AbstractThe FT‐Raman vibrational spectrum of a child's deciduous exfoliated tooth has been analysed and the spectral features assigned to hydroxyapatite and protein. Comparisons made with older teeth from a Romano‐British burial site (∼ 2k years) and fossilised animal teeth (∼ 1 M‐70 M years) indicate that the organic protein component has disappeared with interment, whereas spectroscopic features due to the inorganic phosphatic matrix are common to all samples, modern and ancient. The application of the technique to the non‐destructive analysis of archaeological samples and the recording of spectra from interred samples without detriment from fluorescent material is demonstrated. © 1995 John Wiley & Sons, Inc.