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Related Experiment Videos

TOF-SIMS: accurate mass scale calibration.

F M Green1, I S Gilmore2, M P Seah2

  • 1Quality of Life Division, National Physical Laboratory, Hampton Road, TW11 0LW, Teddington, Middlesex, UK. Felicia.Green@npl.co.uk.

Journal of the American Society for Mass Spectrometry
|March 1, 2006
PubMed
Summary

Accurate mass calibration in time-of-flight secondary ion mass spectrometry (TOF-SIMS) is improved by optimizing instrumental parameters. This study introduces a new calibration protocol enhancing mass accuracy for both inorganic and organic species.

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Area of Science:

  • Surface Science
  • Analytical Chemistry
  • Spectroscopy

Background:

  • Current time-of-flight secondary ion mass spectrometry (TOF-SIMS) calibration methods yield poor mass accuracy, especially for large molecules.
  • High experimental uncertainty leads to misidentification and ambiguous assignments of peaks.
  • Instrumental stability is high, but mass accuracy limitations hinder unique species identification.

Purpose of the Study:

  • To investigate instrumental parameters affecting mass scale calibration in TOF-SIMS.
  • To understand the reasons for differing peak positions between molecular and atomic ions.
  • To develop an optimized calibration procedure for improved mass accuracy.

Main Methods:

  • Detailed study of instrumental parameters using ion trajectory calculations with SIMION.

Related Experiment Videos

  • Analysis of effects of ion kinetic energy, emission angle, and operating parameters on peak position.
  • Development of a new calibration protocol and a generic set of calibration ions.

    • Main Results:

    • Identified the need for an aperture to restrict ions at large emission angles.
    • Achieved a factor of 5 improvement in mass accuracy in an interlaboratory study.
    • Developed a calibration protocol yielding relative mass accuracy better than 10 ppm for masses up to 140 u.
    • Demonstrated an alternative instrument operating regime for studying molecular fragmentation energies.

    Conclusions:

    • Optimized instrumental parameters and a new calibration protocol significantly enhance TOF-SIMS mass accuracy.
    • The developed protocol provides reliable mass calibration for inorganic and organic species.
    • Recommendations are provided for accurate mass determination of large molecules and for studying fragmentation energies.