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. 2021 Jan 14;11(1):1361.
doi: 10.1038/s41598-020-80462-3.

Profiling of human burned bones: oxidising versus reducing conditions

M P M Marques  1   2 , D Gonçalves  3   4   5 , A P Mamede  1 , T Coutinho  2 , E Cunha  2   3 , W Kockelmann  6 , S F Parker  6 , L A E Batista de Carvalho  7
Affiliations

Profiling of human burned bones: oxidising versus reducing conditions

M P M Marques et al. Sci Rep. .

Abstract

Complementary optical and neutron-based vibrational spectroscopy techniques (Infrared, Raman and inelastic neutron scattering) were applied to the study of human bones (femur and humerus) burned simultaneously under either aerobic or anaerobic conditions, in a wide range of temperatures (400 to 1000 °C). This is the first INS study of human skeletal remains heated in an oxygen-deprived atmosphere. Clear differences were observed between both types of samples, namely the absence of hydroxyapatite's OH vibrational bands in bone burned anaerobically (in unsealed containers), coupled to the presence of cyanamide (NCNH2) and portlandite (Ca(OH)2) in these reductive conditions. These results are expected to allow a better understanding of the heat effect on bone´s constituents in distinct environmental settings, thus contributing for an accurate characterisation of both forensic and archaeological human skeletal remains found in distinct scenarios regarding oxygen availability.

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Conflict of interest statement

The authors declare no competing interests.

Figures

Figure 1
Figure 1
Experimental setups for the burning process of human bone samples under controlled anaerobic conditions: (A) Ansealed—each bone fragment was placed inside a home-made steel airtight chamber (I) which was vacuum-pumped (II) and then inserted into an electric muffle furnace for heating at defined temperatures (at the University of Coimbra, Portugal); (B) Anunsealed—each powdered bone sample was placed into a vanadium container (I) with a perforated lid (allowing volatiles venting), that was inserted into the instrument furnace (II), under vacuum, and heated at defined temperatures (GEM instrument, at the ISIS Facility, United Kingdom).
Figure 2
Figure 2
Human bone samples currently analysed, showing the colour changes according to the burning conditions—aerobic or anaerobic in a sealed chamber (Ansealed).
Figure 3
Figure 3
FTIR-ATR (A) and INS spectra (measured in MAPS, with 2024 cm−1 incident energy) (B) of human femur burned at 1000 °C under anaerobic/unsealed (Anunsealed, brown), anaerobic/sealed (Ansealed, red) and aerobic (A, blue) conditions.
Figure 4
Figure 4
(A) INS (measured in TOSCA), FTIR-ATR and Raman spectra of reference calcium hydroxyapatite (SRM 2910b, HAp)—unburned (Unb, green), and burned at 1000 °C under aerobic (A, blue) and anaerobic/unsealed conditions (Anunsealed, brown); (B) INS spectra (measured in TOSCA) for human femur, unburned (Unb, green) and burned at 1000 °C under anaerobic/unsealed (Anunsealed, brown), anaerobic/sealed (Ansealed, red) and aerobic (A, blue) conditions.
Figure 5
Figure 5
FTIR-ATR spectra (400–2000 cm−1) of human humerus burned at different temperatures (400 to 1000 ° °C) either under aerobic (A) or anaerobic/sealed (Ansealed) conditions. The insert shows a magnification of the phosphate and OH librational bands from hydroxyapatite.
Figure 6
Figure 6
INS spectra of human femur burned at different temperatures (600 to 800 °C) either under aerobic (A) or anaerobic/sealed (Ansealed) conditions. (A) Data measured in TOSCA; (B) Data measured in MAPS (with 2024 cm−1 incident energy).
Figure 7
Figure 7
Temperature dependence of the INS hydroxyapatite´s hydroxyl libration for human femur: (A) burned under anaerobic/sealed conditions (data measured in MAPS, with 2024 cm−1 incident energy); (B) burned under aerobic conditions (data measured in TOSCA).
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