In this paper is presented the study of the painting materials and techniques used in 18th century wall paintings that originated in the orthodox church of St Athanasius, in the city of Moschopolis, Albania. The church was painted in 1745 by Konstantinos and Athanasios Zografi, and during recent years, conservation activities has been performed at the church. A total number of 8 samples that include 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 Total Reflective X-Ray Fluorescence (TXRF). Common pigments used in Balkan peninsula at 15th-16th centuries, such as cinnabar, green earth, manganese oxide, carbon black and calcite were identified. The presence of calcite in almost all the pigments is indicative for the use of the fresco technique however, some areas were identified as containing egg tempera. The detection of gypsum and calcium oxalate indicates environmental degradation and biodeterioration.