EP0310888B1 - Verfahren zum Einbringen von Ionen in die Ionenfalle eines Ionen-Zyklotron-Resonanz-Spektrometers und zur Durchführung des Verfahrens ausgebildetes Ionen-Zyklotron-Resonanz-Spektrometer - Google Patents

Verfahren zum Einbringen von Ionen in die Ionenfalle eines Ionen-Zyklotron-Resonanz-Spektrometers und zur Durchführung des Verfahrens ausgebildetes Ionen-Zyklotron-Resonanz-Spektrometer Download PDF

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Publication number
EP0310888B1
EP0310888B1 EP88115676A EP88115676A EP0310888B1 EP 0310888 B1 EP0310888 B1 EP 0310888B1 EP 88115676 A EP88115676 A EP 88115676A EP 88115676 A EP88115676 A EP 88115676A EP 0310888 B1 EP0310888 B1 EP 0310888B1
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EP
European Patent Office
Prior art keywords
ion
ion trap
ions
magnetic field
wall
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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
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EP88115676A
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German (de)
English (en)
French (fr)
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EP0310888A2 (de
EP0310888A3 (en
Inventor
Pablo Dr. Caravatti
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Spectrospin AG
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Spectrospin AG
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/34—Dynamic spectrometers
    • H01J49/36—Radio frequency spectrometers, e.g. Bennett-type spectrometers, Redhead-type spectrometers
    • H01J49/38—Omegatrons ; using ion cyclotron resonance

Definitions

  • the invention relates to a method for introducing ions into the ion trap of an ion cyclotron resonance spectrometer, which is arranged in a constant, homogeneous magnetic field and designed as electrodes, parallel or perpendicular to an axis of symmetry of the ion trap coinciding with the direction of the magnetic field has arranged walls against which the ion trapping electrical trapping potentials are present and of which one of the walls perpendicular to the magnetic field has a hole, in which method the ions are generated outside the ion trap, an ion beam is formed from the ions and the ion beam is parallel to the axis of symmetry of the ion trap on the one wall of the ion trap arranged hole is directed and then the speed, which the ions penetrating through the hole into the ion trap have in the direction of the magnetic field, is reduced below the value determined by trapping potentials, which the ions must have to leave the ion trap.
  • Such a method is known from EP-A-0 200 027.
  • the known method has two variants. According to one, the gas pressure in the ion trap is temporarily increased in order to reduce the speed of the ions which have penetrated into the ion trap, in order to thereby slow down the ions.
  • This variant requires pumping off gas after the ions have been injected, which not only increases the duration of the process, but can also lead to ion loss and fragmentation of the ions.
  • the speed of the ions is reduced by a brake electrode connected upstream of the ion trap, and at the same time the capture potentials are released so that the ions can penetrate the ion trap despite their reduced speed.
  • the trapping potentials are then switched on again, so that the ions which have entered the ion trap are trapped therein. Even in this way, however, the maximum possible ion concentration in the ion trap cannot be achieved, as is to be aimed for, in order to achieve the greatest possible sensitivity when recording the ion cyclotron resonance spectrum.
  • the object of the invention is to provide a method for reducing the velocity of the ions which have penetrated into the ion trap in the direction of the magnetic field, which method can be carried out in a simple manner and results in an increased density of the trapped ions.
  • This object is achieved according to the invention in that the ions which have penetrated into the ion trap are given a movement component directed perpendicular to the magnetic field.
  • the speed of the ions in the direction of the magnetic field which enables the ions to leave the ion trap, is not reduced by increasing the gas pressure or by means of a brake electrode, but by deflecting the ions from their original ones running in the direction of the magnetic field Orbit, so that the ions move on a path after entering the ion trap, which leads to an increase in the mean length of stay of the ions in the ion trap.
  • the ions are introduced into the ion trap with a lateral offset to the axis of symmetry of the ion trap parallel to the magnetic field. All that is required is to arrange the ion beam and ion trap laterally offset from one another.
  • the lateral offset when the ions enter the ion trap, they reach a region in which the electrical field prevailing in the ion trap as a result of the potentials present on the walls of the ion trap has a transverse component through which the ions are deflected laterally.
  • the ions are forced to perform a cyclotron movement on orbits, which result in the desired extension of the length of stay of the ions in the ion trap.
  • an electrical field directed transversely to the direction of the magnetic field is generated during the duration of the ion beam, preferably in the immediate vicinity of the wall of the ion trap provided with the hole.
  • Such a field can be generated in a simple manner by means of additional electrodes arranged in the ion trap. Neither the size of this field nor its duration is critical. The field only has to be switched off before the actual spectra recording begins.
  • the invention also relates to an ion cyclotron resonance spectrometer which is designed to carry out the method according to the invention. It comprises, in a known manner, an ion trap which is arranged in a constant, homogeneous magnetic field and which is designed as electrodes and has walls which are arranged parallel or perpendicular to an axis of symmetry of the ion trap coinciding with the direction of the magnetic field and on which the ions holding electrical ions in the ion trap Capture potentials are present and one of the walls perpendicular to the magnetic field has a hole.
  • the spectrometer comprises a device for introducing ions into the ion trap, with an ion source, means for generating an ion beam which emanates from the ion source and is directed parallel to the axis of symmetry of the ion trap and which is directed onto the hole arranged in one wall of the ion trap, and Means for reducing the speed of the ions which have penetrated through the hole into the ion trap in the direction of the magnetic field to a value below the value determined by the trapping potential which the ions must have to leave the ion trap.
  • the means for reducing the speed of the ions in the direction of the magnetic field are designed to generate a static electrical field component perpendicular to the axis of symmetry of the ion trap and thereby to impart a movement component directed perpendicular to the magnetic field to the ions which have penetrated into the ion trap.
  • the hole arranged in one wall of the ion trap is laterally offset from the axis of symmetry of the ion trap parallel to the magnetic field.
  • electrodes insulated from the wall are attached on both sides of the hole arranged in one wall of the ion trap and connected to a voltage source which can be switched on in a pulsed manner. It goes without saying that such electrodes can also be used if the hole arranged in one wall in the ion trap is arranged off-center.
  • the potential of the wall, that of the hole provided wall is opposite, in the sense of the ion charge from the potential of the wall provided with the hole.
  • the ion cyclotron resonance spectrometer shown schematically in FIG. 1 has an ion source 1 in the form of a chamber, to which an electron gun 2 is assigned, with which an electron beam 3 indicated by a dashed line can be injected into the chamber 1 to ionize the gas contained therein.
  • a wall 4 of the ion source 1 is provided with a small hole 5 from which the ions can emerge from the ion source 1.
  • a flying tube 6, which is arranged coaxially to the hole 5 in the wall 4 of the ion source 1 and, if working with positive ions, is kept at a relatively high potential of -1 kV to -3 kV during operation becomes.
  • an ion trap 10 is arranged which has two walls 11, 12 perpendicular to the direction of the ion beam 9 and four walls parallel thereto, of which only two walls 13, 14 perpendicular to the plane of the drawing are shown in the drawing, while the two other walls are arranged parallel to the plane of the drawing.
  • a hole 15 is provided in the wall 11 of the ion trap adjacent to the flight tube 6 in the wall 11 of the ion trap adjacent to the flight tube 6 in the wall 11 of the ion trap adjacent to the flight tube 6 there is a hole 15 to which the ion beam 9 is aligned.
  • the ion beam 9 is directed parallel to the axis 16 of the ion trap, but laterally offset with respect to this axis.
  • a brake electrode 17 Between the end of the flight tube 6 and the ion trap 10 there is a brake electrode 17, by means of which the ions are first braked to a potential suitable for entry into the ion trap.
  • Typical operating potentials for the walls of the ion trap are 0 V for the wall 11 adjacent to the flight tube 6, +0.5 V for the wall 12 parallel thereto, -1 V for the walls parallel to the ion beam, of which only the walls 13, 14 are shown and -0.5 V for the brake electrode. These values in turn apply to the investigation of positive ions. When examining negative ions, potentials with the opposite signs are used used.
  • the ion trap is in operation in a constant, homogeneous magnetic field B, which is directed parallel to the direction of the ion beam 9 and the axis 16 of the ion trap 10 and is indicated in the drawing by arrows.
  • the pulse of the ions supplied in the form of the ion beam 9 to the ion trap 10 is greatly reduced, but the pulse must still be large enough to the potential of the flight tube 6 adjacent To be able to overcome wall 11 of the ion trap.
  • This pulse is generally sufficient to also allow the ions to reach the other wall 12 perpendicular to the direction of the ion beam and magnetic field B, either by hitting this wall or by leaving the ion trap through a hole 18 that extends concentric to the axis 16 of the ion trap 10 in the wall 12, to be lost if the ion beam along the axis 16 of the ion trap would enter it.
  • the ion beam 9 is offset from the axis 16 of the ion trap 10, so that it enters a region of the ion trap 10 in which the electrostatic field located within the ion trap 10, which due to the the wall applied potentials within the ion trap, has components oriented transversely to the axis 16, with the result that the ions are deflected from their rectilinear path as a result of the prevailing magnetic field and the electrostatic field upon entry into the ion trap 10 and thereby their impulse component in the direction the cell axis 16 is reduced to below the value that they need to leave the cell immediately.
  • the duration of the ion beam which is necessary to achieve a high ion density in the ion trap, corresponds to the achievable residence time of the ions and is in the range between 10 and 500 ms and depends, among other things, on the size of the ion current.
  • an ion cyclotron resonance spectrometer shown in FIG. 2 in turn has an ion source 101 in the form of a gas-filled cell, into which an ionizing beam 103 can be injected by means of an electron gun 102 or a laser.
  • the ions generated in this way can leave the ion source 101 through a hole 105 provided in a wall 104.
  • an ion beam 109 is in turn formed by means of a flight tube 106, which can emerge from the flight tube through the hole 108 of an aperture 107, which is located at the end of the flight tube facing away from the ion source 101.
  • the ion beam 109 is directed onto an ion trap 110 which, like in the embodiment according to FIG. 1, has walls 111 and 112 which are perpendicular to the ion beam 109 and walls 113, 114 which are parallel thereto.
  • two electrodes 121, 122 are mounted diametrically to one another, which have angled sections 123, 124, which protrude into the hole 115 in the wall 111 and are aligned there with the wall 111.
  • the electrodes 121, 122 are fastened to the wall 111 in a manner not shown by means of insulating pieces 125, 126 and at the same time serve as a carrier for the brake electrode 117, which in a similar way by means of Insulating pieces 127, 128 is attached to the electrodes.
  • the insulating pieces 125, 126 and also 127, 128 can be part of plate-shaped, in particular circular, insulating and supporting bodies or can simply be formed by insulating rings which surround screws which are used to fasten the electrodes and are screwed into wall 111.
  • the arrangement shown has the particular advantage that it enables the electrodes to be displaceably attached to the plate 111 for adjustment purposes.
  • a voltage in the range of approximately 2 to 10 V is applied to the electrodes 121, 122 by means of a voltage source 130 that can be switched on in a pulsed manner for the duration of the ion beam.
  • This voltage is preferably symmetrical to the potential that is present at the wall 111 carrying the electrodes 121, 122, but there is no imperative for this. Rather, a certain asymmetry of the voltages can be advantageous, in particular depending on the point of passage of the ion beam between the electrodes.
  • the ion trap 110 is in turn in a constant, homogeneous magnetic field B, which is directed parallel to the axis of the ion trap 116, as illustrated by the arrows in the drawing.
  • a potential of -1 V is constantly present on the walls 113, 114 parallel to the cell axis 116, while a constant potential of 0 V is present on the wall 111 perpendicular to the magnetic field, as illustrated by line (a) in FIG. 3.
  • a so-called quench pulse is applied to the wall 112 perpendicular to the magnetic field, which faces away from the flight tube 106, the voltage of which can be, for example, -9 V, in order to thereby drive out all ions contained in the ion trap 110 which the ion trap through the central hole 118 leave in the wall 112 or strike the walls of the cell and are thereby neutralized.
  • This quench pulse 131 is illustrated in line (b) of FIG. 3. Then this wall 112 is kept at a potential of approximately +0.5 V.
  • a voltage is applied to electrodes 121 and 122, so that one electrode 121 is at a potential of +2 V and the other electrode 122 is at a potential of -2 V with respect to the adjacent wall 111, as illustrated by the pulse-like voltage change 132 or 133 in lines (c) and (d) in FIG. 3.
  • a voltage of -0.5 V is applied to the brake electrode 117, as section 134 in line (e) of FIG. 3 illustrates, and the ion source is then also switched on, so that it generates an ion current 135, the Occurrence in line (f) in Fig. 3 is illustrated.
  • a local electric field is generated which is directed perpendicular to the direction of the magnetic field B.
  • the ions entering the ion trap between the electrodes 121, 122 are forced to move radially in the direction of the lower electrical potential.
  • the effect of the electric field is spatially limited and affects the cell potential only to a considerable extent in the vicinity of the inlet opening 115.
  • the ions leave this area with a deflection obtained perpendicular to the direction of the magnetic field directed pulse component and correspondingly reduced speed in the direction of the cell axis 116.
  • the ions return to the area of influence of the potential prevailing between the electrodes 121, 122, but with a reduced axial pulse component which is no longer sufficient to enable the ions to leave the ion trap 110, especially since the ions are again deflected transversely. Therefore, a high proportion of the ions supplied by the ion current 135 are trapped in the ion trap 110 and an accumulation of the ions takes place during the duration of the ion current, which leads to a very high ion density.
  • RF pulses 136, 137 can then be radiated into the ion trap in a conventional manner, as indicated in line (g) of FIG. 3, in order to excite the ions into cyclotron resonance vibrations which following pulse 137 at time t7 can be detected in the usual way.
  • the first RF pulse 136 can serve to remove undesired ion types from the ion trap.
  • the ion cyclotron resonance spectrometer according to the invention apart from the modifications described, has a customary structure and can also be operated with the usual operating parameters.
  • the potentials that lead to the best results in individual cases can easily be determined experimentally.
  • the above values are therefore only mentioned for example and can be adjusted depending on the special design of the spectrometer, in particular of its ion trap and the types of ions to be investigated can be easily optimized by appropriate tests.
  • the increase in ion density that can be achieved when using the method according to the invention cannot be stated in a general way, because it i.a. depends on the intensity of the ion current.
  • the method according to the invention is particularly advantageous when the ion current is low and a good ion density can only be achieved by accumulation.
  • the detection sensitivity can be improved by about two orders of magnitude by the accumulation of the ions.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Sources, Ion Sources (AREA)
  • Electron Tubes For Measurement (AREA)
EP88115676A 1987-10-07 1988-09-23 Verfahren zum Einbringen von Ionen in die Ionenfalle eines Ionen-Zyklotron-Resonanz-Spektrometers und zur Durchführung des Verfahrens ausgebildetes Ionen-Zyklotron-Resonanz-Spektrometer Expired - Lifetime EP0310888B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19873733853 DE3733853A1 (de) 1987-10-07 1987-10-07 Verfahren zum einbringen von ionen in die ionenfalle eines ionen-zyklotron-resonanz-spektrometers und zur durchfuehrung des verfahrens ausgebildetes ionen-zyklotron-resonanz-spektrometers
DE3733853 1987-10-07

Publications (3)

Publication Number Publication Date
EP0310888A2 EP0310888A2 (de) 1989-04-12
EP0310888A3 EP0310888A3 (en) 1989-12-27
EP0310888B1 true EP0310888B1 (de) 1993-11-18

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EP88115676A Expired - Lifetime EP0310888B1 (de) 1987-10-07 1988-09-23 Verfahren zum Einbringen von Ionen in die Ionenfalle eines Ionen-Zyklotron-Resonanz-Spektrometers und zur Durchführung des Verfahrens ausgebildetes Ionen-Zyklotron-Resonanz-Spektrometer

Country Status (4)

Country Link
US (1) US4924089A (enrdf_load_stackoverflow)
EP (1) EP0310888B1 (enrdf_load_stackoverflow)
JP (1) JPH01163954A (enrdf_load_stackoverflow)
DE (1) DE3733853A1 (enrdf_load_stackoverflow)

Families Citing this family (17)

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US5248883A (en) * 1991-05-30 1993-09-28 International Business Machines Corporation Ion traps of mono- or multi-planar geometry and planar ion trap devices
US5207379A (en) * 1991-06-11 1993-05-04 Landis & Gyr Powers, Inc. Cascaded control apparatus for controlling unit ventilators
US5696376A (en) * 1996-05-20 1997-12-09 The Johns Hopkins University Method and apparatus for isolating ions in an ion trap with increased resolving power
US5650617A (en) * 1996-07-30 1997-07-22 Varian Associates, Inc. Method for trapping ions into ion traps and ion trap mass spectrometer system thereof
DE19930894B4 (de) * 1999-07-05 2007-02-08 Bruker Daltonik Gmbh Verfahren zur Regelung der Ionenzahl in Ionenzyklotronresonanz-Massenspektrometern
US6573495B2 (en) 2000-12-26 2003-06-03 Thermo Finnigan Llc High capacity ion cyclotron resonance cell
US6784421B2 (en) 2001-06-14 2004-08-31 Bruker Daltonics, Inc. Method and apparatus for fourier transform mass spectrometry (FTMS) in a linear multipole ion trap
US6888133B2 (en) * 2002-01-30 2005-05-03 Varian, Inc. Integrated ion focusing and gating optics for ion trap mass spectrometer
DE10213652B4 (de) * 2002-03-27 2008-02-21 Bruker Daltonik Gmbh Verfahren zur Bestrahlung von Ionen in einer Ionenzyklotronresonanz-Falle mit Elektronen und/oder Photonen
DE10325582B4 (de) 2003-06-05 2009-01-15 Bruker Daltonik Gmbh Ionenfragmentierung durch Elektroneneinfang in Hochfrequenz-Ionenfallen mit magnetischer Führung der Elektronen
US7777182B2 (en) * 2007-08-02 2010-08-17 Battelle Energy Alliance, Llc Method and apparatus for ion cyclotron spectrometry
US8334506B2 (en) 2007-12-10 2012-12-18 1St Detect Corporation End cap voltage control of ion traps
US7763849B1 (en) * 2008-05-01 2010-07-27 Bruker Daltonics, Inc. Reflecting ion cyclotron resonance cell
US7973277B2 (en) 2008-05-27 2011-07-05 1St Detect Corporation Driving a mass spectrometer ion trap or mass filter
TWI379330B (en) * 2009-11-18 2012-12-11 Delta Electronics Inc Transformer
US8575542B1 (en) 2012-04-18 2013-11-05 Bruker Daltonics, Inc. Method and device for gas-phase ion fragmentation
EP2858090B1 (en) 2013-10-02 2016-06-22 Bruker Daltonik GmbH Introduction of ions into ion cyclotron resonance cells

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US3922543A (en) * 1972-10-17 1975-11-25 Jesse L Beauchamp Ion cyclotron resonance spectrometer and method
US3984681A (en) * 1974-08-27 1976-10-05 Nasa Ion and electron detector for use in an ICR spectrometer
JPS594444Y2 (ja) * 1982-01-18 1984-02-08 株式会社エイコ−エンジニアリング イオンサイクロトロン共鳴質量分析装置にくける試料供給装置
US4481415A (en) * 1982-10-27 1984-11-06 Shimadzu Corporation Quadrupole mass spectrometer
DE3331136A1 (de) * 1983-08-30 1985-03-07 Spectrospin AG, Fällanden, Zürich Verfahren zur aufnahme von ionen-zyklotron-resonanz-spektren und vorrichtung zur durchfuehrung des verfahrens
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DE3515766A1 (de) * 1985-05-02 1986-11-06 Spectrospin AG, Fällanden, Zürich Ionen-zyklotron-resonanz-spektrometer
DE3538407A1 (de) * 1985-10-29 1987-04-30 Spectrospin Ag Ionen-zyklotron-resonanz-spektrometer
US4739165A (en) * 1986-02-27 1988-04-19 Nicolet Instrument Corporation Mass spectrometer with remote ion source
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DE3627605A1 (de) * 1986-08-14 1988-02-25 Spectrospin Ag Verfahren zum eliminieren unerwuenschter geladener teilchen aus der messzelle eines icr-spektrometers

Also Published As

Publication number Publication date
EP0310888A2 (de) 1989-04-12
DE3733853C2 (enrdf_load_stackoverflow) 1991-03-28
JPH01163954A (ja) 1989-06-28
EP0310888A3 (en) 1989-12-27
DE3733853A1 (de) 1989-04-27
US4924089A (en) 1990-05-08
JPH0459747B2 (enrdf_load_stackoverflow) 1992-09-24

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