Archaeological and Anthropological Sciences

, Volume 11, Issue 12, pp 6803–6827 | Cite as

Documenting the degradation of animal-tissue residues on experimental stone tools: a multi-analytical approach

  • Gilliane MonnierEmail author
  • Kaitlyn May
Original Paper


In lithic residue analysis, the identification of degraded animal tissues on stone tools is challenging due to many factors, not least of which is the fact that residues are complex, heterogeneous mixtures of many different kinds of molecules. In order to aid in their identification, a reference library of infrared spectra of residues collected using Fourier-transform infrared microspectroscopy (FTIRM) has recently been published (Monnier et al J Archaeol Sci: Rep 18:806–823, 2018). The goal of the present study is to explore the effects of decomposition on residues. Accordingly, we buried flakes with residues in compost for 1 year, then excavated them and documented both their appearance (using visible-light microscopy (VLM) and scanning electron microscopy (SEM)) and molecular composition (using FTIRM). The results show that while some residues (like meat and blood) disappeared entirely, others (fat and skin) were preserved on the bottoms of flakes buried in deep layers within the compost. Although the residues were damaged by microbial activity, their FTIRM spectra were clearly interpretable. Residues containing hydroxyapatite (bone and fish scales) and keratin (feather barbules, hair, and skin) were relatively well preserved. Their structures were in many cases recognizable, and their FTIRM spectra were entirely consistent with the FTIRM spectra of the standards. The results of the experiment show that the decay of animal tissues in compost proceeds primarily as a result of microbial activity, which appears to remove the tissues before they have a chance to oxidize or experience other biochemical changes. We conclude that if ancient residues have not been removed by microbial action, they can be identified using FTIR standards based upon fresh residues, such as those published in Monnier et al J Archaeol Sci 78:158–178, (2017), Monnier et al. 2018, J Archaeol Method Theory 25(1):1-44.


Residue analysis FTIR microspectroscopy SEM Stone tools Residue degradation 



This work was funded by NSF grant # BCS-1420702. It was carried out at the University of Minnesota in the Evolutionary Anthropology Laboratories (College of Liberal Arts); at the Advanced Imaging Service for Objects and Spaces (AISOS) in the College of Liberal Arts; at the Characterization Facility (College of Science and Engineering), which receives partial support from the NSF through the MRSEC program; and at LacCore: National Lacustrine Core Facility (College of Science and Engineering), which receives partial support from the NSF. We wish to thank the many people at these centers who helped us along the way: Gil Tostevin, Matt Edling, Samantha Porter, Colin McFadden, Bing Luo, Kristina Brady Shannon, and Amy Myrbo. Many thanks go to Edward Idarraga for his help with the figures, and we thank two anonymous reviewers for their helpful comments.

Author roles

The study was designed and implemented by GM; photographs, VLM images, and SEM images were collected by GM and KM; FTIRM spectra were collected by GM; data analysis, manuscript writing, and figures were accomplished by GM.

Supplementary material

12520_2019_941_MOESM1_ESM.pdf (880 kb)
ESM 1 (PDF 880 kb)


  1. Anderson PC (1980) A testimony of prehistoric tasks: diagnostic residues on stone tool working edges. World Archaeol 12:181–193CrossRefGoogle Scholar
  2. Bordes L, Prinsloo LC, Fullagar R, Sutikna T, Hayes E, Jatmiko, Wahyu Saptomo E, Tocheri M, Roberts RG (2017) Viability of Raman microscopy to identify micro-residues related to tool-use and modern contaminants on prehistoric stone artefacts. J Raman Spectrosc 48(9):1212–1221. CrossRefGoogle Scholar
  3. Bordes L, Fullagar R, Prinsloo LC, Hayes E, Kozlikin MB, Shunkov MV, Derevianko AP, Roberts RG (2018) Raman spectroscopy of lipid micro-residues on Middle Palaeolithic stone tools from Denisova Cave, Siberia. J Archaeol Sci 95(July):52–63. CrossRefGoogle Scholar
  4. Borel A, Olle A, Maria Verges J, Sala R (2014) Scanning electron and optical light microscopy: two complementary approaches for the understanding and interpretation of usewear and residues on stone tools. J Archaeol Sci 48:46–59. CrossRefGoogle Scholar
  5. Cesaro SN, Lemorini C (2012) The function of prehistoric lithic tools: a combined study of use-wear analysis and FTIR microspectroscopy. Spectrochim Acta Part A Mol Biomol Spectrosc 86:299–304. CrossRefGoogle Scholar
  6. Charrie-Duhaut A, Porraz G, Cartwright CR, Igreja M, Connan J, Poggenpoel C, Texier P-J (2013) First molecular identification of a hafting adhesive in the Late Howiesons Poort at Diepkloof Rock Shelter (Western Cape, South Africa). J Archaeol Sci 40(9):3506–3518. CrossRefGoogle Scholar
  7. Croft S, Chatzipanagis K, Kröger R, & Milner N (2018) Misleading residues on lithics from Star Carr: Identification with Raman microspectroscopy. Journal of Archaeological Science: Reports 19(November 2017):430–438. CrossRefGoogle Scholar
  8. Croft S, Monnier G, Radini A, Little A, Milner N (2016) Lithic residue survival and characterisation at star carr: a burial experiment. Internet Archaeol (42).
  9. Forbes SL, Dent BB, Stuart BH (2005). The effect of soil type on adipocere formation. Forensic Sci Int (154):35–43.CrossRefGoogle Scholar
  10. Forbes SL, Stuart BH, Dent BB (2005b) The effect of the burial environment on adipocere formation. Forensic Sci Int 154(1):24–34. CrossRefGoogle Scholar
  11. Hayes E, Rots V (2018) Documenting scarce and fragmented residues on stone tools: an experimental approach using optical microscopy and SEM-EDS. Archaeol Anthropol Sci 11:3065–3099. CrossRefGoogle Scholar
  12. Hayes E, Cnuts D, & Rots V. (2019). Integrating SEM-EDS in a sequential residue analysis protocol: benefits and challenges. J Archaeol Sci Rep, 23(August 2018), 116–126. CrossRefGoogle Scholar
  13. Heaton K, Solazzo C, Collins MJ, Thomas-Oates J, Bergström ET (2009) Towards the application of desorption electrospray ionisation mass spectrometry (DESI-MS) to the analysis of ancient proteins from artefacts. J Archaeol Sci 36(10):2145–2154. CrossRefGoogle Scholar
  14. Hortola P (2001) Experimental SEM determination of game mammalian bloodstains on stone tools. Environ Archaeol 6:97–102CrossRefGoogle Scholar
  15. Jahren AH, Toth N, Schick K, Clark JD, Amundson RG (1997) Determining stone tool use: chemical and morphological analyses of residues on experimentally manufactured stone tools. J Archaeol Sci 24:245–250CrossRefGoogle Scholar
  16. Lange L, Huang Y, Busk PK (2016) Microbial decomposition of keratin in nature—a new hypothesis of industrial relevance. Appl Microbiol Biotechnol 100(5):2083–2096. CrossRefGoogle Scholar
  17. Langejans GHJ (2010) Remains of the day-preservation of organic micro-residues on stone tools. J Archaeol Sci 37(5):971–985. CrossRefGoogle Scholar
  18. Lynch V, Miotti L (2017) Introduction to micro-residues analysis: systematic use of scanning electron microscope and energy dispersive X-rays spectroscopy (SEM-EDX) on Patagonian raw materials. J Archaeol Sci Rep 16:299–308Google Scholar
  19. Monnier GF (2018) A review of infrared spectroscopy in microarchaeology: methods, applications, and recent trends. J Archaeol Sci Rep 18(November 2017):806–823. CrossRefGoogle Scholar
  20. Monnier GF, Ladwig JL, Porter ST (2012) Swept under the rug: the problem of unacknowledged ambiguity in lithic residue identification. J Archaeol Sci 39(10):3284–3300. CrossRefGoogle Scholar
  21. Monnier GF, Hauck TC, Feinberg JM, Luo B, Le Tensorer J-M, al Sakhel H (2013) A multi-analytical methodology of lithic residue analysis applied to Paleolithic tools from Hummal, Syria. J Archaeol Sci 40(10):3722–3739. CrossRefGoogle Scholar
  22. Monnier G, Frahm E, Luo B, Missal K (2017) Developing FTIR microspectroscopy for analysis of plant residues on stone tools. J Archaeol Sci 78:158–178. CrossRefGoogle Scholar
  23. Monnier G, Frahm E, Luo B, Missal K (2018) Developing FTIR microspectroscopy for the analysis of animal-tissue residues on stone tools. J Archaeol Method Theory 25(1):1–44. CrossRefGoogle Scholar
  24. Olsen SL (1988) Scanning electron microscopy in archaeology. BAR International Series, Oxford, p 452Google Scholar
  25. Pawlik AF (2004). Identification of hafting traces and residues by scanning electron microscopy and energy-dispersive analysis of X-rays. In Walker EA, Wenban-Smith F, & Healy F (eds.), Lithics in action: papers from the Conference Lithic Studies in the Year 2000, Oxbow Books, pp. 169–182Google Scholar
  26. Pedergnana A, Ollé A (2018) Building an experimental comparative reference collection for lithic micro-residue analysis based on a multi-analytical approach. J Archaeol Method Theory 25(1):117–154. CrossRefGoogle Scholar
  27. Pedergnana A, Asryan L, Fernández-Marchena JL, Ollé A (2016) Modern contaminants affecting microscopic residue analysis on stone tools: a word of caution. Micron 86:1–21CrossRefGoogle Scholar
  28. Perrault K, Stefanuto P-H, Dubois L, Cnuts D, Rots V, Focant J-F (2016) A new approach for the characterization of organic residues from stone tools using GC × GC-TOFMS. Separations 3(2):16. CrossRefGoogle Scholar
  29. Prinsloo LC, Wadley L, Lombard M (2014) Infrared reflectance spectroscopy as an analytical technique for the study of residues on stone tools: potential and challenges. J Archaeol Sci 41:732–739. CrossRefGoogle Scholar
  30. Solodenko N, Zupancich A, Cesaro SN, Marder O, Lemorini C, Barkai R (2015) Fat residue and use-wear found on Acheulian biface and scraper associated with butchered elephant remains at the site of Revadim, Israel. PLoS One 10(3):UNSP e0118572. CrossRefGoogle Scholar
  31. Stephenson B (2015) A modified Picro-Sirius Red (PSR) staining procedure with polarization microscopy for identifying collagen in archaeological residues. J Archaeol Sci 61:235–243. CrossRefGoogle Scholar
  32. Verges JM, Olle A (2011) Technical microwear and residues in identifying bipolar knapping on an anvil: experimental data. J Archaeol Sci 38(5):1016–1025. CrossRefGoogle Scholar
  33. Wadley L, Lombard M, Williamson B (2004) The first residue analysis blind tests: results and lessons learnt. J Archaeol Sci 31(11):1491–1501. CrossRefGoogle Scholar
  34. Weiner S (2010) Microarchaeology: beyond the visible archaeological record. Cambridge University Press, CambridgeCrossRefGoogle Scholar
  35. Zupancich A, Nunziante-Cesaro S, Blasco R, Rosell J, Cristiani E, Venditti F, Lemorini C, Barkai R, Gopher A (2016) Early evidence of stone tool use in bone working activities at Qesem Cave Israel. Sci Rep 6(October):37686. CrossRefGoogle Scholar

Copyright information

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

Authors and Affiliations

  1. 1.Department of AnthropologyUniversity of MinnesotaMinneapolisUSA

Personalised recommendations