This review describes advances in the XRF group of techniques published approximately between April 2015 and March 2016. Fundamental contributions in the instrumentation sections include the development of synchrotron radiation sources, semiconductor design technology and evaluating the quality of in situ hand-held XRF results. A bench top TXRF spectrometer for the measurement of the elements from carbon to uranium is described that offers achievable detection limits that range from ng g−1 to μg g−1. The applications sections aim to give a representative overview of the range of applications that use XRF techniques with an emphasis on papers that describe technical or application innovation. Sample size investigated ranged from the planet Mercury down to nano-gram quantities of cement secreted by settlement stage barnacle larvae. The archaeological and cultural heritage section this year includes an authentic report on the use of cannabis as a filler in ancient lime plaster and heartening news that the construction of an underground parking garage in the centre of Zurich (Switzerland) unearthed the remains of seven Neolithic settlements from the 4th and 3rd millennium BC. The X-ray excitation of iron present in ancient iron-gall inks was presented as a step toward the non-invasive reading of fragile and/or unopenable documents. Feedback from readers of this review is most welcome and the review coordinator may be contacted using the email address provided.

https://pubs.rsc.org/en/content/articlepdf/2021/ja/d1ja90033a

2016 Atomic Spectrometry Update – a review of advances in X-ray fluorescence spectrometry and its applications

Excavations at Tell Khaiber in southern Iraq by the Ur Region Archaeological Project have revealed a substantial building (hereafter the Public Building) dating to the mid-second millennium b.c. The results are significant for the light they shed on Babylonian provincial administration, particularly of food production, for revealing a previously unknown type of fortified monumental building, and for producing a dated archive, in context, of the little-understood Sealand Dynasty. The project also represents a return of British field archaeology to long-neglected Babylonia, in collaboration with Iraq's State Board for Antiquities and Heritage. Comments on the historical background and physical location of Tell Khaiber are followed by discussion of the form and function of the Public Building. Preliminary analysis of the associated archive provides insights into the social milieu of the time. Aspects of the material culture, including pottery, are also discussed.

/pdf/tell-khaiber-an-administrative-centre-of-the-sealand-period-4j4ztj6ts3.pdf

Tell Khaiber: An administrative centre of the Sealand period

This paper describes a protocol for quantification of heritage copper alloys by energy-dispersive X-ray fluorescence spectroscopy (ED-XRF). The protocol, nicknamed CHARMed PyMca, is designed for users who wish to maximize inter-laboratory reproducibility of quantitative ED-XRF results for the wide range of copper alloys found in heritage materials. By maximizing reproducibility, this protocol should facilitate collaboration and allow the rigorous use of shared data and databases. The protocol uses free, open-source, fundamental parameters software called PyMca. PyMca allows for a consistent and transparent application of the fundamental parameters approach independent of the ED-XRF instrumentation used. The proposed protocol calls for calibration of standardless PyMca results against a set of certified reference materials designed specifically for use with heritage copper alloys, the so-called copper CHARM set. Finally, this protocol calls for the calibration-to-standards to be carried out following a consistent strategy, including error modelling and the incorporation of a validation procedure. A reproducibility study was conducted using CHARMed PyMca and eight different ED-XRF instruments of six different types. In comparison to a 2010 study conducted according to the same method, CHARMed PyMca showed a dramatic improvement in reproducibility and method sensitivity.

https://hal.archives-ouvertes.fr/hal-01692157/document

CHARMed PyMca, Part I: A Protocol for Improved Inter-laboratory Reproducibility in the Quantitative ED-XRF Analysis of Copper Alloys

Ancient Egyptian mummies were often covered with an outer casing, panels and masks made from cartonnage: a lightweight material made from linen, plaster, and recycled papyrus held together with adhesive. Egyptologists, papyrologists, and historians aim to recover and read extant text on the papyrus contained within cartonnage layers, but some methods, such as dissolving mummy casings, are destructive. The use of an advanced range of different imaging modalities was investigated to test the feasibility of non-destructive approaches applied to multi-layered papyrus found in ancient Egyptian mummy cartonnage. Eight different techniques were compared by imaging four synthetic phantoms designed to provide robust, well-understood, yet relevant sample standards using modern papyrus and replica inks. The techniques include optical (multispectral imaging with reflection and transillumination, and optical coherence tomography), X-ray (X-ray fluorescence imaging, X-ray fluorescence spectroscopy, X-ray micro computed tomography and phase contrast X-ray) and terahertz-based approaches. Optical imaging techniques were able to detect inks on all four phantoms, but were unable to significantly penetrate papyrus. X-ray-based techniques were sensitive to iron-based inks with excellent penetration but were not able to detect carbon-based inks. However, using terahertz imaging, it was possible to detect carbon-based inks with good penetration but with less sensitivity to iron-based inks. The phantoms allowed reliable and repeatable tests to be made at multiple sites on three continents. The tests demonstrated that each imaging modality needs to be optimised for this particular application: it is, in general, not sufficient to repurpose an existing device without modification. Furthermore, it is likely that no single imaging technique will to be able to robustly detect and enable the reading of text within ancient Egyptian mummy cartonnage. However, by carefully selecting, optimising and combining techniques, text contained within these fragile and rare artefacts may eventually be open to non-destructive imaging, identification, and interpretation.

/pdf/an-assessment-of-multimodal-imaging-of-subsurface-text-in-1dh1x1sxpv.pdf

An assessment of multimodal imaging of subsurface text in mummy cartonnage using surrogate papyrus phantoms

This paper argues that portable X-ray fluorescence spectrometry (pXRF) is a suitable elemental measurement technique to study the production of copper-alloy artefacts. However, rather than try to imitate the accuracy and precision of laboratory techniques, it is more beneficial to deploy it in a survey role, one that attempts to model chronological and geographical changes within large quantities of artefacts. To achieve this, it was investigated to what extent corrosion and the issues surrounding surface measurements affect the potential of this type of research. Analyses on early Roman period brooches gathered in the Nijmegen region of the Netherlands were subsequently compared with published data.

/pdf/non-destructive-survey-of-early-roman-copper-alloy-brooches-36mvtjjmkj.pdf

Non-Destructive Survey of Early Roman Copper-Alloy Brooches using Portable X-ray Fluorescence Spectrometry

This paper introduces a new set of certified reference materials designed to aid scientists and conservators working in cultural heritage fields with quantitative X-ray fluorescence analysis of historical and prehistoric copper alloys. This set has been designated as the Copper CHARM Set (Cultural Heritage Alloy Reference Material Set). The Copper CHARM Set is designed to be used by a wide range of museum-, art- and archaeology-oriented scientists and conservators to help improve the accuracy and range of their calibrations for quantitative ED–XRF spectrometry of copper alloys, and also increase the number of elements that can routinely be quantified. In addition, the common use of a single core set of the reference materials is designed to significantly improve inter-laboratory reproducibility, allowing greater data sharing between researchers and thus furthering possibilities for collaborative study.

The Copper CHARM Set: A New Set of Certified Reference Materials for the Standardization of Quantitative X‐Ray Fluorescence Analysis of Heritage Copper Alloys*

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The Copper CHARM Set: A New Set of Certified Reference Materials for the Standardization of Quantitative X‐Ray Fluorescence Analysis of Heritage Copper Alloys*