ASTM International

Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer
 N E2108

Annotation

This practice describes a procedure for calibrating the electron binding-energy (BE) scale of an X-ray photoelectron spectrometer that is to be used for surface analysis with unmonochromated aluminum or magnesium K? X-rays or monochromated aluminum K? X rays.

It is recommended that the BE scale be calibrated after the instrument is installed or modified in any substantive way. Also, it is recommended that the instrumental BE scale be checked, and if necessary, recalibrated at intervals chosen to ensure that BE measurements are statistically unlikely to be made with greater uncertainty than a tolerance limit, specified by the analyst, based on the instrumental stability and the analyst’s needs. Information is provided by which an analyst can select an appropriate tolerance limit for the BE measurements and the frequency of calibration checks.

This practice is based on the assumption that the BE scale of the spectrometer is sufficiently close to linear that the BE scale can be calibrated by measurements of reference photoelectron lines made near the extremes of the working BE scale. In most commercial instruments, X-ray sources with aluminum or magnesium anodes are employed and BEs are typically measured over the 0–1000 eV range. This practice can be used for the BE range from 0 eV to 1040 eV.

The assumption that the BE scale is linear is checked by a measurement made with a reference photoelectron line or Auger-electron line that appears at an intermediate position. A single check is a necessary but not sufficient condition for establishing linearity of the BE scale. Additional checks can be made with specified reference lines on instruments equipped with magnesium or unmonochromated aluminum X-ray sources, with secondary BE standards, or by following the procedures of the instrument manufacturer. Deviations from BE-scale linearity can occur because of mechanical misalignments, excessive magnetic fields in the region of the analyzer, or imperfections or malfunctions in the power supplies. This practice does not check for, nor identify, problems of this type.