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Here, we report the physico-chemical characterization of wall paintings from the Petros and Paulos church in Ethiopia. This work represents the first technical study of paintings located in Ethiopia, rather than paintings in museum collections outside the country, using diverse analytical techniques. In situ examination with a portable X-ray fluorescence spectrometer (pXRF) was followed by analysis of samples using optical microscopy (OM), scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM/EDS), micro-Raman spectroscopy (MRS), attenuated total reflection - Fourier transform infrared spectroscopy (ATR-FT-IR), X-ray powder diffraction (XRD) and pyrolysis gas chromatography - mass spectrometry (Py-GC/MS). The paint stratigraphy, the compositions of the support material, the preparatory and painting layers were studied, as well as the morphology of the pigment particles. The results revealed the use of earth pigments and carbon black. The preparatory layer was uncommon; composed of dolomite, clay rich in clinochlore and sand, in contrast to the more common gypsum and calcite. The binder and the stratigraphic analyses suggested a distempera technique. [ABSTRACT FROM AUTHOR]