EP0459602A2 - Cage quadrupolaire haute fréquence pour spectrométrie de masse avec champs multipolaires superposés - Google Patents

Cage quadrupolaire haute fréquence pour spectrométrie de masse avec champs multipolaires superposés Download PDF

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Publication number
EP0459602A2
EP0459602A2 EP91250128A EP91250128A EP0459602A2 EP 0459602 A2 EP0459602 A2 EP 0459602A2 EP 91250128 A EP91250128 A EP 91250128A EP 91250128 A EP91250128 A EP 91250128A EP 0459602 A2 EP0459602 A2 EP 0459602A2
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EP
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Prior art keywords
ion
field
octupole
electrodes
cage
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EP91250128A
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German (de)
English (en)
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EP0459602A3 (en
EP0459602B1 (fr
EP0459602B2 (fr
Inventor
Jochen Dr. Franzen
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Bruker Daltonics GmbH and Co KG
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Bruken Franzen Analytik GmbH
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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
    • H01J49/42—Stability-of-path spectrometers, e.g. monopole, quadrupole, multipole, farvitrons
    • H01J49/4205—Device types
    • H01J49/424—Three-dimensional ion traps, i.e. comprising end-cap and ring electrodes

Definitions

  • the invention relates to an ion cage mass spectrometer, a quistor, an ion trap or the like according to the preamble of patent claims 1 and 6.
  • a mass spectrometer is known in which the electrodes are arranged so that the surfaces of the ring electrode and the end cap electrodes form a one-piece rotary hyperboloid or a two-part rotary hyperboloid, the end cap electrodes being conductively connected to one another and between the ring electrode and a time-varying voltage is applied to the end cap electrodes. If a potential U + V ⁇ sin ( ⁇ t) is generated between the ring electrode and the end cap electrodes, ions remain, their specific charge e / m is in a certain range between the electrodes, while the others hit the electrodes.
  • the superimposition of direct and high-frequency fields in such mass spectrometers is called a quadrupole memory field.
  • the ion movement forms a good approximation of a spatial overlay of two independent harmonic oscillators.
  • the force integrated over half of the so-called secular period approximately fulfills the condition of a harmonic oscillator, so that such a system is also called a pseudo-harmonic oscillator.
  • Two such pseudoharmonic oscillator systems form the aforementioned ion cage, which is also referred to as a quistor or ion trap (for terminology: Dawson, “Quadrupole Mass Spectrometry", Elsevier, Amsterdam, 1976; Mahrs / Hughes “Quadrupole Storage Mass Spectrometry", John Wiley & Sons, New York, 1989).
  • the two pseudoharmonic oscillator systems of the quistor consist of a cylinder-symmetrical system, which shows the same behavior regardless of the coordinate in the direction of the cylinder axis (z-axis), and a plane system, the behavior of which is independent of the distance r from the cylinder axis.
  • the ions vibrate with so-called "secular frequencies", which are completely independent of one another.
  • the secular frequencies can be determined using known formulas. Since the secular frequencies in the r and z directions and the storage frequency only have a common divisor in rare situations, the movement patterns of the ions are usually very complicated.
  • An ion cage can be used as a mass spectrometer.
  • the well-known basic principle of mass spectrometry consists in the proportions of ions with different masses relative to one another ascertain.
  • so-called scan methods are used, which carry out the measurement of the different types of ions one after the other by varying measurement or filter conditions.
  • Various scanning methods are known for the ion cage.
  • the ions of successive masses are ejected sequentially in time from the cage and fed to a detection system, so that the measurement signals of the ions can be processed to a mass spectrum in a known manner.
  • mass-selective ejection can be carried out in three different ways.
  • the ions can be ejected by changing the storage conditions in the ion cage such that the ions move mass by mass beyond the edge of the stability range, become unstable, and leave the ion cage ("Mass-selective instability scan", US Pat. No. 4,440 884).
  • the secular frequency of successive ion masses can be excited by an externally applied high-frequency voltage in such a way that they absorb kinetic energy in resonance and thus leave the cage (“mass-selective resonance scan by excitation frequency", US Pat. No. 4,736,101).
  • the ions can be introduced into a device-specific nonlinear resonance condition in which they absorb kinetic energy and leave the cage (“mass-selective scan by means of nonlinear device resonance”, US Pat. No. 4,882,484).
  • the known quadrupole cage can not only be used to identify individually supplied substances based on their primary spectra, but can also be used to identify mixture components by tandem mass spectrometry, whereby daughter ion spectra are generated.
  • an ion type the parent ion
  • the parent ion is selected; all other types of ions are removed from the cage.
  • the parent ion is fragmented by collision with a gas introduced into the cage. To do this, the parent ion must be accelerated to increase the collision energy above the fragmentation threshold. It is easiest to excite ion oscillation in the z direction by an alternating voltage between the end cap electrodes which is in resonance with the corresponding secular frequency.
  • the excitation is critical in the known quadrupole cages.
  • the amplitude of the secular motion increases linearly with time, and eventually the ions will collide with the end cap electrodes.
  • Fine tuning is required between a low excitation voltage and a high collision gas density, and a yield of about 30 to 50% of daughter ions can be achieved; the rest of the parent ions are lost.
  • the invention is therefore based on the object of developing the generic mass spectrometer in such a way that in order to increase the ability and the detection power while further - resolving - accelerating the measurement of the mass spectrum a general rule for the appropriate type of multi-field overlay is given, the ion losses from the spectrometer being reduced by unwanted resonances in use for tandem mass spectrometry and the yield should be increased in the case of shock-induced fragmentation.
  • the invention is based on the surprising finding that it is possible to sharpen the temporal smearing of the ejection process in a multipole superposition according to the invention, be it in a mathematically exact description or according to the approximate formula of claim 6, thereby accelerating the creation of the mass spectrum. Furthermore, ion losses are reduced and the yield of daughter ions is improved. The superposition of z-asymmetrical multipole fields intensifies the ejection by the non-linear resonance effects that then occur.
  • the surface shape of the electrodes is chosen in the invention so that the effect of the desired multipole field overlay results.
  • the exact dimensions of the electrodes are determined by the relative strength A3 of the sextupole field or the relative strength A4 of the octupole field in relation to the strength A2 of the quadrupole field.
  • the strengths of the sextupole field or the octupole field with respect to the quadrupole field can be between approximately 0% and 20%, it being particularly advantageous if the proportion of the superimposed fields is between 0.5% and 4.5%; the proportion is particularly preferably between 1% and 3%.
  • the electrodes can easily be shaped in such a way that mathematically exact superimpositions of the quadrupole field with predetermined contributions of the octupole field or the sextupole field are obtained.
  • the deviations due to the superimposed fields are mainly noticeable in the outer areas of the spectrometer area, while an almost exact quadrupole field is present in the area of the center.
  • the manufacture of electrodes according to the regulation of the invention in one embodiment, as is the subject of claim 6, is carried out by successively adding higher-order thermal springs in w, once the measure p 1 for the proportion of the octupole field, the measure p2 are specified for the portion of the sextupole field or the correction portion p3 of the octupole field. It is again advantageous if p1, p2 and p3 are between 0% and 20%, these variables should not, however, take the value 0 at the same time, so that in any case a superimposed heat contributes.
  • Figure 1 shows the arrangement of two end cap electrodes 1, 2, which are each arranged at a distance z0 from the equatorial plane 4.
  • a ring electrode 3 such that the entire arrangement of the electrodes 1, 2, 3 is axially symmetrical, the axis of symmetry coinciding with the z axis of the coordinate system.
  • the octupole field generated by the electrode shape has a strength A4 / A2 of 2%, measured in the equatorial plane 4 at the ring electrode 3.
  • the overlaid field causes non-linear forces both in the z direction and as a function of r, the distance from the z -Axis generated.
  • the secular frequencies become dependent on the secular amplitudes and either increase or at.
  • a resonance catastrophe of the secular amplitude is prevented.
  • the increasing secular oscillation shifts in frequency and phase through the octupole field and reaches a maximum amplitude when the phase shift is 90 °, after which the amplitude decreases again. Therefore, like all other "even" multipole fields, the octupole field has a surprisingly positive effect. Almost all ion losses due to resonance effects are prevented, whatever the cause of the resonance.
  • the excitation voltage can be selected such that the parent ions never reach the end cap electrodes 1, 2. Yields of daughter ions in the order of 80 to 100% of the parent ions are possible.
  • An octupole field that normally blocks the resonance reactions of ions can still have positive effects on the resonance reaction during a scan.
  • the secular frequency reaches the external excitation frequency, due to the coupling of the secular frequency and the secular amplitude, the effects of the increase in the sampling frequency and the decrease in the amplitude are compensated, whereby the ion is expelled from the mass spectrometer.
  • FIG. 2 shows an electrode arrangement comprising end cap electrodes 1, 2 and ring electrode 3, in which the electrodes are shaped in such a way that a sextupole field is superimposed on the base quadrupole field.
  • the dotted lines 5, 6 indicate the corresponding electrode structure in which a pure quadrupole field would be present. It can be seen that deviations only occur in the outer regions of the electrode arrangement, while an almost exact quadrupole field results in the interior.
  • the secular frequency remains essentially unchanged in the z direction, while frequency splitting takes place in the r direction.
  • the sextupole field produces a strong nonlinear resonance at a frequency that is exactly one third of the storage frequency. If an excitation voltage is now applied in phase and at this frequency, the ion oscillation is first increased by this excitation voltage, which leads to a linear increase in the secular amplitude, then the oscillation will increase exponentially through the sextupole resonance.
  • the hexapole resonance can therefore be used for mass-selective ejection of the ion. The ejection process is therefore exacerbated by overlaying the sextupole field. Good results are achieved when the proportion A3 of the overlying sextupole field is 2% of the quadrupole field.
  • FIG. 3 shows an electrode arrangement in which both a superimposed octupole field and a superimposed one Sextupol field have been generated, the octupole portion is 2% and the sextupole portion is 6%.
  • the combination of the two superimposed fields has the result that the advantages of both systems are realized in the arrangement.
  • the loss of ions is reduced by the octupole effect, the non-linear resonance of the sextupole field promotes the ejection of the ions and sharpens the ejection process. It has been found that the best results are achieved if the proportion A3 of the overlaid sextupole field is twice as large as the proportion A4 of the overlaid octupole field.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Electron Tubes For Measurement (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
EP91250128A 1990-05-29 1991-05-08 Cage quadrupolaire haute fréquence pour spectrométrie de masse avec champs multipolaires superposés Expired - Lifetime EP0459602B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4017264 1990-05-29
DE4017264A DE4017264A1 (de) 1990-05-29 1990-05-29 Massenspektrometrischer hochfrequenz-quadrupol-kaefig mit ueberlagerten multipolfeldern

Publications (4)

Publication Number Publication Date
EP0459602A2 true EP0459602A2 (fr) 1991-12-04
EP0459602A3 EP0459602A3 (en) 1992-07-01
EP0459602B1 EP0459602B1 (fr) 1996-03-13
EP0459602B2 EP0459602B2 (fr) 2000-02-09

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EP91250128A Expired - Lifetime EP0459602B2 (fr) 1990-05-29 1991-05-08 Cage quadrupolaire haute fréquence pour spectrométrie de masse avec champs multipolaires superposés

Country Status (3)

Country Link
US (1) US5170054A (fr)
EP (1) EP0459602B2 (fr)
DE (2) DE4017264A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2267385A (en) * 1992-05-29 1993-12-01 Finnigan Corp Ion trap mass spectrometer method
EP0608885A1 (fr) * 1993-01-27 1994-08-03 Varian Associates, Inc. Spectromètre de masse du type piège ionique
GB2261988B (en) * 1991-11-27 1995-05-10 Bruker Franzen Analytik Gmbh A method of removing ions from an ion trap mass spectrometer
WO2004093122A3 (fr) * 2003-04-16 2004-12-16 Univ British Columbia Ejection axiale a geometrie amelioree pour generer un champ bidimensionnel sensiblement quadripolaire
US6897438B2 (en) 2002-08-05 2005-05-24 University Of British Columbia Geometry for generating a two-dimensional substantially quadrupole field

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US5451782A (en) * 1991-02-28 1995-09-19 Teledyne Et Mass spectometry method with applied signal having off-resonance frequency
DE4324224C1 (de) * 1993-07-20 1994-10-06 Bruker Franzen Analytik Gmbh Quadrupol-Ionenfallen mit schaltbaren Multipol-Anteilen
DE4425384C1 (de) * 1994-07-19 1995-11-02 Bruker Franzen Analytik Gmbh Verfahren zur stoßinduzierten Fragmentierung von Ionen in Ionenfallen
US5714755A (en) * 1996-03-01 1998-02-03 Varian Associates, Inc. Mass scanning method using an ion trap mass spectrometer
US5693941A (en) * 1996-08-23 1997-12-02 Battelle Memorial Institute Asymmetric ion trap
DE19751401B4 (de) 1997-11-20 2007-03-01 Bruker Daltonik Gmbh Quadrupol-Hochfrequenz-Ionenfallen für Massenspektrometer
US6124592A (en) * 1998-03-18 2000-09-26 Technispan Llc Ion mobility storage trap and method
DE10028914C1 (de) * 2000-06-10 2002-01-17 Bruker Daltonik Gmbh Interne Detektion von Ionen in Quadrupol-Ionenfallen
US20050229003A1 (en) 2004-04-09 2005-10-13 Miles Paschini System and method for distributing personal identification numbers over a computer network
US7676030B2 (en) 2002-12-10 2010-03-09 Ewi Holdings, Inc. System and method for personal identification number distribution and delivery
US6608303B2 (en) 2001-06-06 2003-08-19 Thermo Finnigan Llc Quadrupole ion trap with electronic shims
US6777673B2 (en) 2001-12-28 2004-08-17 Academia Sinica Ion trap mass spectrometer
JP3653504B2 (ja) * 2002-02-12 2005-05-25 株式会社日立ハイテクノロジーズ イオントラップ型質量分析装置
US10205721B2 (en) 2002-12-10 2019-02-12 Ewi Holdings, Inc. System and method for distributing personal identification numbers over a computer network
US6710334B1 (en) 2003-01-20 2004-03-23 Genspec Sa Quadrupol ion trap mass spectrometer with cryogenic particle detector
US7019289B2 (en) * 2003-01-31 2006-03-28 Yang Wang Ion trap mass spectrometry
WO2004107280A2 (fr) 2003-05-28 2004-12-09 Ewi Holdings, Inc. Systeme et procede pour reconstitution de compte prepaye electronique
CA2539221A1 (fr) * 2003-09-25 2005-03-31 Mds Inc., Doing Business As Mds Sciex Procede et appareil pour la fourniture de champs bidimensionnels sensiblement quadrupolaires ayant des composantes hexapolaires selectionnees
US6982417B2 (en) * 2003-10-09 2006-01-03 Siemens Energy & Automation, Inc. Method and apparatus for detecting low-mass ions
US11475436B2 (en) 2010-01-08 2022-10-18 Blackhawk Network, Inc. System and method for providing a security code
US11599873B2 (en) 2010-01-08 2023-03-07 Blackhawk Network, Inc. Systems and methods for proxy card and/or wallet redemption card transactions
US12260396B2 (en) 2010-01-08 2025-03-25 Blackhawk Network, Inc. System for payment via electronic wallet
US7280644B2 (en) 2004-12-07 2007-10-09 Ewi Holdings, Inc. Transaction processing platform for faciliating electronic distribution of plural prepaid services
US7034293B2 (en) * 2004-05-26 2006-04-25 Varian, Inc. Linear ion trap apparatus and method utilizing an asymmetrical trapping field
US20060045244A1 (en) 2004-08-24 2006-03-02 Darren New Method and apparatus for receipt printing and information display in a personal identification number delivery system
US10296895B2 (en) 2010-01-08 2019-05-21 Blackhawk Network, Inc. System for processing, activating and redeeming value added prepaid cards
US7656236B2 (en) 2007-05-15 2010-02-02 Teledyne Wireless, Llc Noise canceling technique for frequency synthesizer
US8179045B2 (en) 2008-04-22 2012-05-15 Teledyne Wireless, Llc Slow wave structure having offset projections comprised of a metal-dielectric composite stack
US10037526B2 (en) 2010-01-08 2018-07-31 Blackhawk Network, Inc. System for payment via electronic wallet
EP2521999A4 (fr) 2010-01-08 2015-01-07 Blackhawk Network Inc Système de traitement, d'activation et de remboursement de cartes prépayées à valeur ajoutée
CA2809822C (fr) 2010-08-27 2023-09-12 Blackhawk Network, Inc. Carte prepayee avec une fonctionnalite d'epargne
US11042870B2 (en) 2012-04-04 2021-06-22 Blackhawk Network, Inc. System and method for using intelligent codes to add a stored-value card to an electronic wallet
EP2923325A4 (fr) 2012-11-20 2016-08-17 Blackhawk Network Inc Système et procédé pour utiliser des codes intelligents en même temps que des cartes contenant une valeur enregistrée
US9202660B2 (en) 2013-03-13 2015-12-01 Teledyne Wireless, Llc Asymmetrical slow wave structures to eliminate backward wave oscillations in wideband traveling wave tubes

Family Cites Families (3)

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GB8625529D0 (en) * 1986-10-24 1986-11-26 Griffiths I W Control/analysis of charged particles
DE3886922T2 (de) * 1988-04-13 1994-04-28 Bruker Franzen Analytik Gmbh Methode zur Massenanalyse einer Probe mittels eines Quistors und zur Durchführung dieses Verfahrens entwickelter Quistor.
ATE101942T1 (de) * 1989-02-18 1994-03-15 Bruker Franzen Analytik Gmbh Verfahren und geraet zur massenbestimmung von proben mittels eines quistors.

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2261988B (en) * 1991-11-27 1995-05-10 Bruker Franzen Analytik Gmbh A method of removing ions from an ion trap mass spectrometer
GB2267385A (en) * 1992-05-29 1993-12-01 Finnigan Corp Ion trap mass spectrometer method
GB2267385B (en) * 1992-05-29 1995-12-13 Finnigan Corp Method of detecting the ions in an ion trap mass spectrometer
EP0608885A1 (fr) * 1993-01-27 1994-08-03 Varian Associates, Inc. Spectromètre de masse du type piège ionique
US6897438B2 (en) 2002-08-05 2005-05-24 University Of British Columbia Geometry for generating a two-dimensional substantially quadrupole field
US7045797B2 (en) 2002-08-05 2006-05-16 The University Of British Columbia Axial ejection with improved geometry for generating a two-dimensional substantially quadrupole field
WO2004093122A3 (fr) * 2003-04-16 2004-12-16 Univ British Columbia Ejection axiale a geometrie amelioree pour generer un champ bidimensionnel sensiblement quadripolaire

Also Published As

Publication number Publication date
EP0459602A3 (en) 1992-07-01
DE4017264A1 (de) 1991-12-19
US5170054A (en) 1992-12-08
DE4017264C2 (fr) 1992-12-03
EP0459602B1 (fr) 1996-03-13
DE59107529D1 (de) 1996-04-18
EP0459602B2 (fr) 2000-02-09

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