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Fourier Transform Ion Cyclotron Resonance Mass Spectrometry: a Primer

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Fourier Transform Ion Cyclotron Resonance Mass Spectrometry: a Primer FOURIER TRANSFORM ION CYCLOTRON RESONANCE MASS SPECTROMETRY: A PRIMER Alan G. Marshall,*² Christopher L. Hendrickson, and George S. Jackson² Center for Interdisciplinary Magnetic Resonance, National High Magnetic Field Laboratory, Florida State University, 1800 East Paul Dirac Dr., Tallahassee, FL 32310 Received 7 January 1998; revised 4 May 1998; accepted 6 May 1998 I. Introduction .......................................................................................................... 2 II. Ion Cyclotron Motion: Ion Cyclotron Orbital Frequency, Radius, Velocity, and Energy................................ 2 III. Excitation and Detection of an ICR Signal ............................................................................ 5 A. Azimuthal Dipolar Single-Frequency Excitation ................................................................... 5 B. Azimuthal Dipolar Single-Frequency Detection .................................................................... 6 C. Broadband Excitation ............................................................................................. 7 D. Broadband Detection: Detection Limit............................................................................. 9 IV. Ion-Neutral Collisions ................................................................................................ 9 V. Effects of Axial Con®nement of Ions in a Trap of Finite Size ......................................................... 11 A. Axial Ion Oscillation Due to z-Component of Electrostatic Trapping Potential ..................................... 11 B. Radial Ion ``Magnetron'' Rotation Due to Combination of B-Field and r-Component of Electrostatic Trapping Potential .......................................................................................................... 13 C. Mass Calibration .................................................................................................. 14 VI. Quadrupolar Excitation, Axialization, and Remeasurement ............................................................ 15 VII. Effect of Trap Size and Shape on Dipolar and 2D-Quadrupolar Excitation............................................. 16 VIII. Mass Resolving Power, Mass Resolution, and Mass Accuracy......................................................... 17 IX. Upper Mass and Energy Limits ....................................................................................... 17 A. Trap Dimension Mass Limit....................................................................................... 17 B. Trapping Potential Mass Limit .................................................................................... 18 C. Trapping Potential Energy Limit: Space Charge and the Peak Coalescence Mass Limit ............................ 19 X. Ion Sources........................................................................................................... 20 A. Internal Ionization................................................................................................. 20 B. External Ionization ................................................................................................ 20 C. Chromatographic Interfaces ....................................................................................... 21 XI. MS/MS and MSn: CAD (SORI, MECA, VLE), IRMPD, SID, BIRD .................................................. 21 XII. Advantages of High Magnetic Field................................................................................... 22 XIII. Fourier Transform Spectroscopy Aspects.............................................................................. 22 XIV. Relation to Paul (quadrupole) Ion Trap ............................................................................... 24 XV. Selected Applications ................................................................................................. 24 A. Elemental Composition from Accurate Mass Measurement ........................................................ 24 B. Detection Limit for Biological Analysis ........................................................................... 25 C. High Mass ........................................................................................................ 26 D. Isotopic Ampli®cation for Unit Mass Accuracy of Biomacromolecules............................................. 27 Appendix A: FT-ICR Reviews ............................................................................................. 27 Appendix B: List of Physical Constants: Precise Masses of Various Common Elements .................................... 29 Appendix C: Further Reading .............................................................................................. 30 References ................................................................................................................. 31 Mass Spectrometry Reviews, 1998, 17, 1±35 q 1998 by John Wiley & Sons, Inc. CCC 0277-7037/98/010001-35 8218/ 8218$$0329 09-14-98 10:53:33 msra W: MSR 329 n MARSHALL, HENDRICKSON, AND JACKSON This review offers an introduction to the principles and generic damental aspects of FT-ICR can be understood from very applications of FT-ICR mass spectrometry, directed to readers simple idealized models. First, ion cyclotron frequency, with no prior experience with the technique. We are able to radius, velocity, and energy as a function of ion mass, ion explain the fundamental FT-ICR phenomena from a simpli®ed charge, and magnetic ®eld strength follow directly from theoretical treatment of ion behavior in idealized magnetic and the motion of an ion in a spatially uniform static magnetic electric ®elds. The effects of trapping voltage, trap size and ®eld. Second, ion cyclotron motion may be rendered spa- shape, and other nonidealities are manifested mainly as pertur- bations that preserve the idealized ion behavior modi®ed by tially coherent (and thus observable) by the application of appropriate numerical correction factors. Topics include: effect a spatially uniform rf electric ®eld (excitation) at the same of ion mass, charge, magnetic ®eld, and trapping voltage on ion frequency as (i.e., ``resonant'' with) the ion cyclotron fre- cyclotron frequency; excitation and detection of ICR signals; quency. The ICR (time-domain) signal results from induc- mass calibration; mass resolving power and mass accuracy; tion (detection) of an oscillating ``image'' charge on two upper mass limit(s); dynamic range; detection limit, strategies conductive in®nitely extended opposed parallel electrodes. for mass and energy selection for MSn; ion axialization, cooling, A frequency-domain spectrum (convertible to a mass-do- and remeasurement; and means for guiding externally formed main spectrum) is obtained by Fourier transformation of ions into the ion trap. The relation of FT-ICR MS to other types the digitized time-domain ICR signal. Third, con®nement of Fourier transform spectroscopy and to the Paul (quadrupole) of ions by the application of a three-dimensional axial ion trap is described. The article concludes with selected appli- quadrupolar d.c. electric ®eld shifts the ion cyclotron fre- cations, an appendix listing accurate fundamental constants needed for ultrahigh-precision analysis, and an annotated list quency, whereas excitation and detection remain essen- of selected reviews and primary source publications that de- tially linear (i.e., doubling the excitation amplitude dou- scribe in further detail various FT-ICR MS techniques and bles the detected ICR signal) but with a reduced propor- applications. q 1998 John Wiley & Sons, Inc., Mass Spec Rev tionality constant. A simple mass calibration rule follows 17, 1±35, 1998 from this treatment. Thus, FT-ICR MS may be performed in essentially the same way in ion traps of widely different shape (e.g., cubic, cylindrical). Fourth, collisions broaden I. INTRODUCTION the ICR signal in a simple way, and actually make it possible to cool and compress an ion packet for improved Fourier transform ion cyclotron resonance mass spectrom- detection (and even multiple remeasurement). Fifth, al- etry (FT-ICR MS or FTMS) is widely practiced (more though FT-ICR MS has been coupled to virtually every than 235 installations worldwide by 1998). In the 24 years type of ion source, most ion sources work best (or at since its inception (Comisarow and Marshall, 1974; Comi- least most conveniently) outside the magnet. Thus, several sarow and Marshall, 1974), FT-ICR MS has been the sole methods have been developed to guide externally gener- or principal subject of three books, four journal special ated ions into an ion trap inside a high-®eld magnet. Fi- issues, and more than 60 review articles (see Appendix nally, the above features may be combined in various ex- A). However, the various prior descriptions and reviews perimental ``event sequences'' (much like pulse sequences are distributed among dozens of primary publications with in FT-NMR spectroscopy) to perform tandem-in-time n different formalism and notation, and those articles are mass spectrometry (MS/MS, or MS ). directed mainly at FT-ICR MS practitioners. Here, we present an introduction to the principles and generic appli- cations of FT-ICR MS, at the minimum depth needed II. ION CYCLOTRON MOTION: ION to explain the concepts, directed to those without prior CYCLOTRON ORBITAL FREQUENCY, experience in the ®eld. RADIUS, VELOCITY, AND ENERGY Fortunately for beginners, it turns out that many fun- An ion moving in the presence of a spatially uniform magnetic ®eld, B Å0B0k
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