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Recent developments of X-ray photoelectron spectroscopy using excitation energies different from the usual lab-sources Mg Kα and Al Kα, thus covering larger and different kinetic energy ranges, require more flexible approaches for determining the transmission function than the well-established ones using reference spectra. Therefore, the approach using quantified peak areas (QPA) was refined allowing a more precise estimation of the transmission function. This refinement was tested by comparing the results obtained with the new version with former calculations. Furthermore, the obtained transmission function was validated by comparing the results with a transmission function using the reference spectrum of polyethylene. Additionally, an ionic liquid was used as reference for estimating the transmission function at the energy resolved HE-SGM beamline at BESSY II. Comparison between the measured and stoichiometric composition shows that a transmission function was determined, which allows a reasonable quantification.
The uncertainty of measurement in quantitative XPS analysis can be reduced by using a calibrated spectrometer transmission function T (E), which is usually determined by taking spectra from Au, Ag, Cu and Ge elemental reference materials. However, this approach is quite time-consuming due to required sample preparation steps like sputter cleaning etc., and the relatively big number of samples to be measured. This contribution proposes the use of the ionic liquids [C2C1im][NTf2] and [C3C1im][NTf2] as reference materials for a determination of T(E). These multi-elemental samples deliver five intensive photoemission peaks, F 1s, O 1s, N 1s, C 1s and S 2p, in an energy window from 160 eV to 700 eV which is of specific interest for applications of quantitative XPS for surface chemical analysis of soft matter, one of the major applications of XPS.
Objectives. There is concern that the integrity of fiberglass dental posts may be affected by chairside trimming during treatment. We hypothesize that hard X-ray methods of phase contrast-enhanced micro-CT (PCE-CT) and synchrotron based X-ray refraction (SXRR) can reliably identify and help characterize the extent of damage.
Methods. Fiberglass posts were imaged both as manufactured and following trimming with a diamond bur. Each of the posts was imaged by SXRR and by PCE-CT. Datasets from PCE-CT were used to visualize and quantify 2D and 3D morphological characteristics of intact and of damage-affected regions caused by trimming. Results. The SXRR images revealed fiber inhomogeneities from manufacturing with a significant increase in internal surfaces in sample regions corresponding to damage from trimming. PCE-CT volumes unveiled the micromorphology of single fibers in the posts and some damage in the trimmed area (e.g. fractures, splinters and cracks). Area, perimeter, circularity, roundness, volume and thickness of the glass fibers in the trimmed area were statistically different from the control (p < 0.01).
Significance. The integrity of single fibers in the post is critical for bending resistance and for long-term adhesion to the cement in the root canals. Damage to the fibers causes substantial structural weakening across the post diameter. Glass fragments produced due to contact with the dental bur may separate from the post and may significantly reduce bond capacity. The above mentioned synchrotron-based imaging techniques can further facilitate assessment of the structural integrity and the appearance of defects in posts (e.g. after mechanical load).