In this study, two sample sets from Zeugma Archaeological Area had been examined. The sample Set I includes 7 sediment, 18 stone, 4 brick/roof tile, 9 mortar, 4 plaster samples and the sample Set II consists of 24 mural painting samples. Samples were examined to get their raw material characteristics, mineralogical and chemical compositions, and microstructural properties using various analytical techniques such as Optical Microscopy, XRD, FTIR, PED-XRF, SEM-EDX and Raman Spectroscopy. In addition, mikroclimatic monitorings for temperature and relative humidity were also performed in that area. Sediments were calcereous soils of Eocene. Rock types of stones were mainly limestone which had 3 subgroups: micritic, biomicritic and recrytallised micritic limestones. The source of the limestones should be from the local formation. The firing temperature of brick/roof tile samples were estimated as 800-850&deg / C. Binder of mortar samples were mainly lime. Aggregate materials of brick/roof tiles, mortars, plasters and mural paintings may come from the river deposites of Euphrates. Mural painting samples have one intonaco layer, and single or double arriccio layers. The mural painting technique was fresco technique. Calcite was common mineral identified for all pigments. The sources of white, black and green coloured pigments were found as vaterite, graphite and malachite respectively. The sources of yellow coloured pigments were identified as ankerite, siderite and goethite. The red colours were identified as hematite, jasper and red earth/ochre. Jasper and vaterite, jasper and calcite, red earth/ochre and calcite, and hematite were the colour forming minerals of pink coloured pigments.