EP1220291A2 - Massenpektrometrisches Verfahren und massenpektrometrische Vorrichtung - Google Patents

Massenpektrometrisches Verfahren und massenpektrometrische Vorrichtung Download PDF

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Publication number
EP1220291A2
EP1220291A2 EP01310017A EP01310017A EP1220291A2 EP 1220291 A2 EP1220291 A2 EP 1220291A2 EP 01310017 A EP01310017 A EP 01310017A EP 01310017 A EP01310017 A EP 01310017A EP 1220291 A2 EP1220291 A2 EP 1220291A2
Authority
EP
European Patent Office
Prior art keywords
vacuum chamber
mass spectrometer
electrodes
ion guide
ion
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.)
Granted
Application number
EP01310017A
Other languages
English (en)
French (fr)
Other versions
EP1220291B1 (de
EP1220291A3 (de
Inventor
Robert Harold Bateman
Kevin Giles
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.)
Micromass UK Ltd
Original Assignee
Micromass UK Ltd
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
Priority claimed from GBGB0029088.2A external-priority patent/GB0029088D0/en
Priority claimed from GB0110149A external-priority patent/GB0110149D0/en
Priority claimed from GBGB0115504.3A external-priority patent/GB0115504D0/en
Priority claimed from GB0120029A external-priority patent/GB2370685B/en
Application filed by Micromass UK Ltd filed Critical Micromass UK Ltd
Publication of EP1220291A2 publication Critical patent/EP1220291A2/de
Publication of EP1220291A3 publication Critical patent/EP1220291A3/de
Application granted granted Critical
Publication of EP1220291B1 publication Critical patent/EP1220291B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • H01J49/06—Electron- or ion-optical arrangements
    • H01J49/062—Ion guides
    • H01J49/065—Ion guides having stacked electrodes, e.g. ring stack, plate stack

Definitions

  • the present invention relates to mass spectrometers and methods of mass spectrometry.
  • Ion guides comprising rf-only multipole rod sets such as quadrupoles, hexapoles and octopoles are well known.
  • An ion guide comprised of electrodes having apertures may take two main different forms. In a first form all the internal apertures of the electrodes are substantially the same size. Such an arrangement is known as an "ion tunnel". However, a second form referred to as an “ion funnel” is known wherein the electrodes have internal apertures which become progressively smaller in size. Both forms are intended to fall within the scope of the present invention.
  • the apertured electrodes in either case may comprise ring or annular electrodes.
  • the inner circumference of the electrodes is preferably substantially circular. However, the outer circumference of the electrodes does not need to be circular and embodiments of the present invention are contemplated wherein the outer profile of the electrodes takes on other shapes.
  • the preferred embodiment of the present invention uses an ion tunnel ion guide and it has been found that an ion tunnel ion guide exhibits an approximately 25-75% improvement in ion transmission efficiency compared with a conventional multipole, e.g. hexapole, ion guide of comparable length.
  • a conventional multipole e.g. hexapole
  • ion guide of comparable length.
  • the reasons for this enhanced ion transmission efficiency are not fully understood, but it is thought that the ion tunnel may have a greater acceptance angle and a greater acceptance area than a comparable multipole rod set ion guide.
  • one advantage of the preferred embodiment is an improvement in ion transmission efficiency.
  • the inter-vacuum chamber ion guide may comprise an ion funnel.
  • a dc potential gradient is applied along the length of the ion funnel in order to urge ions through the progressively smaller internal apertures of the electrodes.
  • the ion funnel is believed however to suffer from a narrow mass to charge ratio bandpass transmission efficiency. Such problems are not found when using an ion tunnel ion guide.
  • ion optical devices including multipole rod sets, Einzel lenses, segmented multipoles, short (solid) quadrupole pre/post filter lenses ("stubbies"), 3D quadrupole ion traps comprising a central doughnut shaped electrode together with two concave end cap electrodes, and linear (2D) quadrupole ion traps comprising a multipole rod set with entrance and exit ring electrodes.
  • stubbies segmented multipoles
  • 3D quadrupole ion traps comprising a central doughnut shaped electrode together with two concave end cap electrodes
  • 2D linear quadrupole ion traps comprising a multipole rod set with entrance and exit ring electrodes
  • one of the electrodes forming the ion guide may form or constitute a differential pumping aperture between two vacuum chambers.
  • Such an arrangement is particularly advantageous since it allows the interchamber orifice to be much smaller than that which would be provided if a multipole rod set ion guide were used. A smaller interchamber orifice allows the vacuum pumps pumping each vacuum chamber to operate more efficiently.
  • the electrode forming the differential pumping aperture may either have an internal aperture of different size (e.g. smaller) than the other electrodes forming the ion guide or may have the same sized internal aperture.
  • the electrode forming the differential pumping aperture and/or the other electrodes may have an internal diameter selected from the group comprising: (i) 0.5-1.5 mm; (ii) 1.5-2.5 mm; (iii) 2.5-3.5 mm; (iv) 3.5-4.5 mm; (v) 4.5-5.5 mm; (vi) 5.5-6.5 mm; (vii) 6.5-7.5 mm; (viii) 7.5-8.5 mm; (ix) 8.5-9.5 mm; (x) 9.5-10.5 mm; (xi) ⁇ 10.0 mm; (xii) ⁇ 9.0 mm; (xiii) ⁇ 8.0 mm; (xiv) ⁇ 7.0 mm; (xv) 6.0 mm; (xvi) ⁇ 5.0 mm; (xvii) ⁇
  • the differential pumping aperture may have an area selected from the group comprising: (i) ⁇ 40 mm 2 ; (ii) ⁇ 35 mm 2 ; (iii) ⁇ 30 mm 2 ; (iv) ⁇ 25 mm 2 ; (v) ⁇ 20 mm 2 ; (vi) ⁇ 15 mm 2 ; (vii) ⁇ 10 mm 2 ; and (viii) ⁇ 5 mm 2 .
  • the area of the differential pumping aperture may therefore be more than an order of magnitude smaller than the area of the differential pumping aperture inherent with using a multipole ion guide to extend between two vacuum regions.
  • the ion guide may comprise at least 4, 5, 6, 7, 8, 9, 10, 20, 30, 40, 50, 60, 70, 80, 90, 100, 110, 120, 130, 140, 150, 160, 170, 180, 190 or 200 electrodes. At least 90%, preferably 100% of the electrodes may be arranged and adapted to be maintained at substantially the same dc reference potential upon which an AC voltage is superimposed.
  • the pressure in the upstream vacuum chamber may, preferably, be: (i) ⁇ 0.5 mbar; (ii) ⁇ 0.7 mbar; (iii) ⁇ 1.0 mbar; (iv) ⁇ 1.3 mbar; (v) ⁇ 1.5 mbar; (vi) ⁇ 2.0 mbar; (vii) ⁇ 5.0 mbar; (viii) ⁇ 10.0 mbar; (ix) 1-5 mbar; (x) 1-2 mbar; or (xi) 0.5-1.5 mbar.
  • the pressure is less than 30 mbar and further preferably less than 20 mbar.
  • the pressure in the downstream vacuum chamber may, preferably, be: (i) 10 -3 -10 -2 mbar; (ii) ⁇ 2 x 10 -3 mbar; (iii) ⁇ 5 x 10 -3 mbar; (iv) ⁇ 10 -2 mbar; (v) 10 -3 -5 x 10 -3 mbar; or (vi) 5 x 10 -3 -10 -2 mbar.
  • At least a majority, preferably all, of the electrodes forming the ion guide may have apertures having internal diameters or dimensions: (i) ⁇ 5.0 mm; (ii) ⁇ 4.5 mm; (iii) ⁇ 4.0 mm; (iv) ⁇ 3.5 mm; (v) ⁇ 3.0 mm; (vi) ⁇ 2.5 mm; (vii) 3.0 ⁇ 0.5 mm; (viii) ⁇ 10.0 mm; (ix) ⁇ 9.0 mm; (x) ⁇ 8.0 mm; (xi) ⁇ 7.0 mm; (xii) ⁇ 6.0 mm; (xiii) 5.0 ⁇ 0.5 mm; or (xiv) 4-6 mm.
  • the length of the ion guide may be: (i) ⁇ 100 mm; (ii) ⁇ 120 mm; (iii) ⁇ 150 mm; (iv) 130 ⁇ 10 mm; (v) 100-150 mm; (vi) ⁇ 160 mm; (vii) ⁇ 180 mm; (viii) ⁇ 200 mm; (ix) 130-150 mm; (x) 120-180 mm; (xi) 120-140 mm; (xii) 130 mm ⁇ 5, 10, 15, 20, 25 or 30 mm; (xiii) 50-300 mm; (xiv) 150-300 mm; (xv) ⁇ 50 mm; (xvi) 50-100 mm; (xvii) 60-90 mm; (xviii) ⁇ 75 mm; (xix) 50-75 mm; (xx) 75-100 mm; (xxi) approx. 26 cm; (xxii) 24-28 cm; (xxiii) 20-30 cm; or (xxiv
  • the ion source is an atmospheric pressure ion source such as an Electrospray (“ES”) ion source or an Atmospheric Pressure Chemical Ionisation (“APCI”) ion source.
  • the ion source may be a Matrix Assisted Laser Desorption Ionisation (“MALDI”) ion source or an Inductively Coupled Plasma (“ICP”) ion source.
  • the MALDI ion source may be either an atmospheric source or a low vacuum source.
  • the ion source is a continuous ion source.
  • the mass spectrometer preferably comprises either a time-of-flight mass analyser, preferably an orthogonal time of flight mass analyser, a quadrupole mass analyser or a quadrupole ion trap.
  • an electrode of the ion guide forms a differential pumping aperture between the input and intermediate vacuum chambers.
  • the mass spectrometer comprises means for supplying an AC-voltage to the electrodes.
  • an AC generator is provided which is connected to the electrodes in such a way that at any instant during an AC cycle of the output of the AC generator, adjacent ones of the electrodes forming the AC-only ion guide are supplied respectively with approximately equal positive and negative potentials relative to a reference potential.
  • the AC power supply may be an RF power supply.
  • the present invention is not intended to be limited to RF frequencies.
  • AC is intended to mean simply that the waveform alternates and hence embodiments of the present invention are also contemplated wherein non-sinusoidal waveforms including square waves are supplied to the ion guide.
  • At least 5, 10, 15, 20, 25, 30, 35, 40, 45, 50 or 100 of the electrodes are disposed in one or both vacuum chambers.
  • a differential pumping aperture between the vacuum chambers is formed by an electrode of the ion guide, the differential pumping aperture having an area ⁇ 20 mm 2 , preferably ⁇ 15 mm 2 , further preferably ⁇ 10 mm 2 .
  • a mass spectrometer as claimed in claim 33.
  • a substantially continuous ion tunnel ion guide may be provided which extends through two, three, four or more vacuum chambers. Also, instead of each vacuum chamber being separately pumped, a single split flow vacuum pump may preferably be used to pump each chamber.
  • an ion tunnel 15 comprises a plurality of electrodes 15a,15b having apertures. Adjacent electrodes 15a,15b are connected to different phases of an AC power supply which may in one embodiment be an RF power supply.
  • the first, third, fifth etc. electrodes 15a may be connected to the 0° phase supply 16a
  • the second, fourth, sixth etc. electrodes 15b may be connected to the 180° phase supply 16b.
  • Ions from an ion source pass through the ion tunnel 15 and are efficiently transmitted by it.
  • preferably all of the electrodes 15a,15b are maintained at substantially the same dc reference potential about which an AC voltage is superimposed. Unlike ion traps, blocking dc potentials are not applied to either the entrance or exit of the ion tunnel 15.
  • Fig. 2 shows a preferred embodiment of the present invention.
  • An Electrospray (“ES”) ion source 1 or an Atmospheric Pressure Chemical Ionisation (“APCI”) ion source 1 (which requires a corona pin 2) emits ions which enter a vacuum chamber 17 via a sample cone 3.
  • Vacuum chamber 17 is pumped by a rotary or mechanical pump 4.
  • a portion of the gas and ions pass through a differential pumping aperture 21 with the plate surrounding the aperture being preferably maintained at 50-120V into a vacuum chamber 18 housing an ion tunnel ion guide 15 which extends into another vacuum chamber 19.
  • Vacuum chamber 18 is pumped by a rotary or mechanical pump 7.
  • Ions are transmitted by the ion guide 15 through the vacuum chamber 18 and pass, without exiting the ion guide 15, through another differential pumping aperture 8 formed by an electrode of the ion tunnel ion guide 15 into vacuum chamber 19 which is pumped by a turbo-molecular pump 10. Ions continue to be transmitted by the ion tunnel ion guide 15 through the vacuum chamber 19. The ions then leave the ion guide 15 and pass through differential pumping aperture 11 into an analyser vacuum chamber 20 which is pumped by a turbo-molecular pump 14.
  • Analyser vacuum chamber 20 houses a prefilter rod set 12, a quadrupole mass filter/analyser 13 and may include other elements such as a collision cell (not shown), another quadrupole mass filter/analyser together with an ion detector (not shown) or a time of flight analyser (not shown).
  • An AC-voltage is applied to the electrodes and the ion tunnel 15 is preferably maintained at 0-2 V dc above the dc potential of the plate forming the differential pumping aperture 11 which is preferably at ground (0 V dc). According to other embodiments, the plate forming the differential pumping aperture 11 may be maintained at other dc potentials.
  • the ion tunnel 15 is preferably about 26 cm long and in one embodiment comprises approximately 170 ring electrodes.
  • Upstream vacuum chamber 18 is preferably maintained at a pressure ⁇ 1 mbar, and downstream vacuum chamber 19 is preferably maintained at a pressure of 10 - 3 -10 -2 mbar.
  • the ion guide 15 is preferably supplied with an AC-voltage at a frequency of between 1-2 MHz. However, according to other embodiments, frequencies of 800kHz-3MHz may be used.
  • the electrodes forming the ion tunnel 15 preferably have circular apertures which preferably have a diameter in the range of 3-5 mm.
  • Electrodes of the ion tunnel in one vacuum chamber have a different peak AC voltage amplitude compared with electrodes of the same ion tunnel which are disposed in another vacuum chamber.
  • the electrodes disposed in chamber 18 may be coupled to the AC power supply 16a,16b via a capacitor but the electrodes disposed in chamber 19 may be directly coupled to the AC power supply 16a,16b. Accordingly, the electrodes disposed in chamber 19 may see a peak AC voltage of 500V, but the electrodes disposed in chamber 18 may see a peak AC voltage of 300V.
  • the electrode which forms the differential pumping aperture 8 may be maintained at the AC voltage of either the electrodes in chamber 18 or the electrodes in chamber 19, or alternatively the electrode may be maintained at a voltage which is different from the other electrodes.

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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)
EP01310017A 2000-11-29 2001-11-29 Massenspektrometer und massenspektrometrisches Verfahren Expired - Lifetime EP1220291B1 (de)

Applications Claiming Priority (10)

Application Number Priority Date Filing Date Title
GB0029088 2000-11-29
GBGB0029088.2A GB0029088D0 (en) 2000-11-29 2000-11-29 Ion tunnel
GB0109760 2001-04-20
GBGB0109760.9A GB0109760D0 (en) 2000-11-29 2001-04-20 Mass spectrometers and methods of mass spectrometry
GB0110149 2001-04-25
GB0110149A GB0110149D0 (en) 2000-11-29 2001-04-25 Mass spectrometers and methods of mass spectrometry
GB0115504 2001-06-25
GBGB0115504.3A GB0115504D0 (en) 2000-11-29 2001-06-25 Mass spectrometers and methods of mass spectrometry
GB0120029A GB2370685B (en) 2000-11-29 2001-08-16 Mass spectrometers and methods of mass spectrometry
GB0120029 2001-08-16

Publications (3)

Publication Number Publication Date
EP1220291A2 true EP1220291A2 (de) 2002-07-03
EP1220291A3 EP1220291A3 (de) 2004-08-25
EP1220291B1 EP1220291B1 (de) 2007-02-28

Family

ID=27515995

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01310017A Expired - Lifetime EP1220291B1 (de) 2000-11-29 2001-11-29 Massenspektrometer und massenspektrometrisches Verfahren

Country Status (3)

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EP (1) EP1220291B1 (de)
AT (1) ATE355608T1 (de)
DE (2) DE20122469U1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2422051A (en) * 2004-10-05 2006-07-12 Bruker Daltonik Gmbh Ion guides with rf diaphragm stacks

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2447539C2 (ru) * 2009-05-25 2012-04-10 Закрытое акционерное общество "Геркон-авто" Анализатор пролетного квадрупольного масс-спектрометра (типа фильтр масс, "монополь" и "триполь")

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997049111A1 (en) * 1996-06-17 1997-12-24 Battelle Memorial Institute Method and apparatus for ion and charged particle focusing
JP3571546B2 (ja) * 1998-10-07 2004-09-29 日本電子株式会社 大気圧イオン化質量分析装置

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2422051A (en) * 2004-10-05 2006-07-12 Bruker Daltonik Gmbh Ion guides with rf diaphragm stacks
US7391021B2 (en) 2004-10-05 2008-06-24 Bruker Dalton K Gmbh Ion guides with RF diaphragm stacks
GB2422051B (en) * 2004-10-05 2009-11-18 Bruker Daltonik Gmbh Ion guides with RF diaphragm stacks

Also Published As

Publication number Publication date
DE60126901T2 (de) 2007-06-14
EP1220291B1 (de) 2007-02-28
EP1220291A3 (de) 2004-08-25
ATE355608T1 (de) 2006-03-15
DE20122469U1 (de) 2005-11-24
DE60126901D1 (de) 2007-04-12

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