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Analytical and Bioanalytical Chemistry

, Volume 407, Issue 18, pp 5393–5403 | Cite as

Improving FTIR imaging speciation of organic compound residues or their degradation products in wall painting samples, by introducing a new thin section preparation strategy based on cyclododecane pre-treatment

  • Zoi Eirini Papliaka
  • Lisa Vaccari
  • Franco Zanini
  • Sophia Sotiropoulou
Research Paper

Abstract

Fourier transform infrared (FTIR) imaging in transmission mode, employing a bidimensional focal plane array (FPA) detector, was applied for the detection and spatially resolved chemical characterisation of organic compounds or their degradation products within the stratigraphy of a critical group of fragments, originating from prehistoric and roman wall paintings, containing a very low concentration of subsisted organic matter or its alteration products. Past analyses using attenuated total reflection (ATR) or reflection FTIR on polished cross sections failed to provide any evidence of any organic material assignable as binding medium of the original painting. In order to improve the method’s performance, in the present study, a new method of sample preparation in thin section was developed. The procedure is based on the use of cyclododecane C12H24 as embedding material and a subsequent double-side polishing of the specimen. Such procedure provides samples to be studied in FTIR transmission mode without losing the information on the spatial distribution of the detected materials in the paint stratigraphy. For comparison purposes, the same samples were also studied after opening their stratigraphy with a diamond anvil cell. Both preparation techniques offered high-quality chemical imaging of the decay products of an organic substance, giving clues to the painting technique. In addition, the thin sections resulting from the cyclododecane pre-treatment offered more layer-specific data, as the layer thickness and order remained unaffected, whereas the samples resulting from compression within the diamond cell were slightly deformed; however, since thinner and more homogenous, they provided higher spectral quality in terms of S/N ratio. In summary, the present study illustrates the appropriateness of FTIR imaging in transmission mode associated with a new thin section preparation strategy to detect and localise very low-concentrated organic matter subjected to deterioration processes, when the application of FTIR in reflection mode or FTIR-ATR fails to give any relevant information.

Graphical Abstract

Visible image of a thin section, C12H24 pre-treated, originating from prehistoric wall paintings at Akrotiri, Thera (Greece). FTIR images representing the spatial distribution of the consolidant, the minerals: wollastonite, riebeckite, and a proteinaceous binder. The size of the FTIR images is 170 × 340 μm2

Keywords

FTIR imaging Thin sections Organic binder Oxalates Carboxylates Conservation studies 

Supplementary material

216_2015_8698_MOESM1_ESM.pdf (1.7 mb)
ESM 1 (PDF 1698 kb)

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Copyright information

© Springer-Verlag Berlin Heidelberg 2015

Authors and Affiliations

  1. 1.Elettra Sincrotrone Trieste S.C.p.A.BasovizzaItaly
  2. 2.Art Diagnosis CenterOrmylia FoundationOrmyliaGreece
  3. 3.Institute of Electronic Structure and LaserFoundation for Research and Technology-Hellas (IESL-FORTH)HeraklionGreece

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