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Die Befunde eines Forschungsprojektes zur Hinterglasmalerei werfen ein neues Licht auf die gegenseitige Einflussnahme von Glas-, Hinterglas- und Tafelmalerei. Die Autoren veranschaulichen die Forschungsergebnisse, die darauf hinweisen, dass sich vor allem Glasmaler der Hinterglasmalerei annahmen. Zudem zeigen ihre Untersuchungen, dass in der Renaissance und im Mittelalter innerhalb der verschiedenen Malerhandwerke ein enger Austausch existierte.
A combination of 3D micro X-ray fluorescence spectroscopy (3D micro-XRF) and micro-XRF was utilized for the investigation of a small collection of highly heterogeneous, partly degraded Dead Sea Scroll parchment samples from known excavation sites. The quantitative combination of the two techniques proves to be suitable for the identification of reliable marker elements which may be used for classification and provenance studies. With 3D micro-XRF, the three-dimensional nature, i.e. the depth-resolved elemental composition as well as density variations, of the samples was investigated and bromine could be identified as a suitable marker element. It is shown through a comparison of quantitative and semiquantitative values for the bromine content derived using both techniques that, for elements which are homogeneously distributed in the sample matrix, quantification with micro-XRF using a one-layer model is feasible. Thus, the possibility for routine provenance studies using portable micro-XRF instrumentation on a vast amount of samples, even on site, is obtained through this work.
The library of the remote monastery of Qäqäma Maryam Kidanä Mehrät in Däg'a Tämben (Tagray, North Ethiopia) was investigated by the team of the project Ethio-SPaRe in June and November 2012. A preliminary study of the library showed that the collection was extended and profoundly renovated in the nineteenth Century, in the course of the revival the monastery had during the reign of King Yohannas IV (1872-89). The shaping of the collection was apparently linked to the figure of the powerful abbot, Gäbrä Giyorgis, who donated dozens of books of diverse provenance, which he himself gathered or received as gifts.1 As the result, the extensive library contains a huge amount of information, but its heterogeneity poses a very serious challenge to the researcher.
In this work, the applicability of a new 3D micro X-ray fluorescence (3D Micro-XRF) laboratory spectrometer for the investigation of historical glass objects is demonstrated. The non-destructiveness of the technique and the possibility to measure three-dimensionally resolved fluorescence renders this technique into a suitable tool for the analysis of cultural heritage objects. Although absorption and resolution effects complicate qualitative analysis of the data, layered structures can be distinguished from homogeneous samples without the need for full quantification. Different manufacturing techniques were studied in this work with the help of hand-made reference samples. With the gained knowledge it could be shown for the investigated historical glass object, that black enamel as a stained glass contour colour was used in a cold painting. The object was not fired after the application of the black enamel, but instead the adhesion of the paint was solely provided through organic binding agents and the backing with metal foils. Thus, for the manufacturing of the object, a mixture of cold painting technique with a stained glass color was used. Quantitative measurements with a 3D Micro-XRF setup at the Berlin synchrotron BESSY II confirm the assumptions drawn on the basis of the qualitative investigation with the 3D Micro-XRF spectrometer with X-ray tube excitation.
This work addresses the identification of synthetic organic pigments (SOP) in eight modern reverse paintings on glass (1913–1946) by means of an in-situ multi-analytical approach. We combined the complementary properties of mobile Raman spectroscopy and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) to overcome the main disadvantages of each method: extensive band overlapping in DRIFT spectra and fluorescence problems in Raman spectra. A collection of DRIFTS reference spectra enables a precise pigment identification by DRIFTS and establishes this method as a serious non-destructive alternative for the identification of SOP. The group of β-naphthol pigments yielded valuable results for both methods, whereas synthetic alizarin (PR83) was preferentially detected by DRIFTS. Finally, uncommon triaryl carbonium pigments and two azo group-based yellows were identified in the paintings by means of Raman spectroscopy.
Nowadays, micro-x-ray fluorescence analysis has become an established tool for the non-destructive investigation of art objects. However, as these types of sample often forms complex and inhomogeneous layer systems, the quantitative evaluation of the measurements is far from a standard routine. In this paper a fingerprint model is described, which we developed to discriminate between different iron-gall inks of historical manuscripts or compositions. Fundamental parameter methods are used to take self-attenuation, interference from the paper background and diffusion of the ink into the paper into account. The capability of the method to contribute to the solution of archaeometric problems is exemplified by the investigation of an ancient composition. Finally, the restrictions of the model and possible improvements are discussed. Copyright © 2004 John Wiley & Sons, Ltd.
Nowadays, micro-x-ray fluorescence analysis has become an established tool for the non-destructive investigation of art objects. However, as these types of sample often forms complex and inhomogeneous layer systems, the quantitative evaluation of the measurements is far from a standard routine. In this paper a fingerprint model is described, which we developed to discriminate between different iron-gall inks of historical manuscripts or compositions. Fundamental parameter methods are used to take self-attenuation, interference from the paper background and diffusion of the ink into the paper into account. The capability of the method to contribute to the solution of archaeometric problems is exemplified by the investigation of an ancient composition. Finally, the restrictions of the model and possible improvements are discussed. Copyright © 2004 John Wiley & Sons, Ltd.
A new fundamental parameter based calibration procedure for micro X-ray fluorescence spectrometers
(2011)
Fundamental parameter based quantification of X-ray fluorescence (XRF) measurement data requires an accurate knowledge of the spectrometer parameters, including the spectral distribution of the excitation radiation. In case of micro-XRF where a polycapillary optic is utilized in the excitation channel this distribution is changed due to the transmission properties of the lens. A new calibration procedure, based on fluorescence data of thin standard samples, was developed to determine the excitation spectrum, i.e., the product of the X-ray tube spectrum and the transmission of the used X-ray optic of a micro-XRF setup. The calibration result was validated by the quantitative analyses of certified multi-element reference standards and shows uncertainties in the order of 2% for main components, 10% for minor elements and 25% for trace elements. The influence of secondary order effects like Coster–Kronig transitions and cascade effects is analyzed and the accuracy of fundamental parameters in common databases is discussed.
Our standard protocol for the characterisation of writing materials within advanced manuscript studies has been successfully used to investigate manuscripts written with a pure ink on a homogeneous writing surface. However, this protocol is inadequate for analysing documents penned in mixed inks. We present here the advantages and limitations of the improved version of the protocol, which now includes imaging further into the infrared region (1100−1700 nm).
Parchment has been in use for thousands of years
and has been used as the writing or drawing support for
many important historic works. A variety of analytical
techniques is currently used for routine assessment of the
degree of denaturation of historic parchment; however,
because parchment has a heterogeneous nature, analytical
methods with high spatial resolution are desirable. In this
work, the use of small-angle X-ray scattering (SAXS) and
synchrotron-IR (SR-IR) was examined in conjunction with
multivariate data analysis to study degradation of an
extended set of historic parchment samples, and particularly
to investigate the effect of lipids and the presence of iron
gall ink on the degradation processes. In the data analysis,
shrinkage temperature, lipid content, sample age, presence
of ink and accelerated degradation were included. The
analysis of loading factors in partial least-squares regression
and principal component analyses based on SAXS, SR-IR
and other analytical and descriptive data reveals the effect
of lipid removal on diffraction patterns, and lipids are found
to cause the degradation process in parchment to accelerate.
The effect of iron gall ink is also evident, although the
mechanism of ageing is different to that of natural ageing in
the absence of ink. In addition, a historic parchment score
from ca. 1750 is examined, demonstrating the significant
effect of iron gall ink, and lipids and inorganic soiling on its
increased degradation.