AbstractIn this paper are presented the studies of the paint materials and the technique used in 18th century wall paintings, originated from the orthodox church of St Athanasius, in the city of Maschopolis, a flourishing economical and cultural center, in Albania. The church was painted in 1745 by Konstantinos and Athanasios Zografi, and during the last years, restoration activities are being performed at the church. Samples that included plasters and pigments of different colors were collected from important points of the wall paintings. Additionally, as some parts of the wall-paintings were over-painted, the analysis was extended to the compositional characterization of these areas. The identification of the used materials was done by using complementary analytical methods such as Optical Microscopy, Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM-EDS) and X-ray fluorescence (TXRF).The presence of calcite in almost all the pigments is indicative for the use of the fresco technique at the studied areas, while the detection of gypsum and calcium oxalate, indicates an environmental degradation along with a biodegradation. Common pigments used in this area at 15-16th centuries, such as cinnabar, green earth, manganese oxide, carbon black and calcite were identified.