<p>This study focuses on the characterization of representative stone, plaster, soil, and mortar samples from Mor Kuryakos Monastery using both destructive and non-destructive techniques. Optical microscopy (OM), polarized energy-dispersive X-ray fluorescence (PED- XRF), X-ray diffraction (XRD), Fourier transform infrared (FTIR), thermogravimetric-differential thermal analysis (TG-DTA), and scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM-EDX) are employed as advanced analytical techniques. Additionally, basic tests such as water absorption, unit weight, porosity, unit volume, aggregate/binder granulometric analysis, and salt testing were performed. The results indicated four types of stone, which could be attributed to local or regional sources, given the area's geology. The variety in the stone groups also suggested that restoration interventions may have been carried out in the past. For the mortars, the results indicated different compositions, but a single type of binding mortar appeared to be used at the main entrance gate. The diversity in particle size distribution in mortars was attributed to differences in raw material sources and/or preparation methods. The plaster samples displayed clear similarities with their lime-dominant compositions. The soil sample, from the top cover of the monastery’s stone wall, was identified by its high calcium content. This indicates a calcareous character with possible marly-clay inclusions. Such soil may also have been used as an additive in some of the mortars containing clay minerals. It is anticipated that the archaeometric data from this study will provide a guide for understanding the monastery’s building materials. Such knowledge is believed to be useful, particularly for further conservation and restoration applications, as well as the archaeometric studies on building materials in the Upper Tigris region.</p>