Diagenetic alteration to archaeological bone can cause significant disruption to both the biogenic mineral structure and the preservation of biomolecular resources such as protein and DNA over archaeological time. We report here the use of a technique, small-angle X-ray scattering, which makes it possible to examine the alteration to the mineral surface due to diagenesis. This method has previously been applied to archaeological bone thin sections, but has been modified in this case for use on bone powder as a high-throughput screening technique for bone preservation. Our results show that mineral structural change is not necessarily reflected in the currently used methods of measuring lattice perfection, and that the preservation of archaeological biomolecules may be linked to structural alteration as much as to crystallinity.