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The lecture traces the origins of paper, the manufacture and the spread from China to the Middle East and Europe.
Though technological progress considerably affected each step of the manufacture of paper, the essence of the invention remains unchanged until today. The process of manufacturing handmade paper can be divided into a number of steps:
- choosing the raw material (e.g. cellulose from wood, cotton, rags)
- beating and grinding the fibres into small pieces
- producing a liquid pulp of the desired texture
- treating the pulp with various additives
- filling the pulp suspension into a paper mould
- draining the water
- pressing and drying to get the actual sheet
- various post-production treatments
We will see how the manufacturing process is reflected in the properties of the paper and its degradation. A special attention will be paid to the instrumental analysis for identification of the paper types. Also watermark play an important role in the studies of the manuscripts. A short overview will be offered at the ends of the lecture.
This paper reports the outcome of an interdisciplinary team’s application of multispectral imaging techniques and material analysis to a music fragment from the first decades of the fifteenth century: Atri, Archivio Capitolare, Museo della Basilica Cattedrale, Biblioteca del Capitolo della Cattedrale, Frammento 17. This important parchment leaf has rarely been investigated since its discovery 45 years ago. Thanks to the applied techniques and methods (such as the evaluation of the data using the fingerprint model), it is now possible to discuss new evidence supporting conclusions regarding the fragment’s origin and afterlife.
Light damage to selected organic materials in display cases: A study of different light sources
(2016)
The protection of works of art and cultural assets against light-induced aging is vital when planning exhibitions. Newly developed lighting systems render the selection of suitable light sources more difficult, not least in the context of energy–economical systems. This study accordingly examines different lighting systems (fluorescent tubes, halogen lamps, low-voltage metal halide lamps, and LED lamps) in terms of the damage potential they hold for the materials concerned. The changes in color were evaluated using the CIEDE2000 color-difference formula. This study focuses on selected organic materials and shows that changes in color already occur after only a brief exposure time. The color changes induced by the fluorescent tubes were consistently more intense than those induced by the other light sources. The results obtained with the remaining lamps show that the color changes depend more on the material under investigation than on the source used. The changes determined after a relatively short exposure period (five months) vividly demonstrate that exposing sensitive materials to light for longer terms (as is the case during a permanent exhibition) is most definitely a non-viable option.
Investigations of physical properties and chemical composition generate important data for answering cultural–historical questions that cannot be solved by historical and philological methods alone. In its individual materiality, each cultural asset is the result of a wide variety of influences (e.g. production, storage, restoration, preservation). Due to recent technological developments (e.g. miniaturization of structural units, enlargement of memory capacity), technical diagnostics in art and culture are becoming more and more coveted in such fields of trans-disciplinary research.
The qualitative and quantitative investigation of historical writing materials using micro-X-ray fluorescence analysis (micro-XRF) is a suitable method for obtaining information about the chemical composition of these materials. One the one hand these chemical composition fingerprints may answer some questions concerning the provenance of different materials, the chronology of their use, and give furthermore, the possibility to date unknown fragments in the lifework of an artist. On the other hand this method might be useful for the development and validation of conservation treatments.
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.
Nondestructive analyses of medieval reverse paintings on glass revealed the same dyes and pigments customarily used in panel paintings. However, there is one exception: the black colorant is not a carbon-based pigment, but black enamel. In this respect, the stylistic as well as the technical influence of stained glass artwork can clearly be seen on reverse paintings on glass. However, there is a crucial difference: in reverse paintings, the black enamel is not fired onto the glass but painted (cold painting). Additional analyses confirmed these findings. Based on these results, the art form "reverse painting on glass" has technically to be characterized as a mixture of "stained glass" and "panel painting" that nonetheless develops into a genre of its own.
Fe K-edge XANES measurements were performed to determine the oxidation state of iron in iron gall inks. These data are used to investigate the relationship between the Fe oxidation state and ink corrosion in historical manuscripts. The oxidation state is determined using the pre-edge based on a general variation trend that was derived from model compounds and validated here independently on a suite of samples with known oxidation state and Fe in octahedral coordination (i.e. similar to Fe in gall ink). As long as suitable references for the pure ferric and ferrous state of iron gall inks cannot be pointed out, the analysis of the pre-edge of the Fe K-edge represents the only way to acquire absolute values for the Fe oxidation state (Fe3+/Fetot) with spatial resolution for this usually non-crystalline compound. Fe3+/Fetot values for the ink samples vary between ca. 0.7 and 1.0. Spatially resolved analyses performed across ink strokes of various historical manuscripts as well as newly made samples did not reveal any systematic spatial dependence. On average, historical samples that were exposed to conservation treatments show a more oxidized state. However, the measurements demonstrate explicitly that the exposure to X-rays during the XANES acquisition affects the oxidation state of Fe in most iron gall inks.
The investigation of an ancient Chinese ceramic served to further develop and validate fundamental parameter-based quantitation procedures in reference-free x-ray fluorescence (XRF) analysis. The XRF measurements of this sample were performed at the four-crystal monochromator beamline of the Physikalisch-Technische Bundesanstalt (PTB) at the BESSY II synchrotron radiation facility employing different excitation energies. The parallel processing of the XRF spectra recorded at different excitation energies provides a means to simultaneously evaluate relevant fundamental parameters and secondary enhancement processes such as those induced by photoelectrons. Employing well-characterized and absolutely calibrated instrumentation, all experimental parameters involved in XRF are known for small relative uncertainties allowing for a completely reference-free quantitation. Apart from traces of rare earth elements, the analytical results of the Chinese ceramic achieved by reference-free XRF are in line with target values given within a proficiency test of the International Atomic Energy Agency (IAEA) involving atomic and nuclear methods.
The Erfurt Hebrew Giant Bible and the Experimental XRF Analysis of Ink and Plummet Composition
(2007)
Application of synchrotron infrared radiation in the study of organic coatings in cross-sections
(2008)
The Dead Sea Scrolls belong to the most important cultural assets of mankind. Their long term preservation and study is a challenge that demands an interdisciplinary approach. As early as the 1950s natural scientists assisted the scholars in studying the scrolls. It was at this time that the first extensive study of the scroll material took place. It was found that most fragments were written not on leather but on parchment. In addition, a method for determining the age of the parchment was developed which is still of value today. In the 1990s the AMS-C14 method confirmed the palaeographic determination of the age of the manuscripts. The use of carbon ink throughout the scrolls is also consistent with the known scribal practices of that time. There are, however, manuscripts, and among them the famous Genesis Apocryphon Scroll, which exhibit ink corrosion, normally associated with iron-gall inks.
Today, 60 years after their discovery, a community of scientists from the Jewish National and University Library (JNUL), the Technical University of Berlin (TU Berlin), the Federal Institute for Materials Research and Testing (BAM) and Fritz-Haber-Institute of the MPG (FHI) set out to scientifically investigate the finds of Qumran using the most modern methods. The results of the study will be used to determine the provenance of the texts as well as to contribute to their long-term preservation. A considerable part of the non-destructive investigation is taking place in the Berlin State Library and at the Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung , BESSY II.
Preliminary investigations, performed at the BAM on some fragments, were used to evaluate the extent to which X-ray analytical methods can provide information regarding the geographical origin of the fragments and match the individual pieces. The interpretation of the measurement results is made more difficult by age and storage of the objects. It is believed that ageing processes as well as conservation methods have altered the samples in addition to the changes caused by environmental influences.
In collaboration with the TU Berlin, the samples from the parchments found in the caves near Qumran were tested by means of three-dimensional synchrotron based X-ray fluorescence analysis (3D-SyXRF). The aim of this non-destructive investigation was the identification of the inorganic material used in the manufacture of the parchments.
The XRF experiments are supported by the non-destructive analysis by means of synchrotron based infrared spectroscopy (SyFTIR) in collaboration with BESSY II as well as optical and electron microscopy in collaboration with Fritz-Haber-Institute (FHI).
3D Micro X-ray fluorescence analysis was used for the investigation of reverse-glass paintings. The material-specific combination used in reverse-glass paintings leads to damage phenomena reinforced by glass corrosion. To elucidate the mechanism of corrosion processes taking place in the glass object depth profiles of mobile elements are of interest. In order to obtain elemental depth profiles of such kind of fragile objects the method of choice should be non-destructive. Our first results demonstrate the usefulness of the 3D Micro-XRF measurements for this kind of investigations. The assumption that certain binding media may initiate corrosion processes beginning at the interface glass/binding material could be confirmed.
The present study comprises the characterisation of museum show cases concerning their hazardous potential for
art objects. In order to estimate potential risks of damage the emission of volatile organic compounds coming from
several construction materials is monitored and different air exchange rates from exhibit cases are determined. For
the determination of the VOCs different methods were applied. The first step is a direct thermal extraction of the
materials followed by emission test chamber measurements. The tracer gas method with N2O that is used in this study is a convenient procedure to investigate air exchange rates under working conditions greater than 0.05 d-1. The results of this study confirm the importance of the careful choice concerning building materials for show cases. Furthermore the analyses clarify that certain organic compounds might be a problem for the exhibits in show cases with low air exchange rates.
We studied the oxidation and migration processes of inorganic compounds in iron gall inks with a combination of micro X-ray fluorescence analysis (micro-XRF) and micro X-ray absorption near edge structure spectroscopy (micro-XANES). With elemental mapping by micro-XRF, the correlation of the minor elements in the ink to the major element Fe was investigated. Along concentration profiles of Fe, micro-XANES measurements were carried out in order to determine the oxidation state and the local environment. With the help of model inks, we could show that Cu is a further important element in the paper degradation process due to iron gall ink corrosion.