Fragments of painted limestone reliefs from the Palace of Apries in Upper Egypt excavated by Flinders Petrie in 1908–1910 have been investigated using visible-induced luminescence imaging, micro X-ray fluorescence, laser ablation inductively coupled plasma mass spectrometry, micro X-ray powder diffraction, and Fourier transform infrared spectrometry. The pigments have been mapped, and the use and previous reports of use of pigments are discussed. Mainly lead–antimonate yellow, lead–tin yellow, orpiment, atacamite, gypsum/anhydrite, and Egyptian blue have been detected. It is the first time that lead–antimonate yellow and lead–tin yellow have been identified in ancient Egyptian painting. In fact, this is the earliest examples known of both of these yellow pigments in the world.