Archaeological Bone from Macro- to Nanoscale: Heat-Induced Modifications at Low Temperatures
The present work focuses on the characterization of structural modifications in bone material induced by heating at low temperatures (90 - 250°C). This is of outmost importance when archaeological bone material is concerned. Changes occurring in the structure of the type I collagen and of the mineral-organic arrangement are especially investigated. This precise characterization required the combination of complementary analytical techniques: Differential Scanning Calorimetry (DSC) for global analysis of the collagen state of conservation, Scanning Electron Microscopy coupled with an Energy Dispersive X-Ray system (SEM-EDX), micro-Proton-Induced X-ray and Gamma-ray Emission (micro-PIXE/PIGE) for chemical analysis of the mineral fraction, Infrared microspectroscopy in attenuated total reflectance mode (micro-ATR-FT-IR) combined with curve-fitting for microscopic investigations and Transmission Electron Microscopy (TEM) on ultrathin sections to characterize the modifications in the mineral/organic interface at nanoscale. New criteria characterizing the effect of a thermal treatment at low temperatures on the bone structure from the macroscopic to the nanoscale were determined. There are namely a broadening of the Haversian canals, the inversion of the turns to -sheet ratio in the collagen structure determined by decomposition of the amide I IR band as well as a shift of amide II IR band position with the heating temperature to lower wavenumbers. At nanoscale, melting of the organic phase and clustering of hydroxyapatite (HAP) bone crystals can be observed. For comparison, unheated archaeological bones have been analyzed in order to test if the heat-induced modification can be distinguished from diagenetic alterations, generally dissolution-recrystallisation processes, in soils.
C. Chadefaux and I. Reiche, "Archaeological Bone from Macro- to Nanoscale: Heat-Induced Modifications at Low Temperatures", Journal of Nano Research, Vol. 8, pp. 157-172, 2009