The present research was carried out to obtain more information on materials and painting techniques used in Egyptian wall paintings during the 19th century. The Hawsh al-Basha courtyard, dating back to Mohammed Ali's family period (1805-1952,) was studied for this purpose. The obtained results will be used to set up a scientific plan for restoration and preservation. Pigments, including white zincite, earth green, blue synthetic ultramarine, yellow massicot, black a mixture of magnetite & graphite, brownish red lead and brass were identified. The binding medium in the painting was identified as animal glue. Two preparation layers were identified: the inner coarse ground layer, composed of gypsum as a major component, with calcite and small amounts of quartz and the outer, fine ground layer, composed of calcite only. Optical Microscopy (OM), Scanning Electron Microscopy coupled with Energy Dispersive X-ray Microanalysis (SEM-EDX), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy with Attenuation Total Reflection (FTIR-ATR) were used in our study.