The triptych icon is a unique type of Coptic icon, that has rarely been studied before. The archaeometric investigation helps to reveal the triptych icons' importance, and composition of the pigment palette and to monitor the manifestations of deterioration to determine appropriate treatment. A triptych icon was chosen from the El-Surian monastery in Wadi El-Natron. Cracks, dimming, yellowing, and parts loss indicate aging processes and chemical interactions with environmental conditions. The examination techniques are used to determine the stratigraphy of the icon. The spectroscopic methods used were Raman spectroscopy (RS), Attenuated total reflectance Fourier transform infrared (ATR-FTIR), Scanning electron microscopy-energy dispersive Xray analysis (SEM-EDX), and X-ray diffraction (XRD), which have revealed the basic composition and characteristic bands of pigments and the type of protective varnishes applied. The painting technique was tempera style applied on Abies alba (Silver Fir) wood and cotton canvas, the ground layer was calcium carbonate mixed with animal glue. The medium of pigments was egg yolk. The icon also contained some pigments that were rarely combined with each other, such as Prussian blue, ultramarine, barium chromate, titanium dioxide, and cadmium yellow. The shellac was used as a varnish. Spectroscopic studies of pigments helped in the dating process and it was concluded that the icon dated back to the late 19th century.