Synchrotron radiation facilities offer intense and tunable X-ray beams, enabling time-efficient acquisition of X-ray absorption spectra, such as X-ray absorption near-edge structure and extended X-ray absorption fine structure, with temporal resolution comparable to the characteristic timescales of structural transformations, including crystallization processes in glasses. In this work, we present the design and implementation of a high-temperature sample holder developed for the ASTRA beamline at the SOLARIS Synchrotron in Kraków, Poland. The holder supports in situ and operando X-ray absorption spectroscopy experiments in both transmission and fluorescence detection modes at temperatures up to 500°C. Its performance was validated through temperature-dependent X-ray absorption spectroscopy measurements of binary vanadate–phosphate glasses undergoing crystallization. The preliminary results confirm the stability, reliability, and applicability of the setup for tracking thermally induced structural changes in solid-state materials using absorption spectroscopy.
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