionizing primary particles, the reactant gas and the substance gas and an outlet opening for the reaction products formed in the chamber , wherein the inlet opening for the ionizing primary particles is opposite the outlet opening.
  • the ionization of atoms or molecules, in particular organic substances, by means of an ion-molecule reaction, also called chemical ionization, has the advantage over the usual ionization by means of electron impact that fragmentation of the investigated substances is low and furthermore enables a higher sensitivity in principle, but in practice is not yet achieved with ionization chambers of conventional design.
  • Chemical ionization usually takes place in an ionization chamber between the ions of a reactant gas and the molecules of the substance to be examined at pressures of 0.1 to 2 mbar, in particular in the range of 0.5 to 1 mbar.
  • the pressure is generated essentially by the reactant gas while having mbar to substance under investigation with their vapors or its gas only has a partial pressure of 10- 6 to 10-.
  • the reactant gas and the gas or vapor of the substance to be investigated are either mixed or generally introduced individually into the ionization chamber through special openings.
  • the reactant gas must have an ionization energy whose level is higher than the ionization energy of the desired productions of the substance to be investigated; Common reactant gases are isobutane, methane, water vapor or ammonia.
  • the reactant gas is usually partially ionized by a primary ionization process, in that electrons generated by a hot cathode enter the ionization chamber through a focussing aperture and react there with the reactant gas.
  • the resulting reactant gas ions then react - partly via intermediate processes with the participation of further reactant gas molecules - with the molecules of the substance to be investigated, the reactions taking place quickly and with a high yield because of the extraordinarily large cross sections of the reaction. Since recombinations of the resulting productions are only possible in triplets due to the selected energy levels, the productions remain ionized for a long time, i.e. up to a time of several minutes.
  • the yield of the ionized molecules of the substance to be examined relates to 50 to 100% if the conditions for carrying them out are selected appropriately.
  • the electrons for the primary ionization process of the reactant gas are injected into the ionization chamber with an energy of a few hundred electron volts, generally 100-500 eV.
  • the simultaneous direct ionization of molecules of the substance to be investigated that occurs is negligible.
  • primary ionization can also be achieved by chemical ionization with suitably introduced ions, for example noble gas, H 2 , N 2 or O 2 ions, as described by B. Högger and P. Bommer in Int. J. Mass Spectrom. Ion. Phys. 13, 35 (1974) and by DF Hunt, CN McEwen and TM Harvey in Anal. Chem. 47, 1730 (1975).
  • ions for example noble gas, H 2 , N 2 or O 2 ions
  • the ions of the substance to be investigated emerge together with all other ionic and neutral particles from a small outlet opening into the surrounding vacuum of a mass spectrometer and are fed to the analysis volume by suitable electrostatic acceleration and focusing fields.
  • this outlet opening are particularly critical since, on the one hand, a small channel-like opening causes too many wall impacts of the ions, as a result of which the ions are discharged and the ion yield is therefore reduced to a fraction; on the other hand, a large, hole-like outlet makes it difficult to maintain the pressure in the ionization chamber and therefore requires an excessively large pumping power on the mass spectrometer. Therefore, the practically achieved yield of commercially available ion sources for chemical ionization is generally below 10- 3 Ions per substance molecule.
  • the present invention has for its object to improve the known ionization chambers for chemical ionization of the type described above while avoiding their disadvantages and, in particular, to create an ionization chamber which gives an increased yield of ions of the substance to be investigated at low chamber pressures.
  • this object is achieved with an ionization chamber of the generic type in that the ionization chamber is elongated and cylindrical; that the inlet opening for the ionizing primary particles, on the one hand, and the outlet opening for the reaction products, on the other hand, are provided in alignment with one another on the longitudinal axis of the ionization chamber in its opposite end walls; and that a separate inlet opening for the reactant gas and / or the substance vapor is provided and is arranged spatially adjacent to the inlet opening for the ionizing primary particles.
  • the ionization chamber is thus given an elongated cylindrical shape, at one end of which the reactants enter, in particular through different inlet openings, and at the other end of which the resulting reaction products flow out through a common, central opening.
  • the ionizing primary particles also enter through a central opening at the entrance end of the elongated ionization chamber so that the ionization reactions take place along the longitudinal axis of the ionization chamber.
  • Another advantage of the ionization chamber according to the invention is that the mixing of the reactants and the primary ions is facilitated by the geometrical shape of the ionization chamber and by the pressure reduction which is brought about.
  • a longitudinal magnetic field is present along the ionization chamber.
  • the magnetic field is generated by a permanent magnet, and it can further be provided that the permanent magnet consists of a number of individual ring magnets surrounding the elongated ionization chamber.
  • a magnetic coil can also be arranged around the ionization chamber.
  • Preferred embodiments of the invention are alternatively characterized in that there is an electrical multipole in the interior of the ionization chamber composed of at least four radially symmetrically arranged, insulated, elongated pole rods, to which symmetrical or asymmetrical high-frequency alternating voltages are applied in pairs or that the wall of the ionization chamber is designed as a multipole tube with electrodes, to which symmetrical or asymmetrical high-frequency alternating voltages are applied in pairs.
  • inventions can be configured in a preferred manner in that the pole rods or the pole faces of the metal electrodes run parallel to the axis of symmetry of the ionization chamber or that the pole rods or the pole faces of the metal electrodes are arranged conically to the axis of symmetry of the ionization chamber. As a result, the particles are kept in a corresponding manner near the axis.
  • Another embodiment of the invention provides that a potential gradient is provided in the longitudinal axis of the ionization chamber.
  • the generated electrostatic potential drop causes the desired ions to drift in the direction of the outlet opening.
  • the potential gradient can be generated by a charged pusher or by applying a voltage to isolated end faces of the chamber.
  • a diaphragm arrangement associated with the outlet opening and generating an electrostatic lens field that engages symmetrically to the longitudinal axis of the ionization chamber can also be provided.
  • the diaphragm arrangement effects a focusing extraction of the ions from the ionization chamber, with particular emphasis
  • the advantage is that the substance ions are thereby detected at a point in the ionization chamber at which the longitudinal magnetic field does not yet have any disruptive edge effects.
  • the chamber is preceded by a gas discharge chamber in which the ionizing primary particles are generated.
  • the ionization chamber according to the invention thus differs from the known ionization chambers in particular in that the ionizing primary particles are injected perpendicularly to the outflow direction, while according to the invention the ionizing primary particles are injected in the escape opening or in that the known ionization chambers, because of their brevity, have a pressure of need at least 0.1 mbar to achieve a high ion yield.
  • a gas discharge chamber 3 is connected upstream of an actual ionization chamber 1. At the end of the gas discharge chamber 3 opposite the ionization chamber 1, an electrode 5 is attached within the gas discharge chamber 3.
  • the gas discharge chamber 3 has two openings. An inlet opening 7 is located to the side of the electrode 5.
  • the outlet opening of the gas discharge chamber 3 is arranged opposite the electrode 5 and leads into the ionization chamber 1 as an inlet opening 9.
  • the inlet opening 9 leading into the ionization chamber 1 from the gas discharge chamber is located in a narrow end wall of the elongate ionization chamber 1. At the same end, another inlet opening 11 leads laterally into the ionization chamber 1. At the head end of the ionization chamber 1 opposite the inlet opening 9 there is one Outlet opening 13 of the ionization chamber 1.
  • a cylindrical magnet coil 15 is arranged around the cylindrical ionization chamber 1 and generates an axial magnetic field in the ionization chamber 1.
  • a focusing and acceleration system 17 in the form of electrical lenses provided with pinholes.
  • FIGS. 2 and 3 has a similar structure to the embodiment of the ionization chamber 1 of FIG. 1; only the ionization chamber 1 is located in a quadrupole tube 22, which is formed by a cylindrical tube with tube recesses 24 on which metal electrodes 26, for example in the form of thin foils, are applied.
  • Primary gas flows into the gas discharge chamber 3 through the inlet opening 7 of the gas discharge chamber 3 and is at least partially ionized there by the electrode 5.
  • the partially ionized primary gas flows through the axial opening 9 from the gas discharge chamber 3 into the longitudinally extending ionization chamber 1.
  • a mixture of reactant and substance gas enters through the inlet opening 11.
  • the reactant gas is then ionized by the primary particles in a primary ionization and in turn ionizes the substance gas.
  • the magnet 15 creates an axial magnetic field in the ionization chamber 1, whereby the ionized particles are held together.
  • reaction products finally exit the ionization chamber through the outlet opening 13 and are directed and accelerated by the focusing and acceleration system 17 onto the inlet opening 19 of the mass spectrometer.

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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)

Claims (8)

1. Source d'ions comportant une chambre d'ionisation pour l'ionisation chimique de vapeurs de substances par réaction ions- molécules en utilisant des particules primaires ionisantes et un gaz réacteur, comportant des orifices d'entrée pour les particules primaires ionisantes, le gaz réacteur et le gaz de la substance et un orifice de sortie des produits de la réaction formés dans la chambre, l'orifice d'entrée des particules primaires ionisantes étant à l'opposé de l'orifice de sortie, caractérisée par le fait que la chambre d'ionisation (1) est cylindrique et allongée, l'orifice d'entrée (9) des particules primaires ionisantes et l'orifice de sortie (13) des produits de la réaction sont situés sur l'axe longitudinal de la chambre d'ionisation (1) et pratiqués dans les parois d'extrémité opposées de celle-ci, et il est prévu près de l'orifice d'entrée (9) des particules primaires ionisantes un orifice d'entrée séparé (11) pour le gaz réacteur et/ôu la vapeur de la substance.
2. Chambre d'ionisation selon la revendication 1, dans laquelle, le long d'elle, règne un champ magnétique longitudinal.
3. Chambre d'ionisation selon la revendication 2, dans laquelle, à l'intérieur de cette chambre (1) se trouve un multipôle électrique constitué d'au moins quatre baguettes polaires allongées, isolées et placées symétriquement par rapport à l'axe, baguettes auxquelles sont appliquées des tensions alternatives symétriques ou asymétriques par rapport à l'axe de la chambre.
4. Chambre d'ionisation selon la revendication 2, dont la paroi est formée d'un tube multipolaire (22) et sur cette paroi (24) se trouvent des électrodes conductrices (26) auxquelles sont appliquées des tensions alternatives haute fréquence symétriques ou asymétriques par paires suivant la circonférence.
5. Chambre d'ionisation selon l'une des revendications 3 ou 4, dans laquelle les baguettes ou les surfaces polaires des électrodes (26) sont parallèles a son axe de symétrie.
6. Chambre d'ionisation selon l'une des revendications 3 ou 4, dans laquelle les baguettes ou les surfaces polaires des électrodes (26) sont inclinées sur son axe de symétrie.
7. Chambre d'ionisation selon l'une des revendications 1 à 6, dans laquelle une chute de potentiel est prévue le long de son axe longitudinal.
8. Chambre d'ionisations selon l'une des revendications 1 à 7, dans laquelle est prévu un système de diaphragme (17) adjoint à son orifice de sortie (13) et produisant un champ électrostatique de lentille y pénétrant symétriquement par rapport à son axe longitudinal.
EP78100259A 1977-08-23 1978-06-28 Source d'ions comportant une chambre d'ionisation pour l'ionisation chimique Expired EP0000865B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2737852A DE2737852C2 (de) 1977-08-23 1977-08-23 Ionenquellen zur chemischen Ionisierung
DE2737852 1977-08-23

Publications (2)

Publication Number Publication Date
EP0000865A1 EP0000865A1 (fr) 1979-03-07
EP0000865B1 true EP0000865B1 (fr) 1981-08-19

Family

ID=6017032

Family Applications (1)

Application Number Title Priority Date Filing Date
EP78100259A Expired EP0000865B1 (fr) 1977-08-23 1978-06-28 Source d'ions comportant une chambre d'ionisation pour l'ionisation chimique

Country Status (3)

Country Link
US (1) US4220545A (fr)
EP (1) EP0000865B1 (fr)
DE (1) DE2737852C2 (fr)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3134337A1 (de) * 1981-08-31 1983-03-24 Technics GmbH Europa, 8011 Kirchheim Ionenstrahlkanone
US4542293A (en) * 1983-04-20 1985-09-17 Yale University Process and apparatus for changing the energy of charged particles contained in a gaseous medium
US5003178A (en) * 1988-11-14 1991-03-26 Electron Vision Corporation Large-area uniform electron source
US5300266A (en) * 1992-05-27 1994-04-05 Scientific Products Corporation Electrical apparatus and method for generating antibiotic
AT406206B (de) * 1997-04-15 2000-03-27 Lindinger Werner Dr Gewinnung von nh4+-ionen
US5889404A (en) * 1997-08-29 1999-03-30 Hewlett-Packard Company Discharge ionization detector having efficient transfer of metastables for ionization of sample molecules
WO2004079765A2 (fr) * 2003-03-03 2004-09-16 Brigham Young University Nouvelle source d'ionisation electronique pour spectrometrie de masse par temps de vol a acceleration orthogonale
AT413463B (de) 2003-12-16 2006-03-15 Hansel Armin Dr Verfahren zur gewinnung eines ausgangs-ionenstroms
US8362421B2 (en) * 2008-04-02 2013-01-29 Sociedad Europea de Analisis Diferencial de Movilidad Use ion guides with electrodes of small dimensions to concentrate small charged species in a gas at relatively high pressure
US20110260048A1 (en) * 2010-04-22 2011-10-27 Wouters Eloy R Ion Transfer Tube for a Mass Spectrometer Having a Resistive Tube Member and a Conductive Tube Member

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3371205A (en) * 1964-11-17 1968-02-27 Cons Electrodynamics Corp Multipole mass filter with a pulsed ionizing electron beam
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
US3665245A (en) * 1969-10-27 1972-05-23 Research Corp Quadrupole ionization gauge
US3984692A (en) * 1972-01-04 1976-10-05 Arsenault Guy P Ionization apparatus and method for mass spectrometry
GB1550853A (en) * 1975-10-06 1979-08-22 Hitachi Ltd Apparatus and process for plasma treatment
DE2701395C3 (de) * 1977-01-14 1979-12-06 Dr. Franzen Analysentechnik Gmbh & Co Kg, 2800 Bremen Ionenquelle für die chemische Ionisierung von Atomen und Molekülen

Also Published As

Publication number Publication date
DE2737852C2 (de) 1982-04-22
DE2737852A1 (de) 1979-03-08
EP0000865A1 (fr) 1979-03-07
US4220545A (en) 1980-09-02

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