Archaeological and Anthropological Sciences

, Volume 11, Issue 9, pp 4847–4872 | Cite as

Structural characterization and decontamination of dental calculus for ancient starch research

  • María Soto
  • Jamie Inwood
  • Siobhán Clarke
  • Alison Crowther
  • Danielle Covelli
  • Julien Favreau
  • Makarius Itambu
  • Steve Larter
  • Patrick Lee
  • Marina Lozano
  • Jason Maley
  • Aloyce Mwambwiga
  • Robert Patalano
  • Ramaswami Sammynaiken
  • Josep M Vergès
  • Jianfeng Zhu
  • Julio MercaderEmail author
Original Paper


Ancient dental calculus research currently relies on destructive techniques whereby archeological specimens are broken down to determine their contents. Two strategies that could partly remediate a permanent loss of the original sample and enhance future analysis and reproducibility include (1) structural surface characterization through spectroscopy along with crystallographic and spectroscopic analysis of its molecular structure, and (2) surface decontamination protocols in which the efficacy of cleaning dental calculus prior to extraction is demonstrated. Dental calculus provides ancient starch research a niche where granules may be adsorbed to minerals, coated, overgrown, entrapped, and/or protected from chemical degradation. While encapsulation offers protection from degradation, it does not shield the sample’s surface from contamination. The most common approach to retrieving microbotanical particles from archeological calculus has been the direct decalcification of the sample, after a cleaning stage variously consisting of immersion in water, acids, and mechanical dislodgment via gas, sonication, and/or toothbrushes. Little is known about the efficiency of these methods for a complete removal of sediment/soil and unrelated microbotanical matter. In this paper, controlled laboratory experimentation leads to chemical structural characterization and a decontamination protocol to eradicate starch granules. Several concentrations of acids, bases, and enzymes were tested at intervals to understand their potential to gelatinize and fully destroy starch granules; arriving at a procedure that effectively eradicates modern starch prior to dissolution without damaging the matrix or entrapped starch microremains. This is the first attempt at creating synthetic calculus to understand and systematically test effective decontamination protocols for ancient starch research.


Structural chemical characterization Raman XPS P-XRD Ancient dental calculus Ancient starch research Decontamination prior to decalcification Starch contamination 



This work was sponsored by the Canadian Social Sciences and Humanities Research Council under its Partnership Grant Program no. 895-2016-1017. The Saskatchewan Structural Sciences Centre (SSSC) is acknowledged for providing facilities to conduct this research. Canada Foundation for Innovation, Natural Sciences and Engineering Research Council of Canada and the University of Saskatchewan support research at the SSSC. The following Spanish institutions and grants made this work possible: MINECO/FEDER: CGL2015-65387-C03-1-P, Generalitat de Catalunya: 2017SGR1040 (URV: 2016PFR-URVB2-17). Junta de Castilla y León, and Fundación Atapuerca.


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  • María Soto
    • 1
  • Jamie Inwood
    • 1
  • Siobhán Clarke
    • 1
  • Alison Crowther
    • 2
    • 3
  • Danielle Covelli
    • 4
  • Julien Favreau
    • 1
  • Makarius Itambu
    • 1
    • 5
  • Steve Larter
    • 6
  • Patrick Lee
    • 1
    • 7
  • Marina Lozano
    • 8
  • Jason Maley
    • 4
  • Aloyce Mwambwiga
    • 1
    • 9
  • Robert Patalano
    • 1
  • Ramaswami Sammynaiken
    • 4
  • Josep M Vergès
    • 8
    • 10
  • Jianfeng Zhu
    • 4
  • Julio Mercader
    • 1
    Email author
  1. 1.Department of Anthropology and ArcheologyUniversity of CalgaryCalgaryCanada
  2. 2.School of Social ScienceThe University of QueenslandSt LuciaAustralia
  3. 3.Department of ArcheologyMax Planck Institute for the Science of Human HistoryJenaGermany
  4. 4.Saskatchewan Structural Sciences CentreUniversity of SaskatchewanSaskatoonCanada
  5. 5.Department of Archeology and Heritage StudiesUniversity of Dar es SalamDar es SalaamTanzania
  6. 6.Petroleum Reservoir Group (PRG), Department of GeoscienceUniversity of CalgaryCalgaryCanada
  7. 7.Department of AnthropologyUniversity of TorontoTorontoCanada
  8. 8.Institut Català de Paleoecologia Humana i Evolució Social (IPHES)TarragonaSpain
  9. 9.National Natural History MuseumArushaTanzania
  10. 10.Àrea de PrehistòriaUniversitat Rovira i VirgiliTarragonaSpain

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