XRF Boot Camp Lite (August 2020)

Includes a Live Event on 08/14/2020 at 1:00 PM (EDT)

August 14, 1:00 - 3:00 p.m. EDT, Online
Virtual Annual Meeting Workshop
Instructors:
Aniko Bezur, Lynn Lee, Maggi Loubser, Karen Trentelman

X-ray fluorescence spectroscopy (XRF) has become a widely used analytical technique in the cultural heritage field due to the availability of relatively inexpensive, easy to use, and portable instruments. As a result an increasing number of institutions have acquired instrumentation in recent years, but the scientific background of the personnel charged with its use varies considerably and available training from the instrument sales representatives (ranging from several hours to up to two days) is typically insufficient and/or not available when new staff are hired. The Getty Conservation Institute (GCI) and Yale Institute for the Preservation of Cultural Heritage (IPCH) created the XRF Boot Camp for Conservators course to help address this training gap. This workshop will touch on some of the major concepts covered in the Boot Camp and will focus on how to use a newly available book, “Handheld XRF in Cultural Heritage: A Practical Workbook for Conservators”, as a self-guided learning resource.

Intended for new as well as seasoned XRF users, this workshop will introduce important fundamental concepts include demonstrations of workbook exercises, discussion of practical application of XRF to cultural heritage objects, and general guidance for spectral interpretation and potential pitfalls. Participants will be able to download XRF spectra used in the workbook along with open access software to facilitate engagement with the materials presented during workshop. 

"Handheld XRF in Cultural Heritage: A Practical Workbook for Conservators" is available from the GCI website as a free, downloadable PDF.

The book can also be ordered for print-on-demand (delivery approximately 2 weeks within the US).

Aniko Bezur

Anikó Bezur, the Wallace S. Wilson Director of Scientific Research at the Yale Institute for the Preservation of Cultural Heritage, has over 17 years of experience with the application of x-ray fluorescence spectroscopy to the study of cultural heritage objects. She was assistant professor in conservation science at the Art Conservation Department, Buffalo State College and adjunct professor in the Chemistry Department at Rice University. Anikó was involved in the conceptualization, organization and teaching of the XRF Boot Camp since its inception in 2011.

Lynn Lee

Lynn Lee is an Assistant Scientist at the Getty Conservation Institute. She is a point person at the GCI for handheld XRF (hhXRF), and has taught hhXRF to conservators at various museums. She was an instructor for a short course on XRF at the Denver X-ray Conference (2018, 2019) and an invited speaker at the conference (2019). Lynn was involved in the conceptualization, organization and teaching of the XRF Boot Camp since its inception in 2011.

Maggi Loubser

Maggi Loubser is currently the program manager and senior lecturer in the Tangible Heritage Conservation program at the University of Pretoria (South Africa). Her teaching responsibilities include leading the science curriculum for students with a humanities background. She has been an instructor for the XRF Boot Camp since 2013, and has taught the annual XRF Short Course at Western University (London, Canada) since 2005. Her background in XRF includes over thirty years of experience in academia and industry.

Karen Trentelman

Karen Trentelman is Senior Scientist at the Getty Conservation Institute. She has extensive experience in the application of XRF to works of art and teaching XRF to conservators, conservation scientists, students and the general public. She organized XRF round robins with conservation scientists at various museums from 2002-2010. Karen was involved in the conceptualization, organization and teaching of the XRF Boot Camp since its inception in 2011.

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Live Session
08/14/2020 at 1:00 PM (EDT)   |  120 minutes
08/14/2020 at 1:00 PM (EDT)   |  120 minutes Participate in the live workshop session or view the recording after the session is complete.
WEBINAR PRESENTATION | PDF Version of PowerPoint presentation
Open to download resource.
Open to download resource.
WORKBOOK | Handheld XRF in Cultural Heritage: A Practical Workbook for Conservators
WEB SITE | Handheld XRF In Cultural Heritage: A Practical Workbook for Conservators
Select the "Open" button to begin.
Select the "Open" button to begin. Link to the web page of the Getty Conservation Institute where you may download the PDF version of the worksbook.
WEB SITE | Lulu.com for ordering printed copy of the workbook
Select the "Open" button to begin.
Select the "Open" button to begin.
CORRIGENDUM: Page 91 of the Workbook with correct acquisition times listed
Open to download resource.
Open to download resource.
VIRTUAL WORKBOOK: XRF spectra and software for spectral interpretation
WEB SITE | Software for spectral interpretation: NIST DTSA-II
Select the "Open" button to begin.
Select the "Open" button to begin. This is a link to the web page dedicated to the DTSA-II software developed by Dr. Nicholas Ritchie at the National Institute of Standards and Technology. From here you can access: - software download (latest software version is now available through the site) - instructional video tutorials on YouTube - "Getting Started": text and image introduction to the software - "Documentation": links to video tutorials as well as PDFs that document software functions The software was originally designed for handling x-ray spectra collected by energy-dispersive spectrometers attached to scanning electron microscopes (SEM-EDS). We are using it to look at spectra collected by energy-dispersive spectrometers in XRF units (ED-XRF). We chose it because it is freely available for a variety of operating systems, has an intuitive user interface, and does a great job at labeling peaks, including escape peaks and sum peaks. Additionally, it allows users to visualize absorption edges and MAC curves (mass attenuation constant vs. x-ray energy) for elements of interest. Dr. Ritchie has generously made some modifications to facilitate the use of DTSA-II for this workshop. We will be seeking your feedback about the software to inform further adaptation of the software for learning XRF and for use in data analysis of spectra acquired using a variety of XRF instruments.
INSTRUCTIONS | Installing NIST DTSA-II Software on Windows
Open to download resource.
Open to download resource. These instructions will walk you through how to install NIST DTSA-II on a Windows PC. Installation may require that you download Java through Amazon Coretto 11 and instruct Windows to look to this version of Java when opening DTSA-II. There is a video that accompanies these instructions.
VIDEO | Installing NIST DTSA-II Software on a Windows
Open to view video.
Open to view video. This video accompanies written instructions on installing NIST DTSA-II on a Windows PC, which may require installing Java through Amazon Coretto 11.
INSTRUCTIONS | Installing NIST DTSA-II Software on a Mac
Open to download resource.
Open to download resource. UPDATED This PDF contains instructions and screen captures to illustrate the process of installing and launching NIST DTSA-II on a Mac. In addition to downloading the software from the NIST DTSA-II web site, Mac users will need to download version 11 of Java (from Amazon Coretto). The instructions show you how to force the Mac OS to install DTSA and then to launch the software.
VIDEO | Installing NIST DTSA-II Software on a Mac
Open to view video.
Open to view video. This is a brief video that shows the installation and launching of DTSA-II on a Mac. This includes (1) downloading DTSA; (2) downloading and installing Java from Amazon; (3) installing DTSA with the new version of Java; (4) launching DTSA with Java.
SPECTRUM FILES | All Exercises in Chapters 2 and 3
Open to download resource.
Open to download resource. Zipped file containing all the spectra needed to complete the exercises in Chapters 2 and 3.
VIDEO | DTSA-II: Open and view spectrum files (2:42 minutes)
Open to view video.
Open to view video. Brief instructions for opening and viewing spectrum files. (by Aniko Bezur)
VIDEO | DTSA-II: Zooming in and out on spectra (3:16 minutes)
Open to view video.
Open to view video. A brief introduction on various ways to look at spectrum details. by Aniko Bezur
VIDEO | DTSA-II: Spectrum properties window (2:53 minutes)
Open to view video.
Open to view video. Tips and tricks for viewing and using information in the spectrum properties window. by Aniko Bezur
VIDEO | DTSA-II: Peak labeling, part 1 (6:05 minutes)
Open to view video.
Open to view video. Introduction to labeling peaks by Aniko Bezur
VIDEO | DTSA-II: Peak labeling, part 2 (4:20 minutes)
Open to view video.
Open to view video.
VIDEO | DTSA-II: Spectrum comparison (3:19 minutes)
Open to view video.
Open to view video. Introduction to normalizing spectra using the spectrum comparison pop-up menu. by Aniko Bezur
INSTRUCTIONS | Using scripts in DTSA-II to visualize elemental data and mass absorption coefficients
Open to download resource.
Open to download resource.
VIDEO | Introduction to NIST DTSA-II (video by Nicholas Ritchie)
Select the "View On-Demand Recording" button to begin.
Select the "View On-Demand Recording" button to begin. A video introducing the basic features of NIST DTSA-II, "power tools for X-ray microanalysis." It discusses the basic user interface and mentions briefly the various different tools available to process and analyze spectra and to simulate spectra. The software is available from https://cstl.nist.gov/div837/837.02/epq/dtsa2/
REAL-LIFE ADVICE: Resources for Bruker Tracer Users
VIDEO | Bruker Tracer Assembly
Recorded 03/30/2017
Recorded 03/30/2017 This video describes the components and assembly of Bruker Tracer III-V and III-SD models. The video was produced for XRF Boot Camps.
VIDEO | Intro to Bruker XRayOps
Recorded 03/30/2017
Recorded 03/30/2017 This video was created for the XRF Boot Camp and provides step-by-step instructions on how to use the X-ray Ops software that controls voltage and current settings for Bruker Tracer III-V and III-SD units.
VIDEO | Intro to Bruker S1PXRF
Select the "View On-Demand Recording" button to begin.
Select the "View On-Demand Recording" button to begin. This video was created for XRF Boot Camp workshops and introduces the use of S1PXRF software to control Bruker handheld units.
VIDEO | Introduction to Artax software for Bruker XRF product users
Recorded 03/30/2017
Recorded 03/30/2017 This video was produced for XRF Boot Camps and provides instructions on how to export the data from S1PXRF software and to utilize the Artax software for spectrum analysis.
BIBLIOGRAPHY for Chapter 1: Radiation Safety
ALARA - As Low As Reasonably Achievable (CDC web page)
Select the "Open" button to begin.
Select the "Open" button to begin. The guiding principle of radiation safety is “ALARA”. ALARA stands for “as low as reasonably achievable”. This principle means that even if it is a small dose, if receiving that dose has no direct benefit, you should try to avoid it. The CDC web page explains the three basic protective measures in radiation safety: time, distance, and shielding.
Dictionary of Radiation Terms (web page of Radiation Emergency Medical Management)
Select the "Open" button to begin.
Select the "Open" button to begin. This online resource provides an alphabetical listing of terms and their definitions related to radiation. It also provides links to additional resources on radiation.
Radiation doses in our daily lives (web page of the US Nuclear Regulatory Commission)
Select the "Open" button to begin.
Select the "Open" button to begin. This web page provides information about natural background radiation and man-made sources of radiation experienced by people.
BIBLIOGRAPHY for Chapter 2: X-ray Fluorescence Spectroscopy: Fundamental Principles
Periodic Table of x-ray properties (web page)
Select the "Open" button to begin.
Select the "Open" button to begin. This is an interactive periodic table that allows you to view the absorption edge energies for shells as well as the energies of fluorescent x-rays. P. Bandyopadhyay and C.U. Segre, http://www.csrri.iit.edu/mucal.html
A LabVIEW-controlled portable x-ray fluorescencespectrometer for the analysis of art objects
Open to download resource.
Open to download resource. Desnica, Vladan, and Manfred Schreiner. 2006. "A LabVIEW-controlled portable x-ray fluorescence spectrometer for the analysis of art objects." X-Ray Spectrometry 35 (5):280-286. doi: 10.1002/xrs.906.
Evaluation of portable X-ray fluorescence (pXRF) in exploration and mining: Phase 1, control reference materials
Open to download resource.
Open to download resource. Hall, Gwendy E.M., Graeme F. Bonham-Carter, and Angelina Buchar. 2014. "Evaluation of portable X-ray fluorescence (pXRF) in exploration and mining: Phase 1, control reference materials." Geochemistry: Exploration, Environment, Analysis 14 (2):99-123. doi: 10.1144/geochem2013-241.
Portable X-ray Fluorescence Spectrometry: Capabilities for In Situ Analysis | Chapter 1
Open to download resource.
Open to download resource. Potts, Philip J. 2008. "Chapter 1 Introduction, Analytical Instrumentation and Application Overview." In Portable X-ray Fluorescence Spectrometry: Capabilities for In Situ Analysis, edited by Philip J. Potts and Margaret West, 1-12. The Royal Society of Chemistry.
Portable X-ray Fluorescence Spectrometry: Capabilities for In Situ Analysis | Chapter 9
Open to download resource.
Open to download resource. Cesareo, Roberto, Stefano Ridolfi, Maurizio Marabelli, Alfredo Castellano, Giovanni Buccolieri, Marina Donativi, Giovanni E. Gigante, Antonio Brunetti, and Marco A. Rosales Medina. 2008. "Chapter 9 Portable Systems for Energy-Dispersive X-Ray Fluorescence Analysis of Works of Art." In Portable X-ray Fluorescence Spectrometry: Capabilities for In Situ Analysis, edited by Philip J. Potts and Margaret West, 206-246. The Royal Society of Chemistry.
Estimation and account for matrix effects instudying glass materials of cultural heritage by X-ray spectral analysis
Open to download resource.
Open to download resource. Revenko, A. G. 2010. "Estimation and account for matrix effects in studying glass materials of cultural heritage by X-ray spectral analysis." X-Ray Spectrometry 39 (1):63-69. doi: 10.1002/xrs.1223.
Tutorial: Attenuation of X-rays by matter
Select the "Open" button to begin.
Select the "Open" button to begin. Thomsen, Volker, Debbie Schatzlein, and David Mercuro. 2005. "Tutorial: Attenuation of X-rays by matter." Spectroscopy 20 (9):22-25.
Tutorial: Attenuation of X-Rays By Matter
Open to download resource.
Open to download resource. Thomsen, Volker, Debbie Schatzlein, and David Mercuro. 2005. "Tutorial: Attenuation of X-rays by matter." Spectroscopy 20 (9):22-25.
BIBLIOGRAPHY for Chapter 3 | Practical Exercises for Mock-ups
Barrett et al.: XRF analysis of historical paper in open books
Open to download resource.
Open to download resource. Barrett, Tim, Robert Shannon, Jennifer Wade, and Joseph Lang. 2012. "XRF analysis of historical paper in open books." In Handheld XRF for art and archaeology, edited by Aaron N. Shugar and Jennifer L. Mass, 191-214. Leuven: Leuven University Press.
Bezur & Casadio: The analysis of porcelain using handheld and portable X-ray fluorescence spectrometers
Open to download resource.
Open to download resource. Bezur, Anikó, and Francesca Casadio. 2012. "The analysis of porcelain using handheld and portable X-ray fluorescence spectrometers." In Handheld XRF for art and archaeology, edited by Aaron N. Shugar and Jennifer L. Mass, 249-311. Leuven: Leuven University Press.
Casadio et al.: X-ray fluorescence applied to overglaze enamel decoration on eighteenth- and nineteenth-century porcelain from central Europe
Open to download resource.
Open to download resource. Casadio, Francesca, Anikó Bezur, Kelly Domoney, Katherine Eremin, Lynn Lee, Jennifer L. Mass, Andrew Shortland, and Nicholas Zumbulyadis. 2012. "X-ray fluorescence applied to overglaze enamel decoration on eighteenth- and nineteenth-century porcelain from central Europe." Studies in Conservation 57 (s1):S61-S72. doi: http://dx.doi.org/10.1179/2047058412Y.0000000047. Technical and chronological aspects of overglaze enamel production at historic porcelain factories in central Europe are discussed based on studies of over 180 objects at various laboratories. Results of analyses on representative objects, carried out primarily with X-ray fluorescence spectroscopy, are presented. Examples of eighteenth- and nineteenth-century decoration by Meissen, Du Paquier, and Hausmaler painters are described in detail. The findings highlight established glaze formulation practices and enhance understanding of the dating of objects based on the detection of zinc in yellow, blue, and green glazes. This study is the first to provide extensive scientific evidence on the composition of nineteenthcentury overglaze enamel colors. In particular, the research highlights the frequent co-occurrence of both eighteenth- and nineteenth-century enamel formulations on objects, underscoring the need to examine all overglaze enamel colorants on porcelains before attributing the decoration to a particular time period.
Fonicello: Unique Problems with the Use of the Handheld XRF Spectrometer for Pesticide Surveys of Ethnographic Collections
Open to download resource.
Open to download resource. Fonicello, Nancy A. 2007. "Unique Problems with the Use of the Handheld XRF Spectrometer for Pesticide Surveys of Ethnographic Collections." ICOM-CC Ethnographic Conservation Newsletter (28):4-8. The handheld X-ray fluorescence (XRF) spectrometer has become increasingly popular as a practical tool for surveying ethnographic collections for the presence of metallic pesticides. Handheld instruments are efficient, easy to use, and do not require destructive sampling in order to obtain good results. But ethnographic collections pose a unique problem for these surveys. Ethnographic objects are often made up of diverse materials. It is not uncommon to have leather, metal, glass beads, vegetal fibers, feathers, fur, pigments, and textiles combined in a single object. Mercury, arsenic, lead, and other metals deriving from these materials may be mistaken for the presence of pesticides. Environmental factors can introduce detectable levels of metallic pollutants into collections. Data from the analyzer itself can be prone to misinterpretation without the proper understanding of its capabilities and limitations. Nevertheless, the handheld analyzer can provide valuable information about the chemistry, and therefore perhaps, the history, of the objects. It is the intent of this article to provide an overview of some of the complexities associated with the use of the handheld XRF spectrometer in ethnographic collections, and to examine some common sources of non-pesticide metals that one may encounter during an XRF pesticide survey.
Gianoncelli & Kourousias: Limitations of portable XRF implementations in evaluating depth information: an archaeometric perspective
Open to download resource.
Open to download resource. Gianoncelli, A., and G. Kourousias. 2007. "Limitations of portable XRF implementations in evaluating depth information: an archaeometric perspective." Applied Physics A: Materials Science & Processing 89 (4):857-863. Portable instruments that can perform non-destructive analysis techniques are of great importance due to their high applicability, which can extend beyond the controlled laboratory environment. Their importance has long been recognised in the archaeometric field where art historians, conservators and restorers perform analyses on art works without causing any damage and without the need to move the objects to specialized laboratories. The X-ray fluorescence (XRF) technique is a popular choice in the archaeometric field for in situ investigations with portable instrumentations. This enables qualitative (elemental analysis) and quantitative (chemical composition) information retrieval from the objects of interest. Quantitative analyses can be performed under the assumption that the sample is homogeneous and its surface material is the same as in the rest of the object. This work aims to expose various details, including the strengths and the weaknesses of typical XRF analyses in the case of surface alterations, focusing on portable implementations. The chosen approach will be in line with certain issues considered important in archaeometry; nevertheless the presented findings are valid beyond this. We will focus our discussion on two kinds of objects that can be found in the cultural heritage field: artefacts that had their surface material altered due to prolonged exposure to the environment and artefacts that have been gilded. Our work also includes a critically examined overview of relevant information available in the literature. The core of our analysis focuses on two main distinct cases, that of multilayer objects and that of bronzes.
Glinsman: The practical application of air-path X-ray fluorescence spectrometry in the analysis of museum objects
Open to download resource.
Open to download resource. Glinsman, Lisha Deming. 2005. "The practical application of air-path X-ray fluorescence spectrometry in the analysis of museum objects." Reviews in Conservation (6):3-17. This paper furnishes the museum scientist, conservator and curator with a better understanging of the theory an dpractice of X-ray fluorescence spectrometry (XRF) for the study, preservation and exhibition of museum collections. An overview of X-ray fluorescence theory and instrumentation is presented. The scope of X-ray fluorescence spectrometry in the museum laboratory is demonstrated through specific examples from collections of the National Gallery of Art, Washington, D.C. Easel paintings, works on paper, photographic prints, sculpture and the decorative arts are discussed. Protocols for XRF analysis of works of art in different mediums are provided.
Grieten & Casadio: X-ray fluorescence portable systems for the rapid assessment of photographic techniques in notable art collections: the Alfred Stieglitz Collection
Open to download resource.
Open to download resource. Grieten, E., and F. Casadio. 2009. "X-ray fluorescence portable systems for the rapid assessment of photographic techniques in notable art collections: the Alfred Stieglitz Collection." X-Ray Spectrometry 39 (3):221-229. In the late nineteenth and early twentieth century photographers experimented, adapted and combined different techniques, using a wide array of chemicals leading to a vast range of commercial and self-made photographs. Museum professionals, experts and collectors typically rely on visual and microscopic examination to identify photographic processes, however, visual identification alone can be misleading. The present study describes applications of portable and handheld X-ray fluorescence(XRF) spectrometers to determine the metallic elements in photographic images, with special focus on one of the highest-profile photographic collections in the world, that of Alfred Stieglitz. A protocol was developed for two types of XRF spectrometers, a portable micro-focus system and a handheld macro-set-up, and validated with standard replicas of known photographic techniques. Qualitative XRF identification of the metallic salts allows unambiguous identification of the process used for each photograph. The portability of the systems makes the method applicable to the study of large collections in any location. In total, more than 60 photographs from the Alfred Stieglitz Collection were analyzed, leading to the revision of approximately 16% of the previous process identifications. These results are presented here for the first time. The correct identification of these photographs has significant impact on aspects of preventive conservation, exhibition and scholarly research, not only for the Art Institute of Chicago but also for other institutions and private collectors who own photographs from the Alfred Stieglitz Collection.
Hahn et al.: X-ray Fluorescence Analysis of Iron Gall Inks, Pencils and Coloured Crayons
Open to download resource.
Open to download resource. Hahn, Oliver, Birgit Kanngiesser, and Wolfgang Malzer. 2005. "X-ray Fluorescence Analysis of Iron Gall Inks, Pencils and Coloured Crayons." Studies in Conservation 50 (1):23-32. The qualitative and quantitative investigation of historical writing materials using micro X-ray fluorescence analysis (micro-XRF) is a suitable method for obtaining 'composition fingerprints' of different inks and coloured crayons. The quantitative analysis is based on a model that takes into account the heterogeneity and the layer structure of historical samples. Starting from these composition fingerprints, it is possible to distinguish between different iron gall inks used by an individual artist in order to establish a chronology of their use and, furthermore, to date unknown fragments that have not been integrated into the oeuvre of an artist until now. Qualitative and quantitative analyses of several manuscripts of Johann Wolfgang von Goethe clarify the chronology within the genesis of these works. Investigation of Achim von Arnim's manuscript 'Studien zu Naturwissenschaften' indicated that various degradation mechanisms of iron gall inks could also be related to different inorganic compositions. Further measurements on coloured crayons in Friedrich Nietzsche's notebooks reveal that it is possible to distinguish between different notes written by Nietzsche and his successors. Finally the analyses of two different pencils from Goethe's work shows that it might be possible to distinguish between sketches completed before and after 1800.
Heginbotham et al.: The Copper CHARM Set: A New Set of Certified Reference Materials for the Standardization of Quantitative X-Ray Fluorescence Analysis of Heritage Copper Alloys
Open to download resource.
Open to download resource. Heginbotham, A., J. Bassett, D. Bourgarit, C. Eveleigh, L. Glinsman, D. Hook, D. Smith, R. J. Speakman, A. Shugar, and R. Van Langh. 2015. "The Copper CHARM Set: A New Set of Certified Reference Materials for the Standardization of Quantitative X-Ray Fluorescence Analysis of Heritage Copper Alloys*." Archaeometry 57 (5):856-868. doi: 10.1111/arcm.12117. 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.
Hochleitner et al.: Historical pigments: a collection analyzed with X-ray diffraction analysis and X-ray fluorescence analysis in order to create a database
Open to download resource.
Open to download resource. Hochleitner, B., V. Desnica, M. Mantler, and M. Schreiner. 2003. "Historical pigments: a collection analyzed with X-ray diffraction analysis and X-ray fluorescence analysis in order to create a database." Spectrochimica Acta Part B: Atomic Spectroscopy 58 (4):641-649. The main objective of this work is the identification of inorganic pigments with X-ray diffraction analysis in combination with X-ray fluorescence analysis (XRF). By using these techniques, differences of specific pigments with identical names but produced by different manufacturers, techniques, or raw materials are revealed. The purity and the chemical compositions of these pigments are tested and the different phases in the diffractograms identified. Measurements with XRF are carried out in order to facilitate the analysis of the diffractograms and to point out differences in the elemental composition of different pigments. The creation of a database of the obtained data and diffractograms is in progress. It will be a collection of the most common and interesting pigments used in art. Furthermore, this database will enable a fast and easy identification of pigments during the restoration and conservation of an object of art.
Ida et al.: Analysis of painted steel by a hand-held X-ray fluorescence spectrometer
Open to download resource.
Open to download resource. Ida, Hiroyuki, Takao Segawa, Shigeo Tohyama, and Jun Kawai. 2005. "Analysis of painted steel by a hand-held X-ray fluorescence spectrometer." Spectrochimica Acta Part B: Atomic Spectroscopy 60 (2):249-252. doi: https://doi.org/10.1016/j.sab.2004.12.010. Steel with a paint layer was analyzed with a hand-held X-ray fluorescence spectrometer. When the 0.5 mm thick paint layer was composed mainly of light elements, alloying elements in steel such as Fe, Cr, Ni, W, and Mo were easily detected. 0.2% Mo in steel was detectable even if the paint contained Ti or Fe as a main element. The signal intensity of each element in steel decreased exponentially when the paint thickness increased, and the degree of decrease depended on the X-ray energy. Therefore the peak intensity for non-painted steel could be calculated from the paint thickness. The paint thickness was estimated from the intensity ratio Fe Kβ/Kα or W Lβ/Lα. When a paint of Ti (0.07–0.49 mm thick) was used, the peak intensities of the Fe Kα, Cr Kα, Ni Kα, and Mo Kα lines for non-painted steel were estimated by using the intensity ratio Fe Kβ/Kα, with errors of less than 30%. The content of each element in steel is estimated when the fluorescent X-rays are detectable by analysis of painted steel without removing the paint layer. On-site screening of painted steel can be performed on the basis of the alloy composition estimated by analysis with a hand-held XRF spectrometer.
Knipe et al.: Materials and techniques of Islamic manuscripts
Open to download resource.
Open to download resource. Knipe, Penley, Katherine Eremin, Marc Walton, Agnese Babini, and Georgina Rayner. 2018. "Materials and techniques of Islamic manuscripts." Heritage Science 6 (1):55. doi: 10.1186/s40494-018-0217-y. Over 50 works on paper from Egypt, Iraq, Iran and Central Asia dated from the 13th to 19th centuries were examined and analyzed at the Straus Center for Conservation and Technical Studies. Forty-six of these were detached folios, some of which had been removed from the same dispersed manuscript. Paintings and illuminations from five intact manuscripts were also examined and analyzed, although not all of the individual works were included. The study was undertaken to better understand the materials and techniques used to create paintings and illuminations from the Islamic World, with particular attention paid to the diversity of greens, blues and yellows present. The research aimed to determine the full range of colorants, the extent of pigment mixing and the various preparatory drawing materials. The issue of binding materials was also addressed, albeit in a preliminary way.
Liritzis & Zacharias: Portable XRF of archaeological artifacts: current research, potentials and limitations
Open to download resource.
Open to download resource. Liritzis, Ioannis, and Nikolaos Zacharias. 2011. "Portable XRF of archaeological artifacts: current research, potentials and limitations." In X-ray fluorescence spectrometry (XRF) in geoarchaeology, 109-142. Springer. Portable X-ray fluorescence (PXRF) serves as an effective, rapid and non-destructive, method for determining the elemental composition of natural and man-made materials, such as ceramic, glaze, glass, obsidian, pigments, paint, and metal artifacts; based on the analysis, the determination of their origin, technological and production issues, comparative studies, and more knowledge in the field of cultural heritage can be aimed at. The wavelengths of the released energy, known as fluorescent X-rays, are detected and measured by spectrograph in the energy dispersive and wavelength manner of detection. Since only the surface of an object is studied, in dimensions that typically range within some millimeters, care needs to be taken that corrosion and decay do not affect the analysis. A world survey of the major applications of PXRF in the analysis of various cultural material types is reported, and the available PXRF setups are described. A review of the results of obsidian characterization and clustering is included, and the advantages, reliability, and limitations are discussed, with particular emphasis on the calibration procedures.
Manso et al.: Investigation of the Composition of Historical and Modern Italian Papers by Energy Dispersive X-ray Fluorescence (EDXRF), X-ray Diffraction (XRD), and Scanning Electron Microscopy Energy Dispersive Spectrometry (SEM-EDS)
Open to download resource.
Open to download resource. Manso, Marta, Maria Luisa Carvalho, Ignacio Queralt, Silvia Vicini, and Elisabetta Princi. 2011. "Investigation of the Composition of Historical and Modern Italian Papers by Energy Dispersive X-Ray Fluorescence (EDXRF), X-Ray Diffraction (XRD), and Scanning Electron Microscopy Energy Dispersive Spectrometry (SEM-EDS)." Applied Spectroscopy 65 (1):52-59. doi: 10.1366/10-06105. In this work, a study concerning the composition of Italian papers from the seventeenth to the twentieth centuries was carried out using energy dispersive X-ray fluorescence spectrometry (EDXRF), X-ray diffraction (XRD), and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS). The analyzed samples consisted of papers employed for drawing, writing, printing, and absorbance. Observations carried out by SEM magnified the typical paper morphology. EDXRF in combination with XRD and SEM-EDS allowed the determination of calcite, gypsum, kaolin, talc, magnesite, and dolomite, used as fillers in the production of the papers studied herein. The inks present in the handwritten and printed papers, investigated by SEM-EDS and μ-EDXRF, were synthetic, Fe based, and iron gall inks.
Mass & Matsen: Understanding silver hollow wares of the eighteenth and nineteenth centuries: Is there a role for X-ray fluorescence?
Open to download resource.
Open to download resource. Mass, Jennifer L., and Catherine R. Matsen. 2012. "Understanding silver hollow wares of the eighteenth and nineteenth centuries: Is there a role for X-ray fluorescence?" Studies in Conservation 57 (s1):S191-S198. doi: doi:10.1179/2047058412Y.0000000023. Open architecture energy dispersive X-ray fluorescence (XRF) has been used extensively for the study of historic silver alloys since 1970. Silver alloy analyses are carried out to address questions about an object's provenance, technology of manufacture, authenticity, and condition. However, the data generated from this surface analysis technique rarely represent the bulk alloy composition. Quantitative analysis of historic silver alloys using XRF non-destructively is challenging due to: the objects’ curved and irregular surfaces (absence of ideal and reproducible geometries); element segregation in copper–silver alloys; limited availability of alloy standards for instrument calibration; post-manufacturing acid treatments that dissolve surface copper from the alloy (pickling); the presence of firescale (copper oxides) or other corrosion/tarnish layers; and surface inhomogeneities introduced by polishing. This study represents an attempt to quantify these sources of error, and, where possible, to provide analytical protocols that can minimize or even eliminate them. Examples are provided using English and American silver hollow wares from the New York Historical Society.
Modica et al.: XRF analysis to identify historical photographic processes...
Open to download resource.
Open to download resource. Modica, A., M. F. Alberghina, M. Brai, M. Bruno, M. Di Bella, D. Fontana, and L. Tranchina. 2017. "XRF analysis to identify historical photographic processes: The case of some Interguglielmi Jr.’s images from the Palermo Municipal Archive." Radiation Physics and Chemistry 135:76-80. doi: https://doi.org/10.1016/j.radphyschem.2017.02.026. In the early period, even though professional photographers worked with similar techniques and products, their artistic and commercial aims determined different choices and led them to follow different, often personal, recipes. For this reason, identification of the techniques through date and name of the photographer or through some visual features like colour, tonality and surface of the image layer, often needs further investigation to be proved. Chemical characterization, carried out in a non or micro destructive way, can be crucial to provide useful information about the original composition, degradation process, realization technique, in obtaining an indirect dating of the photograph and/or to choose the most correct conservation treatment. In our case, x-ray fluorescence (XRF) analysis was used to confirm the chemical composition of eleven historical photographs dated between the end of the 19th century and the beginning of the 20th, shot in Palermo (Sicily) by a renowned photographer of the time, and pasted on their original cardboards. The elemental identification, obtained with a non destructive approach, provided important information to distinguish among different photographic techniques in terms of distribution and characterization of chemical elements markers in the photographic surface.
Namowicz: XRF of cultural heritage materials: Round-robin IV- paint on canvas
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Open to download resource. Namowicz, C., K. Trentelman, and C. McGlinchey. 2009. "XRF of cultural heritage materials: Round-robin IV- paint on canvas." Powder Diffraction 24 (2):124-129. To establish standard working practices and further understanding of the application of X-ray fluorescence (XRF) spectroscopy to works of art and cultural heritage materials, a series of round-robin tests have been conducted biannually since 2002. In 2008 the round-robin explored the application of XRF to the study of paintings on canvas. Thirteen samples, consisting of both modern and traditional pigments on canvas, were distributed to 25 participating institutions for analysis. The samples were designed to explore common challenges encountered in the XRF analysis of painted works including peak overlaps, sum peaks, layering/shielding effects, detection of low-Z pigments, and modern pigments. The results from representative samples highlighting each topic are discussed.
Stulik & Kaplan: The Atlas of Analytical Signatures of Photographic Processes
Select the "Open" button to begin.
Select the "Open" button to begin. The Atlas of Analytical Signatures of Photographic Processes is intended for practicing photograph conservators, curators, art historians, archivists, library professionals, and anyone responsible for the care of photograph collections. Its purpose is to aid in the formulation of analytical questions related to a particular photograph and to assist scientists unfamiliar with analysis of photographs when interpreting analytical data. The Atlas contains interpretation guides with identification of overlaps of spectral peaks and warnings of potential misidentification or misinterpretation of analytical results.
Thompson: Surface and Interfacial Characterization: Ion Beam Analysis
Open to download resource.
Open to download resource. Thompson, Richard. 2012. "Surface and Interfacial Characterization: Ion Beam Analysis." In Polymer Science: A Comprehensive Reference, edited by Krzysztof Matyjaszewski and Martin Möller, 661-681.
Vila & Centeno: FTIR, Raman and XRF identification of the image materials in turn of the 20th century pigment-based photographs
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Open to download resource. Vila, Anna, and Silvia A. Centeno. 2013. "FTIR, Raman and XRF identification of the image materials in turn of the 20th century pigment-based photographs." Microchemical Journal 106:255-262. doi: http://dx.doi.org/10.1016/j.microc.2012.07.016. Artists at the turn of the 20th century experimented with a wide range of photographic techniques to create complex and unique prints by processes that are difficult to fully identify. FTIR, both in transmission and ATR, Raman spectroscopy and XRF were applied to characterize and identify the materials and processes used in photographs from the period in which pigment-based techniques were employed alone or superimposed to others such as platinum. FTIR in the transmission mode and ATR acquired in the high image density areas of the images allow to characterize the organic components in the photographic colloid, and the analysis of the low image density areas gives vibrational information about the organic compounds used for sizing the paper substrates. Raman spectroscopy allows the identification of the pigments, while the chromium-containing compounds, such as chrome alum used to size the paper substrates and the compound/s that chromium forms with the oxidized organic component in gum print images, were found to be below the detection limit of the technique both in samples prepared strictly following historic recipes and in hundred year old works of art. The advantages and limitations of the multitechnique approach used to identify and differentiate gum prints are discussed.
BIBLIOGRAPHY for Chapter 4 | Practical Application of XRF to Cultural Heritage Materials
Alfeld & Viguerie: Recent developments in spectroscopic imaging techniques for historical paintings - A review
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Open to download resource. Alfeld, M., and L. de Viguerie. 2017. "Recent developments in spectroscopic imaging techniques for historical paintings - A review." Spectrochimica Acta Part B: Atomic Spectroscopy 136:81-105. doi: https://doi.org/10.1016/j.sab.2017.08.003. This paper provides an overview over the application of scanning macro-XRF with mobile instruments for the investigation of historical paintings. The method is compared to synchrotron based macro-XRF imaging and Neutron Activation Auto-Radiography. Full-Field XRF imaging instruments, a potential future alternative to scanning macro-XRF, and confocal XRF, providing complementary depth profiles and developing into a 3D imaging technique itself, are described with the focus on investigations of historical paintings. Recent developments of X-ray radiography are presented and the investigation of cultural heritage objects other than paintings by MA-XRF is summarized. In parallel to XRF, hyperspectral imaging in the visible and range has developed into a technique with comparable capabilities, providing insight in chemical compounds, where XRF imaging identifies the distribution of elements. Due to the complementary nature of these techniques the latter is summarized. Further, progress and state of the art in data evaluation for spectroscopic imaging is discussed. In general it could be observed that technical capabilities in MA-XRF and hyperspectral imaging have reached a plateau and that with the availability of commercial instruments the focus of recent studies has shifted from the development of methods to applications of the instruments. Further, that while simple instruments are easily available with medium budgets only few groups have high-end instrumentation available, bought or in-house built.
Burgio & Clark: Library of FT-Raman spectra of pigments, minerals, pigment media and varnishes, and supplement to existing library of Raman spectra of pigments with visible excitation
Open to download resource.
Open to download resource. Burgio, Lucia, and Robin J. H. Clark. 2001. "Library of FT-Raman spectra of pigments, minerals, pigment media and varnishes, and supplement to existing library of Raman spectra of pigments with visible excitation." Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 57 (7):1491-1521. Sixty pigments, minerals and media have been analysed by Fourier-transform Raman (FT-Raman) microscopy in order to assemble a database of reference FT-Raman spectra for scientists working at the Arts-Science interface. An earlier library of Raman spectra compiled using visible excitation has been extended by the addition of 22 further reference spectra obtained with 780.0, 647.1, 632.8 and/or 514.5 nm excitation. The relative merits of 1064 nm and visible excitation are discussed.
Casadio et al.: Raman Spectroscopy of cultural heritage Materials: Overview of Applications and New Frontiers in Instrumentation, Sampling Modalities, and Data Processing
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Open to download resource. Casadio, Francesca, Céline Daher, and Ludovic Bellot-Gurlet. 2017. "Raman Spectroscopy of cultural heritage Materials: Overview of Applications and New Frontiers in Instrumentation, Sampling Modalities, and Data Processing." In Analytical Chemistry for Cultural Heritage, edited by Rocco Mazzeo, 161-211. Cham: Springer International Publishing.
Cucci et al.: Reflectance Hyperspectral Imaging for Investigation of Works of Art: Old Master Paintings and Illuminated Manuscripts
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Open to download resource. Cucci, Costanza, John K. Delaney, and Marcello Picollo. 2016. "Reflectance Hyperspectral Imaging for Investigation of Works of Art: Old Master Paintings and Illuminated Manuscripts." Accounts of Chemical Research 49 (10):2070-2079. doi: 10.1021/acs.accounts.6b00048. Diffuse reflectance hyperspectral imaging, or reflectance imaging spectroscopy, is a sophisticated technique that enables the capture of hundreds of images in contiguous narrow spectral bands (bandwidth < 10 nm), typically in the visible (Vis, 400–750 nm) and the near-infrared (NIR, 750–2500 nm) regions. This sequence of images provides a data set that is called an image-cube or file-cube. Two dimensions of the image-cube are the spatial dimensions of the scene, and the third dimension is the wavelength. In this way, each spatial pixel in the image has an associated reflectance spectrum. This “big data” image-cube allows for the mining of artists’ materials and mapping their distribution across the surface of a work of art.Reflectance hyperspectral imaging, introduced in the 1980s by Goetz and co-workers, led to a revolution in the field of remote sensing of the earth and near planets (Goetz, F. H.; Vane, G.; Solomon, B. N.; Rock, N. Imaging Spectrometry for Earth Remote Sensing. Science, 1985, 228, 1147−1152). In the subsequent decades, thanks to rapid advances in solid-state sensor technology, reflectance hyperspectral imaging, once only available to large government laboratories, was extended to new fields of application, such as monitoring agri-foods, pharmaceutical products, the environment, and cultural heritage. In the 2000s, the potential of this noninvasive technology for the study of artworks became evident and, consequently, the methodology is becoming more widely used in the art conservation science field.Typically hyperspectral reflectance image-cubes contain millions of spectra. Many of these spectra are similar, making the reduction of the data set size an important first step. Thus, image-processing tools based on multivariate techniques, such as principal component analysis (PCA), automated classification methods, or expert knowledge systems, that search for known spectral features are often applied. These algorithms seek to reduce the large number of high-quality spectra to a common subset, which allow identifying and mapping artists’ materials and alteration products. Hence, reflectance hyperspectral imaging is finding its place as the starting point to find sites on polychrome surfaces for spot analytical techniques, such as X-ray fluorescence, Raman spectroscopy, and Fourier transform infrared spectroscopy. Reflectance hyperspectral imaging can also provide image products that are a mainstay in the art conservation field, such as color-accurate images, broadband near-infrared images, and false-color products.This Account reports on the research activity carried out by two research groups, one at the “Nello Carrara” Institute of Applied Physics of the Italian National Research Council (IFAC–CNR) in Florence and the other at the National Gallery of Art (NGA) in Washington, D.C. Both groups have conducted parallel research, with frequent interchanges, to develop multispectral and hyperspectral imaging systems to study works of art. In the past decade, they have designed and experimented with some of the earliest spectral imaging prototypes for museum applications. In this Account, a brief presentation of the hyperspectral sensor systems is given with case studies showing how reflectance hyperspectral imaging is answering key questions in cultural heritage.
Delaney et al.: Use of imaging spectroscopy, fiber optic reflectance spectroscopy, and X-ray fluorescence to map and identify pigments in illuminated manuscripts
Open to download resource.
Open to download resource. Delaney, John K., Paola Ricciardi, Lisha Deming Glinsman, Michelle Facini, Mathieu Thoury, Michael Palmer, and E. René de la Rie. 2013. "Use of imaging spectroscopy, fiber optic reflectance spectroscopy, and X-ray fluorescence to map and identify pigments in illuminated manuscripts " Studies in Conservation. doi: http://dx.doi.org/10.1179/2047058412Y.0000000078. A paradigm using multispectral visible and near-infrared imaging spectroscopy is presented to semi-automatically create unbiased spectral maps that guide the site selection for in situ analytical methods (e.g. fiber optic reflectance spectroscopy and X-ray fluorescence) in order to identify and map pigments in illuminated manuscripts. This approach uses low spectral resolution imaging spectroscopy to create maps of areas having the same spectral characteristics. This paradigm is demonstrated by analysis of the illuminated manuscript leaf Christ in Majesty with Twelve Apostles (workshop of Pacino di Buonaguida, c. 1320). Using this approach the primary pigments are mapped and identified as azurite, lead-tin yellow, red lead, a red lake (likely insect-derived), a copper-containing green, brown iron oxide, and lead white. Moreover, small amounts of natural ultramarine were found to be used to enhance the blue fields around Christ, and a red lake was used to highlight different colors. These results suggest that the proposed paradigm offers an improved approach to the comprehensive study of illuminated manuscripts by comparison with site-specific analytical methods alone. The choice of broad spectral bands proves successful, given the limited palette in illuminated manuscripts, and permits operation at the low light intensity required for examination of manuscripts.
Dik et al.: Silverpoint underdrawing? - A Note on its Visualization with Synchrotron Radiation based X-ray Fluorescence Analysis
Open to download resource.
Open to download resource. Dik, Joris, Arie Wallert, Geert van Der Snickt, and Koen Janssens. 2008. "Silverpoint underdrawing? - A Note on its Visualization with Synchrotron Radiation based X-ray Fluorescence Analysis." Zeitschrift für kunsttechnologie und konservierung 22 (2).
Dooley: Separating two painting campaigns in Saul and David, attributed to Rembrandt, using macroscale reflectance and XRF imaging spectroscopies and microscale paint analysis
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Open to download resource. Dooley, Kathryn A., E. Melanie Gifford, Annelies van Loon, Petria Noble, Jason G. Zeibel, Damon M. Conover, Matthias Alfeld, Geert Van der Snickt, Stijn Legrand, Koen Janssens, Joris Dik, and John K. Delaney. 2018. "Separating two painting campaigns in Saul and David, attributed to Rembrandt, using macroscale reflectance and XRF imaging spectroscopies and microscale paint analysis." Heritage Science 6 (1):46. doi: 10.1186/s40494-018-0212-3. Late paintings of Rembrandt van Rijn (1606–1669) offer intriguing problems for both art historians and conservation scientists. In the research presented here, the key question addressed is whether observed stylistic differences in paint handling can be correlated with material differences. In Saul and David, in the collection of the Royal Picture Gallery Mauritshuis in The Hague, NL, the stylistic differences between the loose brushwork of Saul’s cloak and the more detailed depiction of his turban and the figure of David have been associated with at least two painting stages since the late 1960s, but the attribution of each stage has been debated in the art historical literature. Stylistic evaluation of the paint handling in the two stages, based on magnified surface examination, is further described here. One of the research goals was to determine whether the stylistic differences could be further differentiated with macroscale and microscale methods of material analysis. To address this, selected areas of the painting having pronounced stylistic differences were investigated with two macroscopic chemical imaging methods, X-ray fluorescence and reflectance imaging spectroscopies. The pigments used were identified and their spatial distribution was mapped. The mapping results show that the passages rendered in more detail and associated stylistically with the first painting stage, such as the orange-red color of David’s garment or the Greek key design in Saul’s turban, were painted with predominately red ochre mixed with vermilion. The regions of loose, bold brushwork, such as the orange-red slashing strokes in the interior of Saul’s cloak, associated with the second painting stage, were painted with predominately red ochre without vermilion. These macroscale imaging results were confirmed and extended with scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM–EDX) analysis of three cross-sections taken from regions of stylistic differences associated with the two painting stages, including one sample each from the right and left sleeve of David, and one from the interior of Saul’s cloak. SEM–EDX also identified a trace component, barium sulfate, associated with the red ochre of the second stage revisions. Combining mapping information from two spectroscopic imaging methods with localized information from microscopic samples has clearly shown that the stylistic differences observed in the paint handling are affiliated with differences in the chemical composition of the paints.
Heginbotham et al.: 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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Open to download resource. Heginbotham, A., J. Bassett, D. Bourgarit, C. Eveleigh, L. Glinsman, D. Hook, D. Smith, R. J. Speakman, A. Shugar, and R. Van Langh. 2015. "The Copper CHARM Set: A New Set of Certified Reference Materials for the Standardization of Quantitative X-Ray Fluorescence Analysis of Heritage Copper Alloys*." Archaeometry 57 (5):856-868. doi: 10.1111/arcm.12117.
Heginbotham et al.: CHARMed PyMca, Part I: A Protocol for Improved Inter-laboratory Reproducibility in the Quantitative ED-XRF Analysis of Copper Alloys
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Open to download resource. Heginbotham, A., and V. A. Solé. 2017. "CHARMed PyMca, Part I: A Protocol for Improved Inter-laboratory Reproducibility in the Quantitative ED-XRF Analysis of Copper Alloys." Archaeometry:n/a-n/a. doi: 10.1111/arcm.12282. 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.
Mass & Matsen: Understanding silver hollow wares of the eighteenth and nineteenth centuries: Is there a role for X-ray fluorescence?
Open to download resource.
Open to download resource. Mass, Jennifer L., and Catherine R. Matsen. 2012. "Understanding silver hollow wares of the eighteenth and nineteenth centuries: Is there a role for X-ray fluorescence?" Studies in Conservation 57 (s1):S191-S198. doi: doi:10.1179/2047058412Y.0000000023. Open architecture energy dispersive X-ray fluorescence (XRF) has been used extensively for the study of historic silver alloys since 1970. Silver alloy analyses are carried out to address questions about an object's provenance, technology of manufacture, authenticity, and condition. However, the data generated from this surface analysis technique rarely represent the bulk alloy composition. Quantitative analysis of historic silver alloys using XRF non-destructively is challenging due to: the objects’ curved and irregular surfaces (absence of ideal and reproducible geometries); element segregation in copper–silver alloys; limited availability of alloy standards for instrument calibration; post-manufacturing acid treatments that dissolve surface copper from the alloy (pickling); the presence of firescale (copper oxides) or other corrosion/tarnish layers; and surface inhomogeneities introduced by polishing. This study represents an attempt to quantify these sources of error, and, where possible, to provide analytical protocols that can minimize or even eliminate them. Examples are provided using English and American silver hollow wares from the New York Historical Society.
Orfanou & Rehren: A (not so) dangerous method: pXRF vs. EPMA-WDS analyses of copper-based artefacts
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Open to download resource. Orfanou, V., and Th. Rehren. 2015. "A (not so) dangerous method: pXRF vs. EPMA-WDS analyses of copper-based artefacts." Archaeological and Anthropological Sciences 7 (3):387-397. doi: 10.1007/s12520-014-0198-z. Analysis of metal objects with portable and handheld X-ray fluorescence spectrometry has become increasingly popular in recent years. Here, methodological concerns that apply to non-destructive, surface examination with XRF instruments of ancient metal artefacts are discussed based on the comparative analyses of a set of copper-based objects by means of portable X-ray fluorescence (pXRF) and electron probe microanalyser (EPMA). The analytical investigation aims to explore issues of instrument comparability and reliability of the non-invasive pXRF results. The different analytical approaches produce a comparable pattern for the major element concentrations, but substantial variation is evident when it comes to the absolute values for major and minor/trace elements.
Ricciardi et al.: Macro X-ray fluorescence (MA-XRF) scanning of illuminated manuscript fragments: potentialities and challenges
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Open to download resource. Ricciardi, Paola, Stijn Legrand, Giulia Bertolotti, and Koen Janssens. 2016. "Macro X-ray fluorescence (MA-XRF) scanning of illuminated manuscript fragments: potentialities and challenges." Microchemical Journal 124:785-791. doi: https://doi.org/10.1016/j.microc.2015.10.020. Macro X-ray fluorescence scanning (MA-XRF) is gradually becoming an established technique for the non-invasive analytical investigation of painted surfaces. This paper discusses some of the benefits and limitations of employing MA-XRF for the study of manuscript illuminations. Art historical research on this type of artefacts that is based on scientific measurements is often limited by the fact that usually no sampling can take place. Hence there is a need for non-invasive analytical tools that make it possible to conduct systematic investigations. As a representative example of this type of objects, a 15th century Italian manuscript fragment from the collection of the Fitzwilliam Museum in Cambridge (UK) is investigated. The aims of the study were to gain insight into the materials and techniques employed by Renaissance illuminators and to help answer specific questions regarding the fragment’s authorship and geographic origin. The complementarity and advantages of MA-XRF mapping versus site-specific analyses are discussed. For this purpose, MA-XRF data are evaluated and compared with the results of other analytical techniques. The interpretation of the elemental maps is discussed along with the challenges faced during the analysis.
Sarrazin et al.: A portable non-invasive XRD-XRF instrument for the study of art objects
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Open to download resource. Sarrazin, P, G Chiari, and M Gailhanou. 2009. "A portable non-invasive XRD-XRF instrument for the study of art objects." JCPDS-International Centre for Diffraction Data:175-186. A non-invasive XRD/XRF instrument for study of works of art has been developed jointly by the Getty Conservation Institute and inXitu Inc. (California). Many aspects of the instrument are based on technologies initially developed for NASA’s planetary XRD/XRF instrument CheMin and used in inXitu’s portable transmission XRD/XRF instrument (Terra). A new geometry was designed based on a reflection configuration to allow analyzing large flat objects such as mural paintings in a non-destructive way. The instrument uses a miniature X-ray tube and a CCD detector to collect both XRD and XRF signatures. All components are in fixed position relative to each other to guarantee a rugged stable geometry. The instrument also includes an imaging camera to collect high magnification images of the area analyzed and allow precise control of its positioning in the focusing plane. The instrument prototype was tested on a number of mockup samples and on art objects of the Getty collection.
Trentelman: Analyzing the Heterogeneous Hierarchy of Cultural Heritage Materials: Analytical Imaging
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Open to download resource. Trentelman, Karen. 2017. "Analyzing the Heterogeneous Hierarchy of Cultural Heritage Materials: Analytical Imaging." Annual Review of Analytical Chemistry 10 (1):247-270. doi: 10.1146/annurev-anchem-071015-041500. Objects of cultural heritage significance are created using a wide variety of materials, or mixtures of materials, and often exhibit heterogeneity on multiple length scales. The effective study of these complex constructions thus requires the use of a suite of complementary analytical technologies. Moreover, because of the importance and irreplaceability of most cultural heritage objects, researchers favor analytical techniques that can be employed noninvasively, i.e., without having to remove any material for analysis. As such, analytical imaging has emerged as an important approach for the study of cultural heritage. Imaging technologies commonly employed, from the macroscale through the micro- to nanoscale, are discussed with respect to how the information obtained helps us understand artists’ materials and methods, the cultures in which the objects were created, how the objects may have changed over time, and importantly, how we may develop strategies for their preservation.
Trentelman et al.: The examination of works of art using in situ XRF line and area scans
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Open to download resource. Trentelman, Karen, Michel Bouchard, Monica Ganio, Carole Namowicz, Catherine Schmidt Patterson, and Marc Walton. 2010. "The examination of works of art using in situ XRF line and area scans." X-Ray Spectrometry 39 (3):159-166. doi: 10.1002/xrs.1242. Spatially resolved element distributions generated by in situ X-ray fluorescence (XRF) line and area scans are shown to provide information about works of art which may not be obtainable from single spot spectra. In addition to generating visually powerful element maps and line profiles, this method also generates a spectrum at each image point, and this large data set is available for additional analysis. When generating line and area scans in the study of works of art, the collection parameters—including X-ray tube choice, spot size, step size, and scan time—must be optimized not only to produce the best signal, but also to perform the analysis within constraints imposed to ensure the security or safety of the object. Examples of the application of this method to several classes of works of art are presented, including illuminated manuscripts, paintings, bronze sculpture, and glazed ceramics.
Trentelman et al.: XRF analysis of manuscript illuminations
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Open to download resource. Trentelman, K., C. Schmidt Patterson, and N. Turner. 2013. "XRF analysis of manuscript illuminations." In Handheld XRF for art and archaeology, edited by Aaron N. Shugar and Jennifer L. Mass, 159-189. Leuven: Leuven University Press.
Turner et al.: Visualizing underdrawings in medieval manuscript illuminations with macro-X-ray fluorescence scanning
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Open to download resource. Turner, Nancy K., Catherine Schmidt Patterson, Douglas K. MacLennan, and Karen Trentelman. 2019. "Visualizing underdrawings in medieval manuscript illuminations with macro-X-ray fluorescence scanning." X-Ray Spectrometry 48 (4):251-261. doi: 10.1002/xrs.2956. The element-specific distribution maps generated by scanning macro-X-ray fluorescence (XRF) spectroscopy are providing cultural heritage researchers with information about the composition of materials present in works of art and, more importantly, unprecedented insight into the techniques employed by artists in their creation. One of the advantages of macro-XRF scanning is that the X-rays probe materials in subsurface layers, allowing, for example, visualizations of hidden paintings to be produced. Consequently, macro-XRF scanning has found wide use in the study of paintings, but the high spatial resolution also makes it particularly well suited for the study of the small-scale painted illustrations and decorative elements found in illuminated manuscripts. The preliminary drawings made by manuscript illuminators to plan a painted composition—known as underdrawings—provide evidence relating to artists' creative vision and working process but are difficult to examine because they are generally hidden under the surface paint layer. Traditionally, underdrawings in a carbon-based medium are visualized using infrared (IR) imaging. In this study, results of the analysis of painted illuminations from medieval illuminated manuscripts demonstrate that macro-XRF scanning can visualize underdrawings in other materials, such as iron-gall ink, metalpoint, and pigmented inks/paints, thus serving as a useful complement to traditional IR imaging. For manuscript illuminations in bound books, this study also discusses the use of interleaving materials to reduce unwanted signals from underlying folios. The ability to reveal manuscript underdrawings will help elucidate artistic intent and workshop practice and provide a new way to examine the history of medieval drawing.
Vandenabeele et al.: A decade of Raman spectroscopy in art and archaeology
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Open to download resource. Vandenabeele, Peter, Howell G. M. Edwards, and Luc Moens. 2007. "A decade of Raman spectroscopy in art and archaeology." Chemical Reviews 107 (3):675-686.