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Dar al Manjara l-kubra (The Royal Chamber of Santo Domingo) is a leisure room from the first period of Nasrid art. Scholars consider that the Chamber is of key importance for defining art during this period and a forerunner of what would subsequently become the palaces of the Alhambra in Granada. This paper presents a study of the materials and techniques used in the plasterwork, carried out before the monument was restored. The study began with a detailed examination of the plasterwork before samples of the more significant areas were selected from what was clearly part of the original work. The study of materials consisted in the identification of the pigments and binding media, as well as the base mortars. Conventional analysis methods were used: optical microscopy, scanning electron microscopy (SEM), and chromatographic methods (gas chromatography, GC and high-pressure liquid chromatography, HPLC) and X-ray diffraction (XRD). The data from material identification and a detailed study of the materials in situ defined the techniques employed and provided key data on Nasrid plasterwork. Very few studies have been made of the materials used in Hispano-Muslim plasterwork, especially in relation to this particular moment in history. [Copyright &y& Elsevier]