| Abstract Scope |
Glass delamination occurs when a container succumbs to chemical attack from its contents, releasing microscopic thin flakes, or lamellae, of glass into the liquid. These lamellae raise serious quality issues for pharmaceutical manufacturers, so microanalytical investigations are required to determine root cause and inform remediation. Compositional characterization of lamellae by X-ray energy dispersive spectrometry (EDS) results in significant uncertainty, since the EDS information depth (micrometers) exceeds the thickness of typical lamellae (tens of nanometers). The present study addresses this uncertainty by demonstrating X-ray photoelectron spectroscopy (XPS), a compositional analysis technique that features an information depth of a few nanometers. XPS mapping to locate lamellae on a filter, argon ion cluster source etching to preferentially remove organic material from the glass surface, and charge-compensated XPS compositional analysis of both lamellae and the source glass will be demonstrated. These data offer more detailed compositions than EDS, elucidating the delamination mechanism. |