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Instruments / Technical Area	Publication Details	Published
I11-High Resolution Powder Diffraction	Complementary analysis to de-convolute co-located contaminants in marine archaeological bricks Rebecca Grethe , Kevin J. W. Etherdo-Sibley , Chiu Tang , Sarah Day , Donna C. Arnold , Eleanor Schofield Journal Of Cultural Heritage 55, 221 - 227 DOI: 10.1016/j.culher.2022.02.013 Diamond Proposal Number(s): [24092] Open Access Show Abstract ▼ Abstract: Marine archaeological artefacts contain unexpected compounds due to prolonged exposure to the sea. These can remain dormant and embedded within materials until a change in their surrounding environment, such as exposure to oxygen, prompts a transformation. These changes can pose a problem, as acidic compounds are formed which disintegrate the material, or crystals form which physically break the artefact apart. The extent of these transformations is highly heterogeneous due to its dependence on the ability for oxygen to reach and catalyse these reactions. Additionally, these transformations are heavily dependent on the environment the artefact is exposed to, and the pathways available for ingress, either naturally or through previous degradation. This results in materials with a range of different compounds which are often co-located on the macro, micro and nano-scale. Trying to de-convolute these compounds is challenging, and usually requires a suite of complementary techniques to achieve. Here we report on damaging salts found within marine archaeological bricks and show how it is only possible to qualitatively and quantitatively understand what is present by employing a range of analytical techniques, such as XRD, SEM-EDS and SR-XPD. The marine archaeological bricks studied were found to contain a range of different sulfate-based salts, which had grown crystals in preferred orientations. This provides information which will guide further conservation strategies such as how these bricks are stored, conserved and protected in the future.	May 2022
B18-Core EXAFS	High-resolution non-invasive X-ray diffraction analysis of artists’ paints Craig I. Hiley , Graeme Hansford , Nicholas Eastaugh Journal Of Cultural Heritage 53, 1 - 13 DOI: 10.1016/j.culher.2021.10.008 Diamond Proposal Number(s): [18533, 23341] Show Abstract ▼ Abstract: Energy-dispersive X-ray diffraction (EDXRD) is extremely insensitive to sample morphology when implemented in a back-reflection geometry. The capabilities of this non-invasive technique for cultural heritage applications have been explored at high resolution at the Diamond Light Source synchrotron. The results of the XRD analysis of the pigments in 40 paints, commonly used by 20th century artists, are reported here. It was found that synthetic organic pigments yielded weak diffraction patterns at best, and it was not possible to unambiguously identify any of these pigments. In contrast, the majority of the paints containing inorganic pigments yielded good diffraction patterns amenable to crystallographic analysis. The high resolution of the technique enables the extraction of a range of detailed information: phase identification (including solid solutions), highly accurate unit cell parameters, phase quantification, crystallite size and strain parameters and preferred orientation parameters. The implications of these results for application to real paintings are discussed, along with the possibility to transfer the technique away from the synchrotron and into the laboratory and museum through the use of state-of-the-art microcalorimeter detectors. The results presented demonstrate the exciting potential of the technique for art history and authentication studies, based on the non-invasive acquisition of very high quality crystallographic data.	Nov 2021
I08-Scanning X-ray Microscopy beamline (SXM)	Investigation of the foil structure and corrosion mechanisms of modern Zwischgold using advanced analysis techniques Qing Wu , Karolina Soppa , Nadim Scherrer , Benjamin Watts , Tadahiro Yokosawa , Laetitia Bernard , Tohru Araki , Max Döbeli , Markus Meyer , Erdmann Spiecker , Rainer H. Fink Journal Of Cultural Heritage DOI: 10.1016/j.culher.2017.12.005 Diamond Proposal Number(s): [15595] Open Access Show Abstract ▼ Abstract: Zwischgold is a two-sided metal foil made by adhering a gold leaf over a silver leaf to present a gold surface while using less gold than gold foils. Corroded Zwischgold surfaces appear dark, accompanied by gloss loss and possible mechanical stability issues. Zwischgold applied artefacts are commonly found in museums and churches across Europe and they currently face an uncertain future as conservators have little knowledge to base conservation treatments on. We present a comprehensive material analysis of Zwischgold models through advanced characterization techniques including focused ion beam coupled with scanning electron microscopy (FIB-SEM), transmission electron microscopy (TEM), scanning transmission X-ray microscopy (STXM), time-of-flight secondary ion mass spectrometry (TOF-SIMS)and Rutherford backscattering spectrometry (RBS). Complementary information on the foil thickness,sharpness of the gold-silver interface, gold purity, and the formation as well as distribution of corrosion products on Zwischgold models have been obtained, representing a starting point for understanding themorphology and the long-term chemistry of Zwischgold artefacts.	Jan 2018
B18-Core EXAFS	Strontium carbonate nanoparticles for the surface treatment of problematic sulfur and iron in waterlogged archaeological wood Eleanor Schofield , Ritimukta Sarangi , Apurva Mehta , Mark Jones , Andrew Smith , Fred Mosselmans , Alan Chadwick Journal Of Cultural Heritage DOI: 10.1016/j.culher.2015.07.013 Diamond Proposal Number(s): [6437] Show Abstract ▼ Abstract: Stabilising waterlogged archaeological wooden artefacts for display presents a challenge for conservators and scientists. Sulfur compounds, incorporated into the wood prior to excavation, can lead to acid formation when exposed to oxygen, and in the presence of iron ions. Strontium carbonate nanoparticles have recently been shown to reduce the production of acid formation at the root by reacting with inorganic sulfur-containing compounds. Here, we show the feasibility of using this treatment on small samples where consolidating treatments have already been performed. It is found that PEG 200 does not prevent the reactivity of the nanoparticles with the sulfur compounds present in the artefacts. A surface brushing application method was found to be successful whilst retaining the visual integrity. In addition, it was found that this technique results in the leaching of iron from the surface layers, preventing future build up of acid catalysed by iron compounds.	Aug 2015

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