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Chemical Mapping of Ancient Artifacts and Fossils with X-Ray Spectroscopy

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Chemical Mapping of Ancient Artifacts and Fossils with X-Ray Spectroscopy Chemical Mapping of Ancient Artifacts and Fossils with X-Ray Spectroscopy Uwe Bergmann, Loïc Bertrand, Nicholas P. Edwards, Phillip L. Manning, and Roy A. Wogelius Contents Introduction.................................................................. 2 Synchrotron-Rapid-Scanning X-ray Fluorescence (SRS-XRF) Imaging: Elemental Mapping............................................................ 4 The Principle of X-Ray Fluorescence........................................... 13 Elemental Mapping Using XRF................................................ 15 Synchrotron-Rapid-Scanning XRF Imaging of Large Objects........................ 16 X-Ray Absorption Spectroscopy: Chemical Speciation Analysis ....................... 20 Combining XAS and SRS-XRF Imaging: Speciation Analysis and Mapping.............. 22 X-Ray Raman Scattering: Carbon Speciation Analysis and Imaging .................... 24 XRS-Based 2D Speciation Mapping............................................ 28 Uncovering Ancient Writings by SRS-XRF........................................ 30 The Archimedes Palimpsest ................................................... 30 The Quran¯ Palimpsest....................................................... 36 Luigi Cherubini’s Opera Médée................................................ 37 The Syriac Galen Palimpsest.................................................. 39 U. Bergmann () Stanford PULSE Institute, SLAC National Accelerator Laboratory, Menlo Park, CA, USA e-mail: [email protected] L. Bertrand IPANEMA CNRS MIC UVSQ, Université Paris-Saclay, Gif-sur-Yvette, France Synchrotron SOLEIL, Gif-sur-Yvette, France e-mail: [email protected] N. P. Edwards Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, CA, USA e-mail: [email protected] P. L. Manning · R. A. Wogelius School of Earth and Environmental Sciences, Interdisciplinary Centre for Ancient Life, University of Manchester, Manchester, UK e-mail: [email protected]; [email protected] © Springer Nature Switzerland AG 2019 1 E. J. Jaeschke et al. (eds.), Synchrotron Light Sources and Free-Electron Lasers, https://doi.org/10.1007/978-3-319-04507-8_77-1 2U.Bergmannetal. SRS-XRF Imaging of Paleontological Material..................................... 39 Darwin’s Bird: Archaeopteryx................................................. 40 Modern (Extant) Feathers..................................................... 49 Conclusion................................................................... 52 References................................................................... 54 Special References (Websites)................................................. 63 Abstract The use of synchrotron radiation for the study of ancient objects has seen a significant increase over the last decade. Many of the major synchrotrons now have expertise and instrumentation that are specialized for the study of ancient objects. After giving an overview of these capabilities in the introduction, we focus in this chapter on synchrotron-rapid-scanning X-ray fluorescence (SRS-XRF) imaging of large objects to uncover ancient writings and chemical preservation in fossils. We will also describe the applications of X-ray absorption spectroscopy and new developments in X-ray Raman scattering, which are used to complement SRS-XRF mapping. Keywords Ancient materials · Ancient writings · Cultural heritage · Paleontology · Fossils · Archimedes Palimpsest · Archaeopteryx · Synchrotron radiation · X-ray fluorescence imaging · X-ray absorption spectroscopy · X-ray Raman scattering Introduction Ancient objects that comprise our planet’s natural and cultural heritage provide evidence upon which we reconstruct our past and help us understand the present, but critically such hindsight yields also insight to our future. Objects studied at synchrotron light sources range widely in size (only constrained by experimental parameters), composition, and complexity. While in some cases there might be a very clear line of enquiry, often the questions are less well-defined or are a function of resulting data. It is rare that one tool alone can interrogate multiple lines of enquiry. However, it has become clear over the last decade that synchrotron radiation, with its wide variety of unique techniques, is a powerful tool in the study of ancient materials. Synchrotron-based imaging has critically contributed to answering some of the core questions that had remained unanswerable for many ancient objects. Taking advantage of synchrotron radiation’s high brightness, small beam size, energy tunability, monochromaticity, polarization, and coherence, scientists have developed an array of techniques that provide structural and chemical information from sub-Ångströms to decimeter scales. As synchrotron facilities have dramatically improved over the first half century of operations, the research performed at these facilities has evolved and adapted Chemical Mapping of Ancient Artifacts and Fossils with X-Ray Spectroscopy 3 to uncountable disciplinary niches. Synchrotron facilities are now among the most interdisciplinary research facilities in existence, and the study of ancient objects alone crosses multiple disciplines in both the natural sciences and humanities. Whether the question is in archaeology, paleontology, paleoanthropology, or the many disciplines that comprise the history community, synchrotron radiation might provide an answer. In addition to the dramatic increase in beam performance at synchrotrons, work on ancient materials has also benefited from advances in instrumentation and, importantly, more user-/sample-friendly interface, intuitive operation, and coupling with laboratory instrumentation. These improvements and the expertise of large interdisciplinary teams have made it less daunting to carry out a synchrotron experiment on precious heritage objects. The growing number of publications and reciprocal growth of synchrotron beam lines and instruments adapted or specialized in the study of ancient materials well illustrates this trend. A comprehensive review of the development and trends in synchrotron studies of ancient and historical materials was produced by Bertrand et al. (2012), where a de- tailed and illustrated description of synchrotron techniques is provided. This chapter also includes a discussion of new approaches, the combination of characterization techniques, and the prevention/mitigation of radiation damage (see also Bertrand et al. 2015). They conclude with perspectives on specific support at synchrotron facilities for conducting studies of ancient materials. In this chapter, we focus on a much narrower topic, namely, the application of synchrotron-rapid-scanning X-ray fluorescence (SRS-XRF) imaging as well as X-ray absorption spectroscopy (XAS) and X-ray Raman scattering (XRS) that can obtain elemental maps and chemical speciation of relatively large (decimeter scale) objects. We will describe basic concepts and explore the practical consider- ations of the instrumentation while reviewing some of our work undertaken over the last decade. It is our aim that this information will inspire the creation of interdisciplinary teams that can tackle some of the most exciting and unsolved questions centered on ancient materials. In addition to the X-ray imaging and data scientists, these teams might include conservation scientists, scholars, curators, historians, archaeologists, and paleontologists, who might be neither familiar with nor interested in synchrotron radiation per se. In addition, the long-term behavior of ancient materials raises a range of questions that may inspire modern research in material science (Bertrand et al. 2018). To provide a more general overview that shows how far this field has advanced in recent years, we present here a list of techniques, parameters, and beamlines that are currently configured to study ancient materials and objects. Most generally, the techniques and information they provide can be categorized as follows: • X-ray fluorescence (XRF) and micro-XRF (μXRF) – elemental composition and spatial mapping in the μm to cm range depending on the object size • X-ray fluorescence micro-computed tomography (XRF-μCT) – 3D imaging of material elemental composition • X-ray absorption spectroscopy (XAS) – element-specific chemical speciation 4U.Bergmannetal. • X-ray Raman scattering (XRS) – bulk-sensitive chemical speciation of low-Z objects • X-ray diffraction (XRD) – atomic scale structure information and texture of objects with crystalline phases • Wide-angle X-ray scattering (WAXS) – atomic scale spatial information of noncrystalline systems • Small angle X-ray scattering (SAXS) – mesoscale spatial information of non- crystalline systems • X-ray micro- and nano-computed tomography (μCT, nCT) – 3D morphologi- cal/spatial information with resolutions ranging from submicrometer to ∼20 nm • X-ray phase-contrast computed tomography (PCCT) – 3D morphological/spatial information of low contrast objects with varying resolution, typically in the few μm range depending on the size of the object • X-ray-excited optical luminescence (XEOL) – chemical speciation • Differential phase contrast imaging (DPC) – 3D morphological/spatial informa- tion that enhances small changes in density • Ptychography (Bragg, reflection, near-field, focused probe, single aperture, and imaging ptychography) – nanometric scale 2D and 3D full-field imaging • Photoluminescence spectroscopy and imaging – identification and imaging
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