Gilding has in all times occupied an important place in the ornamental arts of Islamic civilization, especially the decorated ceilings, which is the art of spreading gold over the surface for the purpose of ornament. Unfortunately we haven't sufficient data about its composition and the application techniques. The main goal of the present study is to investigate and analyze samples from gilding materials and its ground from some Islamic monumental ceilings in Cairo to determine the composition, methods of application and its aspects of deterioration. Samples were taken from the gilded areas of the selected ceilings. Scanning electron microscope–energy dispersive X-ray spectroscopy (SEM–EDX), Light Optical microscope (L.O.M.) and Fourier transmitanceinfrared spectroscopy (FTIR), were adapted for analysis and investigations. The results from samples taken from different gilded ceilings were compared with each other to observe their differences and similarities .Analysis and investigation, methods revealed a further resemblance of the materials and the methodology employed. The deteriorated golden leaves were the main component applied by means of a size, Golden leaves and powder, brass, were used for the previous intervention.