Combined 1D, 2D and 3D micro-XRF techniques for the analysis of illuminated manuscripts

Lachmann, Tim; Snickt, Geert Van der; Haschke, Michael; Mantouvalou, Ioanna

doi:10.1039/c6ja00220j

Cited by 22 publications

(20 citation statements)

References 15 publications

(22 reference statements)

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“…38 The illuminated manuscript has previously been analyzed with a portable Raman-X-ray instrument (PRAXIS) using combined µRaman spectroscopy, µ-XRF and synchrotron µ-XRD, 24 as well as with 3D confocal XRF. 39 Throughout all these studies no visual change to the manuscript folio was noticeable.…”

Section: Illuminated Manuscriptmentioning

confidence: 87%

Macroscopic X-ray Powder Diffraction Scanning, a New Method for Highly Selective Chemical Imaging of Works of Art: Instrument Optimization

et al. 2018

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In the past decade macroscopic X-ray fluorescence imaging (MA-XRF) has become established as a method for the noninvasive investigation of flat painted surfaces, yielding large scale elemental maps. MA-XRF is limited by a lack of specificity, only allowing for indirect pigment identification based on the simultaneous presence of chemical elements. The high specificity of X-ray powder diffraction (XRPD) mapping is already being exploited at synchrotron facilities for investigations at the (sub)microscopic scale, but the technique has not yet been employed using lab sources. In this paper we present the development of a novel MA-XRPD/XRF instrument based on a laboratory X-ray source. Several combinations of X-ray sources and area detectors are evaluated in terms of their spatial and angular resolution and their sensitivity. The highly specific imaging capability of the combined MA-XRPD/XRF instrument is demonstrated on a 15th/16th century illuminated manuscript directly revealing the distribution of a large number of inorganic pigments, including the uncommon yellow pigment massicot ( o-PbO). The case study illustrates the wealth of new mapping information that can be obtained in a noninvasive manner using the laboratory MA-XRPD/XRF instrument.

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Section: Illuminated Manuscriptmentioning

confidence: 87%

Macroscopic X-ray Powder Diffraction Scanning, a New Method for Highly Selective Chemical Imaging of Works of Art: Instrument Optimization

et al. 2018

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“…The commercial MXRF spectrometer (Bruker M4 tornado) was equipped with a Rh microfocus X‐ray tube, a polycapillary lens to focus the radiation and a SDD detector (Lachmann et al ). In front of a second SDD a second polycapillary lens was mounted perpendicular to the first, thus creating a confocal MXRF setup which enabled three‐dimensional‐resolved measurements with a resolution of 30 µm at Fe Kα (Mantouvalou et al ).…”

Section: Methodsmentioning

confidence: 99%

Selective mineral transport barriers at Cuscuta‐host infection sites

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Mantouvalou

Kanngießer

et al. 2019

Physiologia Plantarum

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The uptake of inorganic nutrients by rootless parasitic plants, which depend on host connections for all nutrient supplies, is largely uncharted. Using X‐ray fluorescence spectroscopy (XRF), we analyzed the element composition of macro‐ and micronutrients at infection sites of the parasitic angiosperm Cuscuta reflexa growing on hosts of the genus Pelargonium. Imaging methods combining XRF with 2‐D or 3‐D (confocal) microscopy show that most of the measured elements are present at similar concentrations in the parasite compared to the host. However, calcium and strontium levels drop pronouncedly at the host/parasite interface, and manganese appears to accumulate in the host tissue surrounding the interface. Chlorine is present in the haustorium at similar levels as in the host tissue but is decreased in the stem of the parasite. Thus, our observations indicate a restricted uptake of calcium, strontium, manganese and chlorine by the parasite. Xylem‐mobile dyes, which can probe for xylem connectivity between host and parasite, provided evidence for an interspecies xylem flow, which in theory would be expected to carry all of the elements indiscriminately. We thus conclude that inorganic nutrient uptake by the parasite Cuscuta is regulated by specific selective barriers whose existence has evaded detection until now.

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“…The false color images, with red indicating pigments on the recto side of the manuscript (further from the detector) and green on the verso side, show the artistic interplay of the two pigments: areas of the scrollwork that have been painted with azurite on the front side are gilded on the back side and vice versa (Figure 6A and B). Confocal XRF analyses previously conducted on the illuminated parchment have shown that the gold layer is very thin (< 1 µm) 32 so that the average thickness of the parchment can be estimated from the gold histograms and is about 120 µm. Indeed, only the parchment separates the gilding on the recto and verso sides.…”

Section: Depth-selective Informationmentioning

confidence: 99%

Macroscopic X-ray Powder Diffraction Scanning: Possibilities for Quantitative and Depth-Selective Parchment Analysis

et al. 2018

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At or below the surface of painted works of art, valuable information is present that provides insights into an object's past, such as the artist's technique and the creative process that was followed or its conservation history but also on its current state of preservation. Various noninvasive techniques have been developed over the past 2 decades that can probe this information either locally (via point analysis) or on a macroscopic scale (e.g., full-field imaging and raster scanning). Recently macroscopic X-ray powder diffraction (MA-XRPD) mapping using laboratory X-ray sources was developed. This method can visualize highly specific chemical distributions at the macroscale (dm). In this work we demonstrate the synergy between the quantitative aspects of powder diffraction and the noninvasive scanning capability of MA-XRPD highlighting the potential of the method to reveal new types of information. Quantitative data derived from a 15th/16th century illuminated sheet of parchment revealed three lead white pigments with different hydrocerussite-cerussite compositions in specific pictorial elements, while quantification analysis of impurities in the blue azurite pigment revealed two distinct azurite types: one rich in barite and one in quartz. Furthermore, on the same artifact, the depth-selective possibilities of the method that stem from an exploitation of the shift of the measured diffraction peaks with respect to reference data are highlighted. The influence of different experimental parameters on the depth-selective analysis results is briefly discussed. Promising stratigraphic information could be obtained, even though the analysis is hampered by not completely understood variations in the unit cell dimensions of the crystalline pigment phases.

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Combined 1D, 2D and 3D micro-XRF techniques for the analysis of illuminated manuscripts

Cited by 22 publications

References 15 publications

Macroscopic X-ray Powder Diffraction Scanning, a New Method for Highly Selective Chemical Imaging of Works of Art: Instrument Optimization

Macroscopic X-ray Powder Diffraction Scanning, a New Method for Highly Selective Chemical Imaging of Works of Art: Instrument Optimization

Selective mineral transport barriers at Cuscuta‐host infection sites

Macroscopic X-ray Powder Diffraction Scanning: Possibilities for Quantitative and Depth-Selective Parchment Analysis

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