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Eingeladener Vortrag
- nein (67)
The qualitative and quantitative investigation of historical iron-gall inks using micro-XRF spectrometry is a suitable method for analyzing composition fingerprints of different ink types. The quantitative analysis is based on a model that takes into account the inhomogeneity and the layer structure of archaeometric samples. Starting from these composition fingerprints, it is possible to characterize distinguishable inks of one artist to classify different chronological ink types and, further, to date unknown fragments that have not so far been integrated into the lifework of an artist. The first qualitative and quantitative investigations of the manuscript Faust I and II and of the music composition The Magic Flute demonstrate impressively the identification of J. W. v. Goethe's and W. A. Mozart's artistic work with modern scientific methods. Further investigations on A. v. Arnim's manuscript Studien zu Naturwissenschaften provide evidence that the diversity of various degradation mechanisms of iron-gall inks could be mainly caused by different inorganic compositions.
X-ray absorption fine structure (XAFS) experiments in fluorescence mode have been performed in total reflection excitation geometry and conventional 45°/45° excitation/detection geometry for comparison. The experimental results have shown that XAFS measurements are feasible under normal total reflection X-ray fluorescence (TXRF) conditions, i.e. on droplet samples, with excitation in grazing incidence and using a TXRF experimental chamber. The application of the total reflection excitation geometry for XAFS measurements increases the sensitivity compared to the conventional geometry leading to lower accessible concentration ranges. However, XAFS under total reflection excitation condition fails for highly concentrated samples because of the self-absorption effect.
An verschiedenen Dämmstoffen, Montageschäumen, Computersystemen und Polstermöbeln sowie einer Matratze
wurden mittels unterschiedlicher Emissionsprüfkammern und -zellen in Kombination mit geeigneten Probenahme- und
Analyseverfahren Untersuchungen zur Emission polybromierter und phosphororganischer Flammschutzmittel (FSM)
durchgeführt. Hierbei kamen Emissionsprüfkammern mit Volumina von 0,02 m3 und 1 m3 sowie 0.001 m3 -
Emissionsprüfzellen zum Einsatz. Die hier untersuchten Substanzen zählen zu den SVOC und erfordern eine
Luftprobenahme durch Adsorption an Polyurethanschaum. Die Aufarbeitung des Polyurethanschaums erfolgte mit
Ultraschallbad- bzw. Soxhletextraktion, die Extrakte wurden aufkonzentriert und mit GC/MS oder HPLC/DAD vermessen.
Die ursprünglich angestrebte Versuchsdauer von jeweils 28 Tagen musste auf mindestens 100 Tage verlängert werden,
um einen für die Messung erforderlichen Gleichgewichtszustand zu erreichen. Mit den eingesetzten Verfahren läßt sich
die Emission der phosphororganischen FSM qualitativ und quantitativ gut nachweisen, hierzu gehören insbesondere
TCPP und TPP. Ausnahmen bilden z.B. RDP und BDP, hier wird die Emissionsmessung mittels Luftprobenahme durch
den Einfluss von Senkeneffekte dominiert. Für die bromierten FSM ist eine gute Anwendbarkeit für Verbindungen mit bis
zu sechs Bromatomen gegeben. Mit zunehmendem Bromierungsgrad und zunehmender Schwerflüchtigkeit verstärkt sich
auch hier der Einfluss von Senkeneffekten und erschwert die Bestimmung der Emission. So konnte HBCD zwar auf den
Kammerwandflächen jedoch, abgesehen von Spuren, nicht in der Emissionsprüfkammerluft nachgewiesen werden. Die
Erkenntnisse reichen für eine umfassende Darstellung des Emissionsverhaltens der FSM und darauf aufbauender
Expositionsbewertungen für den Gebrauch flammgeschützter Produkte noch nicht aus. Es bestehen weiterhin
Kenntnislücken, um die z.T. hohen Gehalte an FSM z.B. in Hausstäuben erklären zu können. Gleichwohl bildet die Studie
eine wesentliche Grundlage für weiterführende Untersuchungen. In Abhängigkeit vom Produkttyp betragen die ermittelten
flächenspezifischen (SERa) Emissionsraten z.B. für TCPP zwischen 0,012 und 140 µg m-2 h-1. Nachgewiesene PBDEs
zeigten je nach Produkttyp produktspezifische Emissionsraten (SERu) zwischen 0,1 und 14,2 ng Stück-1h-1 und SERa
zwischen 0,2 und 6,6 ng m-2 h-1. Eine Ausweitung z.B. auf Langzeitmessungen, die Bestimmung des Einflusses der
Materialalterung sowie unterschiedlicher Flammschutzmittelgehalte auf die Emission, die hier mangels hinreichender
Information und entsprechenden Produkten nicht durchgeführt werden konnte, wäre wünschenswert.
The emission levels of high boiling brominated (BFR) and phosphoric (POC) flame retardants (FR) in different materials were examined. For the determination of the emission rate the tests were done in different emission test chambers and cells under standard conditions (23 C, 50% RH and fixed area specific air flow rates). Selected products, e.g. printed circuit boards, were investigated at elevated temperature (e.g. 60 C) to simulate working conditions. Applied analytical techniques for the air samples adsorbed on polyurethane foam (PUF) are soxhlet and ultrasonic extraction. Different conditions were used to analyse the FR via GC-MS. Based on the first results it could be demonstrated that the emission depends on material density and surface condition. The concentrations over time obtained for tris(3-chloropropyl)-phosphate, e.g., from emission test chamber and cell show a good correlation, partly the measured concentration are different. Sampling at elevated temperature gives higher concentrations.
The emissions of selected flame retardants were measured in 1- and 0.02-m3 emission test chambers and 0.001-m3 emission test cells. Four product groups were of interest: insulating materials, assembly foam, upholstery/mattresses, and electronics equipment. The experiments were performed under constant environmental conditions (23°C, 50% RH) using a fixed sample surface area and controlled air flow rates. Tris (2-chloro-isopropyl)phosphate (TCPP) was observed to be one of the most commonly emitted organophosphate flame retardants in polyurethane foam applications. Depending on the sample type, area-specific emission rates (SERa) of TCPP varied between 20 ng m-2 h-1 and 140 ?g m-2 h-1.
The emissions from electronic devices were measured at 60°C to simulate operating conditions. Under these conditions, unit specific emission rates (SERu) of organophosphates were determined to be 1085 ng unit-1 h-1. Increasing the temperature increased the emission of several flame retardants by up to a factor of 500. The results presented in this paper indicate that emissions of several brominated and organophosphate flame retardants are measurable. Polybrominated diphenylethers exhibited an SERa of between 0.2 and 6.6 ng m-2 h-1 and an SERu of between 0.6 and 14.2 ng unit-1 h-1. Because of sink effects, i.e., sorption to chamber components, the emission test chambers and cells used in this study have limited utility for substances low vapour pressures, especially the highly brominated compounds; hexabromocyclododecane had an SERa of between 0.1 and 29 ng m-2 h-1 and decabromodiphenylether was not detectable at all.
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.
Model for inhomogeneous ink paper layer systems measured with micro X-ray fluorescence analysis
(2002)
Naturwissenschaftliche Informationen, insbesondere die chemische Zusammensetzung der Objekte, können Hinweise auf die Hintergründe der Objektherstellung liefern, die der alleinigen kunsthistorischen Begutachtung verborgen blieben. Es können nicht nur Fragen nach dem Prozess, Zeitpunkt und Ort der Herstellung beantwortet werden. Die chemische Analyse gibt auch Hinweise auf Ereignisse und Veränderungen, die erst nach der Fertigstellung des Objektes erfolgten. So werden Alterungsphänomene oder historische Überarbeitungen und Restaurierungen aufgedeckt, aber auch Konservierungsstrategien zur Erhaltung der Kunstwerke unterstützt. Durch den technologischen Fortschritt im Bereich der röntgenanalytischen Methoden, die berührungsfrei, ohne Probennahme und ohne Schädigung für das Untersuchungsobjekt arbeiten, erschließen sich dem Analytiker erstmalig Möglichkeiten, auch sehr wertvolle und fragile Objekte zerstörungsfrei zu untersuchen.
Zerstörungsfreie Mikro-Röntgenluoreszenzanalyse von historischen Schreib- und Zeichenmaterialien
(2005)
Ergebnisse der Tintenanalyse
(2005)
Various insulating boards, assembly foams, PC-systems, upholstery and a mattress were examined for possible
emissions of polybrominated and organophosphorus flame retardants. 0.02 m3- and 1m3- emission test chambers and
1Llitre cells were used to perform the investigations. The substances of interest are mainly classified as SVOC. A
sampling technique using polyurethane foam plugs and special analytical methods was developed. The PUF-plugs were
extracted by ultrasonic and soxhlet extraction and the extracts were concentrated. The analyses were performed by
GC/MS and HPLC/DAD. Chamber measurements were generally taken over 28 days, but in the case of SVOC, a test
period of a minimum of 100 days was necessary to achieve equilibrium. The determination of most of OPCs was
successful using emission test chambers. Due to sink effects the determination of low volatile OPC such as RDP and
BDP needs to be improved. Brominated flame retardants are quantifiable up to hexabrominated compounds using
emission test chambers as a reference method. The emission of lower volatile compounds, e.g. HBCD, was strongly
affected by sink effects. Emission of decaBDE was not quantifiable at all. Based on the results presented further
investigations are required for an adequate risk assessment of flame retarded products and their contribution to the
contamination of the indoor air environment. TCPP was found to be one of the most commonly used organophosphorus
flame retardants in polyurethane foam applications. Depending on the sample type 0.012 to 140 µg m-2 h-1 was obtained
for area-specific emission rates (SERa) for TCPP. PBDEs, for example, exhibited product-specific emission rates (SERu)
between 0.1 and 14.2 ng unit-1 h-1 and SERa between 0.2 and 6.6 ng m-2 h-1. More data about the emission behaviour of FR are required with special regard to substance migration, aging and long-term emission in particular.
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.
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.
Censorship of parts of written text was and is a common practice in totalitarian regimes. It is used to destroy information not approved by the political power. Recovering the censored text is of interest for historical studies of the text. This paper raises the question, whether a censored postcard from 1942 can be made legible by applying multispectral imaging in combination with laser cleaning. In the fields of art conservation (e.g. color measurements), investigation (e.g. Analysis of underdrawings in paintings), and historical document analysis, multispectral imaging techniques have been applied successfully to give visibility to information hidden to the human eye.
The basic principle of laser cleaning is to transfer laser pulse energy to a contamination layer by an absorption process that leads to heating and evaporation of the layer. Partial laser cleaning of postcards is possible; dirt on the surface can be removed and the obscured pictures and writings made visible again. We applied both techniques to the postcard. The text could not be restored since the original ink seems to have suffered severe chemical damage.
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.
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.
Was ist falsch am falschen Rembrandt - Mit High-Tech den Rätseln der Kunstgeschichte auf der Spur
(2011)
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.
The aim of the research project 'Typology of
Dutch Drawing' was to establish an interdisciplinary approach
for investigating heterogeneous drawing collections.
To define a type common to a group of drawings, we
determine elements that are common to them based on style
and the use of identical materials. To that end, we investigated
about 750 Dutch drawings from the sixteenth century at the
Dresden Kupferstich-Kabinett using art historical and
scientific methods. In this work, we present a detailed
analysis of 30 drawings ascribed to the Egmont Master.
In this study, we address the question of the
provenance and origin of the Dead Sea Scrolls manuscripts.
A characteristic low ratio of chlorine to bromine, corresponding
to that of the Dead Sea water, may serve as an indicator for
local production. For this aim we developed a non-destructive
procedure to determine the Cl/Br ratio in the parchment of
these manuscripts. Micro-X-ray fluorescence (µ-XRF) measurements
of a large number of parchment and leather
fragments from the Dead Sea Scrolls were analyzed with a
routine we developed based on fundamental parameter
quantification. This routine takes into account the absorption
of the collagen matrix and the influence of the different sample
thicknesses. To calculate the representative Cl/Br ratio for each
fragment, we investigated the lateral homogeneity and
determined the total mass deposition using the intensity of
the inelastically scattered, characteristic tube radiation. The
distribution of the Cl/Br ratios thus obtained from the µ-XRF
measurements make it possible to distinguish fragments
whose origin lies within the Dead Sea region from those
produced in other locations.
The Dead Sea Scrolls that miraculously survived for over two thousand years suffered considerable damage due to various post-dicovery interventions. Today they are subjected to frequent travelling exhibitions. The current work collates the published information on exhibitions and conservational treatments with the results of the analytic studies of the skin-based material of the scrolls conducted since their discovery. The examination of the properties of the scrolls proves that frequent travel, exhibitons and the associated handling induce collagen deterioration that is covered up by the absence of a proper monitoring program.
Corrosion processes
(2007)
The Erfurt Hebrew Giant Bible and the Experimental XRF Analysis of Ink and Plummet Composition
(2007)
Dead sea Scrolls: materials characterisation by means of synchrotron based µ-FTIR spectroscopy
(2007)
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 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).