INS measurements were performed at the ISIS Neutron and Muon Source of the Rutherford Appleton Laboratory (UK) using the high-resolution MAPS and TOSCA spectrometers (29, 30). The instruments are complementary, as explained elsewhere (30). For the present case, the key differences are that TOSCA provides high-resolution spectra for the range of 0 to 2000 cm−1, while MAPS enables access to the C─H and O─H stretch regions. The bone samples were fixed onto (4 cm by 5 cm) flat Al cans with Al tape and wrapped in aluminum foil (fig. S1)—2 to 5 g for the intact archaeological bones and ca. 5 g for each reference sample, which was previously found to be an optimal amount (16). To reduce the impact of the Debye-Waller factor on the observed spectral intensity, the samples were cooled to cryogenic temperatures (ca. 5 to 10 K). Data on MAPS were recorded in the energy range of 0 to 5000 cm−1 using three incident energies (5240, 2024, and 968 cm−1). For both instruments, the neutron data were reduced to energy transfer spectra using the MANTID software (version 3.4.0) (31). In addition, a spectrum of reference HAp was measured {highly crystalline, stoichiometric calcium hydroxyapatite, [Ca10(PO4)6(OH)2,Ca/P = 1.67], SRM 2910b, from NIST, Gaithersburg, MA, USA} (32).

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